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FIELD OF THE INVENTION
[0001] The present invention relates to compositions and methods for selectively increasing the growth of Staphylococcus epidermidis and inhibiting the growth of Staphylococcus aureus bacteria in the cutaneous microbiome. More particularly, the present invention relates to compositions and methods for increasing the growth of Staphylococcus epidermidis and reducing the incidence of MRSA and MSSA by the selective inhibition of Staphylococcus aureus.
BACKGROUND OF THE INVENTION
[0002] The cutaneous microbiome in humans is comprised of a variety of microorganisms, of which staphylococci, corynebacteria and propionibacteria are among the most prominent (Starkemann et al., 2005, Troccaz et al., 2004, Jackman, 1982). These bacteria act upon odorless precursors contained in sweat per se, producing sugars, sugar amines, amino acids, and short chain carboxylic acids (SCCAs), of which some are degraded further to products that include odorants that are associated to a major extent with cutaneous odor (Zeng et al, 1991; Jackman, 1982).
[0003] One frequent undesirable member of the cutaneous microbiome, Staphylococcus aureus ( Staph. aureus , including methicillin-resistant Staph. aureus (MRSA) and methicillin-susceptible Staph. aureus (MSSA)), has a well-known role in invasive infections in humans. It is one of the most problematic of human pathogens, because it is capable of wide infection and fatalities (see, e.g., David et al., 2010, Mainous III et al., 2006, Klevens et al., 2007). Antibiotics used against it have achieved limited success. Methicillin is effective but limited because of adaptation, which can result in the emergence of MRSA, which is representative of antibiotic failure occurring now more so with increasing frequency of use (see, e.g., David et al 2010, Chen et al 2006, Centers for Disease Control and Prevention 2003).
SUMMARY OF THE INVENTION
[0004] The present invention is directed to compositions of zinc salts and arginine and/or its salts for the selective inhibition of Staph. aureus growth and favoring growth of Staph. epidermidis.
[0005] The present invention is directed to a topical antibacterial composition including arginine or its salt, a zinc salt, and, optionally, a buffer for maintaining the pH of the composition at 6.0 or greater. The antibacterial compositions of the invention are useful in selectively inhibiting the growth of Staphylococcus aureus and increasing the growth of Staphylococcus epidermidis bacteria in the cutaneous microbiome.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] The invention will be more fully understood from the following detailed description taken in conjunction with the accompanying figures, in which:
[0007] FIG. 1 is a graph showing the effect of arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate at 37° C. for 72 hours.
[0008] FIG. 2 is a graph showing the effect of arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus aureus (MSSA), compared to 8.3% (v/v) Staphylococcus epidermidis , incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate at 37° C. for 72 hours.
[0009] FIG. 3 is a graph showing the effect of arginine bicarbonate on growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0010] FIG. 4 is a graph showing the effect of arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0011] FIG. 5 is a graph showing the effect of arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0012] FIG. 6 is a graph showing the effect of zinc carbonate on growth of 8.3% (v/v) Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL at 37° C. for 72 hours.
[0013] FIG. 7 is a graph showing the effect of arginine bicarbonate on the pH and growth of 8.3% (v/v) Staphylococcus aureus (MSSA), 8.3% (v/v) Staphylococcus epidermidis or an 8.3% (v/v) 1:1 mixture of Staphylococcus aureus (MSSA) and Staphylococcus epidermidis incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0014] FIG. 8 is a graph showing the effect of arginine bicarbonate on the growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate at 37° C. for 72 hours.
[0015] FIG. 9 is a graph showing the effect of arginine bicarbonate on the growth of 8.3% (v/v) Staphylococcus aureus (MRSA), compared to 8.3% (v/v) Staphylococcus epidermidis , incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0016] FIG. 10 is a graph showing the effect of arginine bicarbonate on the growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate, and modified versions of this medium, at 37° C. for 72 hours.
[0017] FIG. 11 is a graph showing the effect of arginine bicarbonate on the growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus aureus (MRSA) and Staphylococcus epidermidis incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0018] FIG. 12 is a graph showing the effect of arginine bicarbonate on the growth of 8.3% (v/v) Staphylococcus aureus (MRSA) incubated at various dilutions with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0019] FIG. 13 is a graph showing the effect of arginine bicarbonate on the growth of 8.3% (v/v) Staphylococcus epidermidis incubated at various dilutions with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0020] FIG. 14 is a graph showing the effect of zinc carbonate on the growth of 8.3% (v/v) Staphylococcus aureus (MRSA) incubated at various dilutions with 12.0 mM zinc carbonate and 6.0 mM CIL at 37° C. for 72 hours.
[0021] FIG. 15 is a graph showing the pH responses of 8.3% (v/v) Staphylococcus epidermidis, 8.3% Staphylococcus aureus (MRSA) or an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MRSA) to 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0022] FIG. 16 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0023] FIG. 17 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0024] FIG. 18 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MSSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0025] FIG. 19 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate, at 37° C. for 72 hours.
[0026] FIG. 20 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 0 hour.
[0027] FIG. 21 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of 8.3% (v/v) Staphylococcus epidermidis or 8.3% (v/v) Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate, and modified versions of this medium, at 37° C. for 24 hours.
[0028] FIG. 22 is a photograph showing the effect of 24.0 mM arginine bicarbonate on growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate and 6.0 mM CIL, with or without 24.0 mM arginine bicarbonate, at 37° C. for 48 hours.
[0029] FIG. 23 is a photograph showing the effect of arginine bicarbonate on growth of an 8.3% (v/v) 1:1 mixture of Staphylococcus epidermidis and Staphylococcus aureus (MRSA) incubated with 12.0 mM zinc carbonate, 6.0 mM CIL and 24.0 mM arginine bicarbonate, with or without an additional 24 mM arginine bicarbonate added at indicated times, at 37° C. for 72 hours,
DETAILED DESCRIPTION OF THE INVENTION
[0030] Corynebacteria, staphylococci and proprionibacteria are among the main microorganisms present in the cutaneous microbiome, with Staph. epidermidis, C. striatum and P. avidum as prominent representative bacteria
[0031] Unexpectedly, it has been discovered that certain compositions including a zinc salt and arginine and/or its salt are useful as antibacterial compositions, inhibiting Staph. aureus growth while favoring Staph. epidermidis growth. This ability to select between Staph. aureus and Staph. epidermidis allows the treatment of significant physiological and health-related disease conditions caused by aberrant or excessive growth of Staph. aureus (see, e.g., Peacock et al., 2001, Uehara et al., 2000). Although Staph. aureus is capable of wide infection and fatalities (see, e.g., David et al., 2010, Mainous III et al., 2006, Klevens et al., 2007), current antibiotic treatments have achieved limited success due to the emergence of resistant Staph. aureus strains, e.g., MRSA (see, e.g., David et al 2010, Chen et al 2006, Centers for Disease Control and Prevention 2003). A recent discovery has shown that firmicidin (Gallo et al., 2013, Nakatsuji et al., 2012), a newly discovered antibiotic generated by Staph. epidermidis , can reduce Staph. aureus , but it is not known whether this will, like other antibiotics, succumb to adaptation and loss of effectiveness. From a commercial stand-point, this approach is likely to be costly.
[0032] Unlike traditional antibacterial treatments, the compositions of the present invention are aimed at modulating natural interactions between Staph. aureus and other prominent members of the cutaneous microflora, e.g., Staph. epidermidis (see, e.g., Frank et al., 2010, Vehara et al., 2000, Wertheim et al., 2005). These bacteria naturally compete, e.g., for local resources and attachment to mucosal sites (Frank et al., 2010). The compositions of the invention, rather than merely targeting Staph. aureus , render an ecological change that favors selection of desirable Staph. epidermidis over non-desirable Staph. aureus bacteria.
[0033] Because the compositions of the present invention derive their antibacterial effectiveness not only by targeting Staph. aureus directly, but also by enhancing the ability of other, non-pathogenic bacteria (e.g., Staph. epidermidis ) to out-compete Staph. aureus . The compositions disclosed here are less likely to be susceptible to the emergence of resistant strains (e.g., MRSA) than traditional antibacterial treatments.
[0034] A further advantage of the present invention is that the compositions disclosed herein are effective in reducing cutaneous odor production. Thus, a single topical composition may be used as both deodorant and antibacterial treatment.
[0035] Antibacterial compositions as described herein are administered, preferably topically, for the treatment of any one or more symptoms desirable of change, e.g., Staph. aureus growth. Dosage forms are solid or free-flowing. Dosage forms include, but are not limited to, soaps, sprays, drops, aerosols, powders, roll-ons, lotions, creams, sticks, solutions, sachets, colloidal suspensions, films, patches and ointments.
[0036] Antibacterial compositions as described herein may have a pH of at least 6.0, or at least 7.0, or at least 8.0, or at least 9.0 upon topical administration.
[0037] Antibacterial compositions as described herein may optionally include one or more physiologically acceptable buffers sufficient to maintain the pH of said composition, e.g., at 6.0 or greater, at 7.0 or greater, at 8.0 or greater, or at 9.0 or greater upon topical application. Such buffers are generally known in the art, and may include, e.g., ACES, acetic acid, ADA, AMP, AMPD, bicine, bis-Tris, bis-Tris propane, BES, boric acid, cacodylate, CABS, CAPS, CAPSO, CHES, citric acid, diethanolamine, DIPSO, EPPS/HEPPS, ethanolamine, formic acid, glycine, glycylglycine, HEPES, HEPPSO, histidine, imidazole, lactic acid, maleic acid, malic acid, MES, MOPS, MOPSO, morpholine, phosphate, phosphoric acid, picolinic acid, PIPES, piperazine, piperidine, pivalic acid, POPSO, pyridine, succinic acid, TAPS, TAPSO, TEA, TES, tricine, and/or Tris.
[0038] Except where otherwise noted, the terms “axillary odor” and “foot odor” are used interchangeably herein, the terms “microbiome,” “microbiota,” and “microflora” are used interchangeably herein, the terms “foot,” “foot web,” “foot-web,” “toe,” “toe web” and “toe-web”are used interchangeably herein, and the terms “odor” and “malodor” are used interchangeably herein.
[0039] The terms “cutaneous” and “skin” refer, in the context of the present invention, regions of the human body including, e.g., the axilla, foot-webs and nasal atrium.
[0040] The terms “physiologically acceptable” and “physiologically-acceptable” denote, in the context of the present invention, “safe and effective when administered to humans and/or mammals in need thereof,” e.g., to reduce axillary odor, promote the growth of Staphylococcus epidermidis bacteria, inhibit the growth of Staphylococcus aureus bacteria, or any or all of the preceding.
Examples
[0041] The following examples are intended to illustrate, but not limit, the present disclosure.
[0000] Growth of Staph. aureus (MSSA or MRSA) and Staph. epidermidis when one or the other or a mixture of the two bacteria were incubated in the presence of (i) cysteine and (ii) isoleucine, leucine, phenylalanine. Zinc carbonate was also provided with and without arginine bicarbonate at 37° C. for 72 hours and with additional above ingredients adding into the cultural media in 37° C. water bath in 24 and 48 hours.
[0042] Materials and Methods for Growth Comparison Experiments Between Staph. epidermidis and Staph. aureus
(a) Preparation of Agar plates containing various bacterial growth media. Preparation included (i) BHI Blood agar (Fisher Scientific, Springfield, N.J. USA) and (ii) CHROMagar Staph. aureus agar (CHROMagar, Paris, France), especially prepared for the isolation and identification of Staph. aureus ; if present, it results in colonies that show a characteristic mauve color that enables ease of identification (French, 2009, Han et al., 2007). (b) Stock solutions of CIL amino acids. These amino acids include cysteine, isoleucine and leucine with each present at a concentration of 72 mM. Aqueous solutions of each were sterilized by syringe filtering as described earlier (Zhang and Kleinberg, 2014). (c) Stock aqueous solutions of arginine bicarbonate at 144 mM and zinc carbonate at 72 mM. Stock solutions of 144 mM arginine bicarbonate were sterilized together with 72 mM zinc carbonate by syringe filtering. Zinc carbonate has a limited solubility and hence is sterilized by first autoclaving as a powder and then dissolving it until saturation in sterile distilled water is achieved. This means that at 72 mM and above, it may have to be used as a zinc carbonate suspension. (d) Rabbit coagulase plasma (PL 850) and Prolex Staph Xtra Latex kits (PL.1080). Both of these items are provided as a kit and are obtained from Pro-Lab Diagnostics, Austin, Tex. They are prepared for the identification of pathogenic staphylococci (e.g., Staph. aureus ). (e) Experimental and control incubation mixtures containing Staph. epidermidis (ATCC 12228) and Staph. aureus (MSSA and/or MRSA). These incubation mixtures were prepared for comparison purposes and included MSSA (ATCC 25923) or MRSA (ATCC 33591) bacterial species mixed with the microorganism Staph. epidermidis . Pure cultures of Staph. epidermidis and Staph. aureus (MSSA or MRSA) were each prepared as 25% (v/v) bacterial suspensions in sterile distilled water. As above and as much as possible, bacterial pellets were broken up into fine particles, by stirring with a sterile TB syringe and a 25-27 gauge needle, if and when needed.
[0048] As a preparatory step, the resulting suspensions obtained were incubated in a shaking water bath at 37° C. for one hour, in order to deplete stored substrates acquired by some bacteria, during their preparatory growth period (Wijeyeweera and Kleinberg, 1989). The pH of each of the above bacterial suspensions was then measured by transferring 0.25 ml of such to a small sterile test-tube and measuring its pH. This made it easier to avoid any bacterial contamination during handling. Samples were then stored at 4° C. until time of inoculation of agar plates.
Preparation of Experimental and Control Samples
[0049] Preparation was performed according to information in Table 1 below.
[0000] TABLE 1.1 Experimental (A and B) and negative control (C) samples were prepared according to the following ABC Composition Tables: A. Experimental samples (ml) Composition I II III IV V VI Final concentrations Amino acids Cys 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Ieu 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Ileu 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Zinc Carbonate (72 mM) 0.45 0.45 0.45 0.45 0.45 0.45 12 mM Arg. Bicarbonate (144 mM) 0.45 0.45 0.45 — — — 24 mM (IV, V, VI = 0 mM) Staph. epidermidis (25%) 0.45 — 0.90 0.45 — 0.90 8.3% mixture 4.15% Staph. aureus 25% (MSSA or MRSA) 0.45 0.90 — 0.45 0.90 — 8.3% 4.15% D-water 0.225 0.225 0.225 0.675 0.675 0.675 Total volume (ml) 2.70 2.70 2.70 2.70 2.70 2.70 B. Experimental samples (ml) Composition IA IIA IIIA IB IIB IIIB Final concentrations Amino acids Cys 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Ieu 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Ileu 72 mM 0.225 0.225 0.225 0.225 0.225 0.225 6 mM Zinc Carbonate (72 mM) 0.45 0.45 0.45 0.45 0.45 0.45 12 mM Arg. Bicarbonate (44 mM) 0.45 0.45 0.45 0.45 0.45 0.45 24 mM Staph. epidermidis (25%) 0.45 — 0.90 0.45 — 0.90 8.3% mixture 4.15% Staph. aureus 25% (MRSA) 0.45 0.90 — 0.45 0.90 — 8.3% 4.15% D-water 0.225 0.225 0.225 0.225 0.225 0.225 Total volume (ml) 2.70 2.70 2.70 2.70 2.70 2.70 C. Negative controls Composition 1 2 3 Final concentrations Amino acids Cys 72 mM — — — — Ieu 72 mM — — — — Ileu 72 mM — — — — Zinc Carbonate (72 mM) — — — — Arg. Bicarbonate (144 mM) — — — — Staph. epidermidis (25%) 0.45 — 0.90 8.3% mixture 4.15% Staph. aureus 25% (MSSA or MRSA) 0.45 0.90 — 8.3% 4.15% D-water 1.80 1.80 1.80 Total volume (ml) 2.70 2.70 2.70 Arginine bicarbonate is absent in IV, V and VI
Dilutions of Experimental and Negative Control Samples and Inoculations of BHI Blood Agar and CHROMagar Staph. aureus Plates
[0050] Serial dilutions from 10 1 to 10 10 of each of experimental samples I, II, III, IV, V, VI and control samples 1, 2, 3 (see Table 1) were prepared with sterile distilled water. Each dilution contained 0.1 ml of serial diluted sample and 0.9 ml of sterile distilled water. BHI Blood agar plates were then inoculated with a mixture of 100 μl of a 10 4 to 10 10 concentration of Staph. epidermidis bacteria and 100 μl of a 10 4 to 10 10 sample of Staph. aureus (MSSA or MRSA) mixture (Samples I, IV and Negative Control 1) onto CHROMagar Staph. aureus plates using sterile glass bars on a turning table, respectively.
Incubation Procedures
[0051] As a first precautionary step, all agar plates were incubated for 24 hours in a 37° C. incubator and examined thereafter for bacterial growth to ensure initial agar plate sterility. Plates were then inoculated with samples taken at times 0, 24, 48 and 72 hours in succession throughout the 4 days of incubation. Successive inoculations consisted of the transfer of bacterial samples from a prior incubation to a subsequent fresh sterile plate, followed by incubation at 37° C. for 24-48 hours and subsequently repeating the process.
[0052] Colony density was scored for each of the plates as follows: between 0 and 10 as 0-no colonies; 1-<10 colonies; 2-10 to 20 colonies; 3-20 to 30 colonies; 4-30 to 50 colonies; 5-50 to 100 colonies; 6-100 to 250 colonies; 7-250 to 500 colonies; 8->500 colonies; 9-colonies almost fused to form a layer; 10-colonies forming a bacterial layer.
[0000] Differentiation of Colonies of Staph. aureus and Staph. epidermidis Derived from Growth on BHI Blood and CHROMagar SA Plates of Samples from Incubation Mixtures with Staph. aureus and Staph. epidermidis
[0053] Staph. aureus colonies are usually a golden yellow color and show large and complete blood hemolytic rings around the colonies that grow on BHI Blood agar plates. Use of the coagulase serum test (test procedure of Rabbit Coagulase Plasma provided by Pro-Lab Diagnostics, Austin, Tex. USA) and Prolex Staph Xtra Latex Test (Test Protocol of Prolix™ Staph Xtra Latex Kit provided by Pro Lab Diagnostics, Austin, Tex. USA) showed positive results. On CHROMagar Staph. aureus plates, where Staph. aureus colonies readily grow, they show, as pointed out above, a mauve color. In contrast, their counterpart, Staph. epidermidis colonies, are white and have no or small hemolytic rings around the colonies, when grown on BHI Blood agar plates. On CHROMagar Staph. aureus plates, Staph. epidermidis is unable to grow or able to form tiny white colonies. Coagulase serum and Prolex Staph Xtra Latex testing proved negative (i.e. no coagulation).
[0000] Inoculation of Samples Incubated in a Water Bath at 37° C. for 24 Hours and then Inoculated onto (i) BHI Blood Agar Plates and (ii) CHROMagar Staph. Aureus Plates
[0054] Following the same serial dilution procedures, as done for the Day 1 incubation period, Samples I, II, III, IV, V, VI and 1, 2, 3 were diluted serially 10 4 to 10 10 on BHI Blood agar plates. Similarly, samples of a mixture of Staph. epidermidis and Staph. aureus (I, IV and Negative Control 1) were prepared on CHROMagar Staph. aureus plates and incubated using the same procedures, as were used on Day 1, i.e. incubation at 37° C. for 24-48 hours.
Addition of Extra Ingredients to Samples, IA, IIA, IIIA and D3, IIB, IIIB Incubated as on Day 1, in a Water Bath at 37° C. for 24 Hours
[0000]
Under aseptic conditions, samples, IA, IIA, IIIA and IB, IIB, IIIB were each centrifuged and 1.35 ml of supernatant was removed from each of samples, IA, IIA, IIIA, and 1.125 ml of supernatant from samples, IB, IIB, IIIB, respectively.
The table immediately below, lists additional ingredients introduced into samples:
[0000]
TABLE 1.2
Volumes (ml) added to experimental samples
Ingredients
IA
IIA
IIIA
IB
IIB
IIIB
Cys 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Ieu 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Ileu 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Zinc Carbonate
0.225
0.225
0.225
—
—
—
(72 mM)
Arg. Bicarbonate
0.450
0.450
0.450
0.450
0.450
0.450
(144 mM)
[0057] Incubation of all experimental and control samples in a 37° C. water bath was continued for another 24 hours. Total incubation time to this point was 48 hours.
Day 3 in the Experimental Protocol (i.e., the 48-72 Hour Time Period).
[0058] This period consisted of bacterial growth on the medium agar plates inoculated on Day 2 and incubated at 37° C., (as above), on medium agar plates for another 24 hours and preparation of samples for incubation continuation for another 24 hours. Bacterial growth on BHI Blood agar and CHROMagar Staph. aureus plates was then determined as before.
[0059] The next step was inoculation of samples incubated in a 37° C. water bath for a total of 48 hours on the BHI Blood agar plates and CHROMagar Staph. aureus plates.
The same procedures of serial dilutions, as was done on Day 1, was carried out here; i.e. all samples (I, II, III, IV, V, VI, 1, 2, 3 and IA, IIA, IIIA, IB, IIB, IIIB) Inoculated 10 4 to 10 10 serial dilutions of samples on BHI Blood agar plates and the samples of the mixture of SE and SA (I, IA, IB, IV and Negative Control 1) on CHROMagar Staph. aureus plates were tested by following the same procedures as was done on Day 1. Plates were incubated as before at 37° C. between and for 24 and 48 hours.
Preparation of Samples for Incubation in a Water Bath at 37° C. for 48 Hours and Followed then for a Further 24 Hours
Additional ingredients were added to samples of IA, IIA, IIIA and IB, IIB, IIIB, which were each incubated in a 37° C. water bath for a total period of 48 hours. Samples IA, IIA, IIIA and samples IB, IIB, IIIB were centrifuged as before and 1.35 ml of supernatant was removed from samples, IA, IIA, IIIA; and 1.125 ml of supernatant was also removed from samples, IB, IIB, and IIIB, respectively. Table 1.3, below, was followed in order to serve as a guide for adding additional ingredients into the samples:
[0000]
TABLE 1.3
The (ml) volumes added to the experimental samples
Ingredients
IA
IIA
IIIA
IB
IIB
IIIB
Cys 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Ieu 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Ileu 72 mM
0.225
0.225
0.225
0.225
0.225
0.225
Zinc Carbonate
0.225
0.225
0.225
—
—
—
(72 mM)
Arg. Bicarbonate
0.450
0.450
0.450
0.450
0.450
0.450
(144 mM)
Incubation of all experimental and control samples in the water bath at 37° C. was extended for another 24 hours (i.e. 72 hours total).
Day 4 (72-96 Hours, i.e., the Last Part of the Instant Experimental Protocol)
[0067] Bacterial growth on medium agar plates inoculated on Day 3 was examined and then incubated in a water bath at 37° C. for a total of 72 hours.
[0000] Examination of Bacterial Growth on BHI Blood Agar and CHROMagar Staph. Aureus Plates Inoculated on Day 3
[0068] The same methods were followed as was done on Day 4.
[0000] Inoculation of Samples Incubated at 37° C. for a Total of 72 Hours on BHI Blood Agar Plates and CHROMagar Staph. Aureus Plates
The same procedures of serial dilution were followed as was done on Day 1 for all samples (I, II, III, IV, V, VI, 1, 2, 3 and IA, IIA, IIIA, IB, IIB, IIIB,) Inoculation of 10 4 to 10 10 serial dilutions of samples on BHI Blood agar plates and the samples of the mixture of SE and SA (I, IA, IB, IV and 1) on CHROMagar Staph. aureus plates were the same as the procedures carried out on Day 1. Plates were then incubated at 37° C. for 24-48 hours.
Day 5 (End of Experiment, 96 Hours Total Duration)
[0072] Examination of bacterial growth on media agar plates inoculated on Day 4 and a review of the entire experiment was performed. Examination of bacterial growth on BHI Blood agar and CHROMagar Staph. aureus plates inoculated was performed on Day 4 by following the same methods as was done on Day 1.
Results
[0073] Overview of the bacterial growth of all samples on the BHI Blood agar plates and on the CHROMagar Staph. aureus plates in the 72 hour experiments reported herein are shown in Tables 1.4, 1.5 and 1.6. FIGS. 1-15 depict the effect of different media on bacterial growth. Photographs showing colony growth data from which the Figures were derived are set forth as FIGS. 16-23 .
[0000]
TABLE 1.4
Density (1-10*) of colonies of Staphylococcus epidermidis (SE) and Staphylococcus aureus
(MSSA) when incubated in media comprised of 6 mM cysteine, 6 mM isoleucine, 6 mM leucine
(i.e., 6 mM CIL) and 12 mM zinc carbonate, with or without 24 mM arginine bicarbonate
at 37° C. for 72 hours, compared with negative control (water only)
Medium-Cys, Ileu, Leu,
Medium-Cys, Ileu, Leu,
Negative Control
zinc carbonate with
zinc carbonate without
Medium (Water only)
arginine bicarbonate
arginine bicarbonate
Time of
Times of dilution of 8.3% bacteria incubated in media
Bacteria
Incubation
Plates
10 4
10 5
10 6
10 7
10 4
10 5
10 6
10 7
10 4
10 5
10 6
10 7
SE
0 h
BHI
9
9
8
8
9
9
8
8
9
9
8
8
MSSA
Blood
9
9
9
9
10
9
9
9
10
9
9
9
Mix
Agar
9
9
9
9
10
9
9
9
10
9
9
9
CHRO
9
9
9
9
10
9
9
9
10
9
9
9
SE/SA
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
% (~)
SE
24 h
BHI
9
8
7
7
8
7
6
5
5
1
1
1
MSSA
Blood
9
8
7
5
7
3
2
1
8
7
5
4
Mix
Agar
9
8
7
5
8
6
4
3
8
7
7
6
CHRO
9
8
7
5
6
4
2
1
8
7
7
6
SE/SA
. . .
. . .
5/95
10/90
. . .
70/30
60/40
80/20
. . .
15/85
15/85
20/80
% (~)
SE
48 h
BHI
9
8
7
6
5
2
1
1
0
0
0
0
MSSA
Blood
8
7
6
5
5
2
1
1
8
7
6
6
Mix
Agar
9
8
7
6
6
2
1
1
8
7
6
5
CHRO
9
7
6
5
5
2
1
1
8
7
6
5
SE/SA
. . .
. . .
10/90
20/80
10/90
15/85
. . .
. . .
. . .
5/95
5/95
5/95
% (~)
SE
72 h
BHI
8
7
6
3
1
1
0
0
0
0
0
0
MSSA
Blood
8
6
4
3
0
0
0
0
7
2
1
1
Mix
Agar
9
7
5
3
2
0
0
0
7
5
4
2
CHRO
9
7
5
4
1
0
0
0
7
5
4
X
SE/SA
. . .
5/95
5/95
0
20/80
. . .
. . .
. . .
. . .
0
0
. . .
% (~)
SE, Staph. epidermidis ,
MSSA, Staph. aureus (MSSA),
Mix, mixture of Staph. epidermidis and Staph. aureus (MSSA),
CHRO, CHROMAgar medium plate selective for Staph. aureus ,
X, contamination
*Scale (0-10): 0, no colony; 1, <10; 2, 10-20; 3, 20-30; 4, 30-50; 5, 50-100; 6, 100-250; 7, 250-500; 8, >500; 9, colonies almost form a layer and are unable to count; 10, colonies form a layer
[0000]
TABLE 1.5
Density (1-10*) of colonies of Staphylococcus epidermidis (SE) and Staphyloccus aureus
(MRSA) when incubated in media comprised of 6 mM cysteine, 6 mM isoleucine, 6 mM leucine
(i.e., 6 mM CIL) and 12 mM zinc carbonate, with or without 24 mM arginine bicarbonate
at 37° C. for 72 hours, compared with negative control (water only)
Medium-Cys, Ileu, Leu,
Medium-Cys, Ileu, Leu,
Negative Control
zinc carbonate with
zinc carbonate without
Medium (Water only)
arginine bicarbonate
arginine bicarbonate
Time of
Times of dilution of 8.3% bacteria incubated in media
Bacteria
Incubation
Plates
10 4
10 5
10 6
10 7
10 4
10 5
10 6
10 7
10 4
10 5
10 6
10 7
SE
0 h
BHI
9
9
8
7
9
8
8
8
9
8
8
8
MRSA
Blood
10
9
8
8
10
9
8
8
9
8
8
8
Mix
Agar
10
9
8
7
10
9
8
8
9
8
8
8
CHRO
10
9
8
7
10
9
8
8
9
8
8
8
SE/SA
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
% (~)
SE
24 h
BHI
9
9
8
8
8
8
8
8
7
6
6
6
MRSA
Blood
10
9
9
8
7
5
5
5
9
8
8
8
Mix
Agar
10
9
8
8
8
7
5
5
9
8
8
X
CHRO
10
9
8
8
6
5
3
2
8
8
8
6
SE/SA
. . .
. . .
. . .
. . .
. . .
60/40
80/20
80/20
. . .
. . .
. . .
. . .
% (~)
SE
48 h
BHI
9
8
7
6
6
4
3
1-3
0
0
0
0
MRSA
Blood
9
8
7
7
1
1
0
0
7
6
3
1
Mix
Agar
9
8
7
6
1
0
0
0
7
6
5
5
CHRO
9
8
6
6
0
0
0
0
6
5
4
4
SE/SA
. . .
. . .
. . .
5/95
. . .
. . .
. . .
. . .
10/90
20/80
20/80
20/80
% (~)
SE
72 h
BHI
8
8
7
6
5
5
4
3
1-3
0
1-3
0
MRSA
Blood
9
8
7
7
0
0
0
0
7
6
4
4
Mix
Agar
8
8
7
6
1
1
1
1
7
7
6
6
CHRO
8
8
6
5
0
1
1
0
7
6
6
6
SE/SA
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
5/95
10/90
5/95
5/95
% (~)
SE, Staph. epidermidis ,
MRSA, Staph. aureus (MRSA),
Mix, mixture of Staph. epidermidis and Staph. aureus (MRSA),
CHRO, CHROMAgar medium plate selective for Staph. aureus ,
X, contamination
*Scale (0-10): 0, no colony; 1, <10; 2, 10-20; 3, 20-30; 4, 30-50; 5, 50-100; 6, 100-250; 7, 250-500; 8, >500; 9, colonies almost form a layer and are unable to count; 10, colonies form a layer
[0000] TABLE 1.6 Density (1-10*) of colonies of Staphylococcus epidermidis (SE) and Staphyloccus aureus (MRSA) when incubated in media comprised of 6 mM cysteine, 6 mM isoleucine, 6 mM leucine (i.e., 6 mM CIL) and 12 mM zinc carbonate, with or without 24 mM arginine bicarbonate at 37° C. for 72 hours, compared with negative control (water only) Media containing 6 mM Cys, 6 mM Leu, 6 mM Ileu, 12 mM zinc carbonate, 24 mM arginine bicarbonate Additional same Additional 24 mM No additional above media added arginine bicarbonate added medium added in 24 and 48 hours in 24 and 48 hours Time of Times of dilution of 8.3% bacteria incubated in media Bacteria Incubation Plates 10 4 10 5 10 6 10 7 10 4 10 5 10 6 10 7 10 4 10 5 10 6 10 7 SE 0 h BHI 9 8 8 8 9 8 8 8 9 8 8 8 MRSA Blood 10 9 8 8 10 9 8 8 10 9 8 8 Mix Agar 10 9 8 8 10 9 8 8 10 9 8 8 CHRO 10 9 8 8 10 9 8 8 10 9 8 8 SE/SA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . % (~) SE 24 hr BHI 8 8 8 8 8 8 8 8 8 8 8 8 MRSA Blood 7 5 5 5 7 5 5 5 7 5 5 5 Mix Agar 8 7 5 5 8 7 5 5 8 7 5 5 CHRO 6 5 3 2 6 5 3 2 6 5 3 2 SE/SA 70/30 60/40 80/20 80/20 . . . 60/40 80/20 80/20 . . . 60/40 80/20 80/20 % (~) SE 48 h BHI 6 4 3 1 7 6 4 1 8 7 5 4 MRSA Blood 1 1 0 0 1 0 0 0 1 1 0 0 Mix Agar 1 0 0 0 5 1 1 0 7 5 1 1 CHRO 0 0 0 0 1 0 0 0 3 1 1 0 SE/SA . . . . . . . . . . . . 90/10 . . . . . . . . . 90/10 90/10 . . . . . . % (~) SE 72 h BHI 5 5 4 3 6 5 4 2 7 5 4 4 MRSA Blood 0 0 0 0 0 0 0 0 0 0 0 0 Mix Agar 1 1 1 1 3 0 0 1 7 7 6 5 CHRO 0 1 1 0 0 0 0 0 5 5 4 1 SE/SA . . . . . . . . . . . . 100/0 . . . . . . . . . 90/10 80/20 80/20 80/20 % (~) SE, Staph. epidermidis , MRSA, Staph. aureus (MRSA), Mix, mixture of Staph. epidermidis and Staph. aureus (MRSA), CHRO, CHROMAgar medium plate selective for Staph. aureus , X, contamination *Scale (0-10): 0, no colony; 1, <10; 2, 10-20; 3, 20-30; 4, 30-50; 5, 50-100; 6, 100-250; 7, 250-500; 8, >500; 9, colonies almost form a layer and are unable to count; 10, colonies form a layer
Tables 1.4-1.6, above, include the following elements:
(a) Incubation of Staph. epidermidis and Staph. aureus and their combinations in the medium containing 12 mM zinc carbonate, 24 mM arginine bicarbonate, the CIL amino acids and their controls, showed: (i) Staph. aureus (MSSA or MRSA) quickly decreased, when incubated in the presence of arginine bicarbonate for 24 to 48 hours; all Staph. aureus organisms completely disappeared by 72 hours (see supporting FIGS. 1, 8, 16 and 19 ). (ii) Staph. epidermidis on the other hand decreased only slightly, when incubated with the medium containing arginine bicarbonate during the first 24 hours of incubation and decreased moderately or rapidly in the 48 to 72 hours thereafter (see relevant FIGS. 1, 2, 8, 9, 16 and 19 ). (iii) The mixture of Staph. aureus (MSSA or MRSA) and Staph. epidermidis also showed decreases, albeit only moderately, while being incubated in the medium containing arginine bicarbonate for 24 hours and where approximately 60-80% of survivors were Staph. epidermidis . The Staph. aureus/Staph. epidermidis mixture decreased quickly after 24 hours of incubation and almost all of the bacteria had disappeared by 72 hours (see FIGS. 3, 11, 18 and 22 ). (iv) In the negative control, both Staph. aureus (MSSA or MRSA) and Staph. epidermidis and the mixtures thereof incubated in sterile D-water, showed almost no reduction in 24 to 48 hours and very slight reduction in 48 to 72 hours (see FIGS. 1, 8, 16 and 19 ). (b) Incubating Staph. aureus (MSSA or MRSA), Staph. epidermidis and their combinations in a medium containing the CIL amino acids, and zinc carbonate without arginine bicarbonate exhibited: (i) Staph. aureus (MSSA or MRSA) that showed no or slight reduction, while incubating for 24 to 48 hours and then decreased slightly or moderately thereafter. Staph. aureus showed much slower reduction of its numbers in the medium without arginine bicarbonate than when incubated in medium containing arginine bicarbonate (see FIGS. 2, 9, 17 and 20 ). (ii) Staph. epidermidis showed moderate to rapid reduction in numbers during incubation for 24 hours and disappeared after 48 hours (see FIGS. 2,9, 17 and 20 ). (iii) Within 72 hours, the mixture of Staph. aureus (MSSA or MRSA) and Staph. epidermidis decreased moderately, while incubating in medium without arginine bicarbonate. Also, within 72 hours, approximately 70-90% of survivors were Staph. aureus , whereas in the mixture incubated in the medium containing arginine, bacteria correspondingly decreased slowly in 24 hours. About 70-75% of survivors were Staph. epidermidis and the mixture rapidly decreased in 48 to 72 hours. Almost all bacteria disappeared by 72 hours (see FIGS. 3, 11, 18, 22 and 23 ). (c) The results of Staph. aureus (MRSA) and Staph. epidermidis being incubated in the medium including 12 mM zinc carbonate, 24 mM arginine bicarbonate, the CIL amino acids, and additional same medium or 24 mM arginine bicarbonate being added in 24 and 48 hours during 72 hours of incubation at 37° C. showed: (i) Slow Staph. epidermidis reduction during the first 24 hours and slower reduction after 48 to 72 hours, when additional same medium was added, at 24 and 48 hours. Staph. epidermidis even decreased, albeit more slowly, when additional 24 mM arginine bicarbonate was added after 24 and 48 hours, whereas Staph. aureus (MRSA) decreased, moderately to rapidly, after 48 hours with no microbial survivors after 72 hours. There were no differences among the incubation media and additional medium, whether arginine bicarbonate was or was not added (see FIG. 10 and Photo 21). (ii) The mixture of Staph. aureus (MRSA) and Staph. epidermidis decreased in a similar pattern, as did Staph. epidermidis with 60% of survivors being Staph. epidermidis after 24 hours of incubation and more than 90% Staph. epidermidis survivors after 48 to 72 hours of incubation (see FIG. 11 and Photo 23). (d) Staph. aureus (MSSA or MRSA) was incubated with 12 mM zinc carbonate, 24 mM arginine bicarbonate and the CIL amino acids and decreased more and faster than being incubated in medium without arginine bicarbonate. This occurred within 72 hours of incubation, especially after 24 hours of incubation, when compared to samples diluted 10 4 to 10 6 (see FIGS. 4 and 12 ). In contrast, Staph. epidermidis decreased much less and more slowly in media containing arginine bicarbonate than being incubated in media without arginine bicarbonate, especially during 72 hours of incubation (see FIGS. 5 and 13 ). (e) The pH values of Staph. epidermidis, Staph. aureus (MSSA or MRSA) and mixtures thereof, when incubated with zinc carbonate, CIL and with or without arginine bicarbonate, and additional same medium or 24 mM arginine bicarbonate being added at 24 and 48 hours during 72 hours of incubation at 37° C., in comparison to a negative control (see FIGS. 7 and 15 ). (i) pH values of SE, SA and their mixture incubated in media containing arginine bicarbonate were stable at pH 8.3 to 8.6. (ii) pH values of SE, SA and their mixture incubated in media without arginine bicarbonate stayed at lower pH levels i.e. 6.1 to 6.8. (iii) Bacteria incubated in sterile distilled water that served as negative controls, had similar pH values, as counterpart bacteria incubated in media without arginine bicarbonate at pH 6.0 to 6.4.
DISCUSSION
[0091] The results obtained in the experiments above demonstrated that a medium of 12 mM zinc carbonate, 24 mM arginine bicarbonate and 6 mM CIL (i.e., 6 mM of each of cysteine, isoleucine and leucine), when incubated in a water bath at 37° C. for 72 hours, was able to bring about a decrease in both Staph. epidermidis (SE) and Staph. aureus (MSSA or MRSA) levels ( FIGS. 1 and 8 ). However, such a medium favored much of a reduction of Staph. aureus (MSSA or MRSA) and did so significantly more rapidly than reduction of Staph. epidermidis ( FIGS. 2 and 9 ). The number of both bacteria decreased sharply after 24 hours of incubation ( FIGS. 2 and 9 ). This appeared to be due to substrate depletion, since addition of arginine bicarbonate to the medium during the Staph. epidermidis incubation only decreased its numbers slightly ( FIG. 10 ). To be noted, Staph. aureus (MRSA) showed no positive selection at all. Almost all of the Staph. aureus (MRSA) bacteria involved had disappeared after 48 to 72 hours ( FIG. 10 ).
[0092] In contrast (see FIGS. 4, 5, 12 and 13 ), when Staph. epidermidis was incubated without arginine bicarbonate present, its numbers decreased much sooner than when the medium contained arginine bicarbonate. Staph. aureus (MSSA or MRSA) showed opposite results.
[0093] This implies that the medium containing 12.0 mM zinc carbonate, 24.0 mM arginine bicarbonate and 6.0 mM CIL amino acids was able to inhibit the growth of Staph. aureus (MSSA or MRSA), while maintaining growth of Staph. epidermidis . In other words and needing emphasis is that arginine bicarbonate was able to support the growth of Staph. epidermidis , while not similarly benefiting Staph. aureus (MSSA or MRSA) at all.
As a Non-Limiting Explanation:
[0000]
(1) Media containing arginine bicarbonate was able to maintain the media pH at a constant 8.3-8.6 pH level during 72 hours of incubation (see FIGS. 7 and 15 ). This was beneficial for the growth of Staph. epidermidis , which has proven herein to be a major bacterium for maintenance of a normal skin microflora and for suppressing Staph. aureus (MSSA or MRSA), i.e. pathogens of considerable concern. The medium containing zinc carbonate and CIL, but with no arginine bicarbonate present, had a pH between 6.1 and 6.8 (see FIGS. 7 and 15 ), which evidently was able to inhibit the growth of Staph. aureus (MSSA or MRSA) slightly to moderately (see FIGS. 6 and 14 ). But, it was not able to strongly inhibit Staph. aureus (MSSA or MRSA), in a medium containing arginine bicarbonate (see FIGS. 6 and 14 vs. 4 and 12). In contrast, Staph. epidermidis was quickly reduced in this medium ( FIGS. 5 and 13 ). This would most importantly imply that a reason for this is that the alkaline pH (8.3-8.6), which promoted the growth of Staph. epidermidis , and its anti- Staph. aureus effectiveness, resulting in reduction of the growth of Staph. aureus (MSSA or MRSA).
(2) Evidently, as explanation, the pH may not have been the only factor to affect the survival of Staph. epidermidis and Staph. aureus.
[0096] Although the overall pH of the medium (zinc carbonate, arginine bicarbonate and CIL) and additional same medium or 24 mM arginine bicarbonate being added at 24 and 48 hours during 72 hours of incubation, was maintained at pH 8.3-8.6; it showed remarkably well that as more arginine bicarbonate was added to the medium, the density of Staph. epidermidis that was ultimately obtained was increased. Nonetheless and most importantly, this indicated that arginine bicarbonate can play a significant enhancement role in the growth of Staph. epidermidis and that this effect may be largely but not solely due to the elevated and sustained pH favored by the presence of arginine bicarbonate.
[0097] In contrast, Staph. aureus (MSSA or MRSA) incubated in the medium containing zinc carbonate, CIL and no arginine bicarbonate or in a sterile distilled water negative control (both of which show a pH in the range of 6.0-6.8) showed almost no reduction in growth after 72 hours of incubation in distilled water (see FIGS. 1, 7, 8 and 15 ). However, there was moderate reduction during incubation for 72 hours in a medium containing zinc carbonate, and CIL without arginine bicarbonate (see FIGS. 6 and 14 ). Accordingly, one can conclude that zinc carbonate is an important ingredient for suppression of Staph. aureus (MSSA and MRSA) growth, and plays thereof a significant inhibitory role as well.
[0098] The present invention is not limited in scope by the specific embodiments described herein. Indeed, various modifications of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description and the accompanying figures. Such modifications are intended to fall within the scope of the appended claims.
[0099] It is further to be understood that all values are approximate, and are provided for description. Patents, patent applications, publications, product descriptions, and protocols are cited throughout this application, the disclosures of which are incorporated herein by reference in their entireties for all purposes.
REFERENCES
[0000]
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2. Chen, A. E., Goldstein, M., Carroll, K., Song, X., Perl, T. M., Siberry, G. K.: Evolving epidemiology of pediatric Staphylococcus aureus cutaneous infections in a Baltimore hospital. Pediatr. Emerg. Care, 22:717-723, 2006.
3. David, M. Z., Daum, R. S.: Community-associated methicillin-resistant Staphylococcus aureus : epidemiology and clinical consequences of an emerging epidemic. Clin. Microbiol. Review, 23 (3):616-87, 2010.
4. Denepitiya, L., Kleinberg, I.: A comparison of the acid-base and aciduric properties of various serotypes of the bacterium Streptococcus mutants associated with dental plague. Arch. Oral Biol., 29:385-393, 1984.
5. Denepitiya, L., Kleinberg, I.: A comparison of the microbial compositions of pooled human dental Plaque and salivary sediment. Arch. Oral Biol., 27:739-845, 1982.
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9. Gallo, R. L., Nakatsuji, T.: Firmocidin, an antimicrobial molecule produced by
[0109] Staphylococcus epidermidis . U.S. Patent Application Publication 2013/0331384 A1.
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[0111] CHROMagar Staph aureus and CHROMagar MRSA for detection of methicillin-resistant Staphylococcus aureus from nasal swab specimens. J. Med. Microbiol., 56 (1):43-46, 2007.
11. Jackman, P. J. H.: Body odor—the role of skin bacteria. Sem. Dermatol., 1 (2):143-148, 1982. 12. Kleinberg, I., Codipilly, D.: Cysteine challenge testing: a powerful tool for examining oral malodour processes and treatments in vivo. Inter. Dental J., 52:221-228, 2002. 13. Kleinberg, I., Codipilly, D.: H2S generation and Eh reduction in cysteine challenge testing as a means of determining the potential of test products and treatments for inhibiting oral malodor. J. Breath Res., 2:1-9, 2008. 14. Kleinberg, I., Codipilly, D.: Modeling of the oral malodor system and methods of analysis.
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15. Klevens, R. M., Morrison, M. A., Nadle, J., Petit, S., Gershman, K., Petit, S., Ray, S., Harrison, L. H., Lynfield, R., Dumyati, G., Townes, J. M., Craig, A. S., Zell, E. R., Fosheim, G. E., McDougal, L. K., Carey, R. B., Fridkin, S. K.: Invasive methicillin-resistant Staphylococcus aureus infections in the United States. J. Am. Med. Assoc., 298:1763-1771, 2007. 16. Leyden, J. J., McGinley, K.: Coryneform bacteria. The skin microflora and microbial skin disease. Cambridge Univ. Press, 102-141, 1992. 17. Leyden, J. J., McGonley, K. J., Holzle, E., Labows, J. N., Kligman, A. M.: The microbiology of human axilla and its relationship to axillary odor. J. Inv. Derm., 77:413-416, 1981. 18. Mainous III, A. G., Hueston, W., Everett, C. J., Diaz, V. A.: Nasal Carriage of Staphylococcus aureus and Methicillin-Resistant S aureus in the United States 2001-2002. Ann. Fam. Med., 4 (2):132-137, 2006. 19. Nakatsuji, T., Nam, S., Fenical, W., Gallo, R. L.: Skin commensal bacteria acts as antimicronial shield: Identification of firmocidin, a novel small-molecule antobiotoc produced by Staphylococcus epidermidis . J. Inv. Derm., 132: S114, 2012. 20. Nobel, W. C.: Staphylococci on the skin. The skin microflora and microbial skin disease.
[0123] Cambridge Univ. Press, 135-152, 1992.
21. Pader, M.: Oral hygiene products and practice. Cosmetic science and technology series. New
[0125] York, Basel: Marcel Dekker, 6:344-359, 1988.
22. Peacock, S. J., de Silva, I., Lowy, F. D.: What determines nasal carriage of Staphylococcus aureus ? TRENDS Microbiol., 9 (12):605-610, 2001. 23. Sandham, H. J., Kleinberg, I.: Effect of glucose concentration on carbon dioxide production in a human salivary sediment system. Arch. Oral Biol., 15:1285, 1970. 24. Shehadeh, N., Kligman, A. M..: The bacteria responsible for axillary odor II. J. Invest. Derm., 41:3, 1963. 25. Starkenmann, C., Niclass, Y., Troccaz, M., Clark, A. J.: Identification of the precursor of (S)-3 methyl-3-sulfanylhexan-1-ol, the sulfury malodour of human axilla sweat. Chem Biodivers., 2:705-716, 2005. 26. Taylor, D., Daulby, A., Grimshaw, S., James, G., Mercer, J., Vaziri, S.: Characterization of the microflora of the human axilla. Intern. J. Cosm. Scien., 25:137-145, 2003. 27. Troccaz, M., Starkenmann, C., Niclass, Y., Waal, Mvd., Clark, A. J.: 3 methyl-3-sulfanylhexan-1-ol, as a major descriptor for the human axilla-sweat odour profile. Chem Biodiversity, 1:1022-1035, 2004. 28. Uehara, Y., Nakama, H., Agematsu, K., Uchida, M., Kawakami, Y., Abdul Fattah, A. S. M., Maruchi, N.: Bacterial interference among nasal inhabitants: eradication of Staphylococcus aureus from nasal cavities by artificial implantation of Corynebacterium sp. J. Hosp. Infect., 44:127-133, 2000. 29. Wertheim, H. L. F., Melles, D. C., Vos, M. C., Leeumen, W. V., Belkum, A. V., Verbrugh, H. A., Nouwen, J. L.: The role of nasal carriage in Staphylococcus aureus infection. Lancet Infect. Dis. 5:751-62, 2005. 30. Wijeyeweera, R. L., Kleinberg, I.: Acid-base pH curves in vitro with mixtures of pure cultures of human oral microorganisms. Arch. Oral Biol., 34 (1):55-64, 1989. 31. Zeng, X. N., Leyden, J. J., Lawley, H. J., Sawano, K., Hohara, I., Preti, G.: Analysis of characteristic odors from human male axillae. J. Chem. Ecol., 17 (7):1469-1492, 1991. | An antibacterial composition comprising arginine bicarbonate, zinc carbonate, preferably arginine bicarbonate and zinc carbonate (ABZC), in combination, plus one or more physiologically acceptable excipients, administered for the modification of cutaneous microfloras, generally to inhibit the growth of pathogenic Staphylococcus aureus bacteria by promoting the growth of non-pathogenic Staphylococcus epidermidis bacteria. | 0 |
FIELD OF THE INVENTION
This invention relates to the preparation, by chemical synthesis, of methyl ecgonine phosphonates as analogues of transition states, for the hydrolysis of the benzoyl ester bond in cocaine, and their linking to carrier proteins. By these methods, the phosphonates are produced rapidly in satisfactory yields. The resulting immunogens elicit the formation, in experimental animals, of antibodies capable of hydrolysis of cocaine. Both these catalytic antibodies and the immunogens used to induce them are potentially useful for the treatment of individuals at risk for the abuse of cocaine. Such compounds also are useful for immunodiagnostic purposes with respect to such individuals.
BACKGROUND OF THE INVENTION
Cocaine is an ecgonine ester compound of the formula: ##STR1## (ref. 1--a list of references appears at the end of the descriptive text. This paper provides an overview of nomenclature. Compound names used in this specification are defined in this article).
The abuse of cocaine represents a major threat to the social and economic fabric of many developed countries. Although several dopaminergic agents and the tricyclic antidepressant desipramine have been clinically tested, effective therapies to assist drug-addicted individuals in their return to drug-free life still are not available. Mobilizing the immune system to "block" drugs from reaching their sites of action in the central nervous system represents a potential, but as yet poorly explored, means of therapeutic intervention.
It is well known that drugs of abuse can be rendered inactive by disrupting a structural feature either required for the interaction with their respective receptors or necessary for transport. Thus, in cocaine, the presence of the benzoyl ester moiety in the molecule is essential for maintaining its activity. Therefore, if antibodies possessing cocaine-specific esterase activity could be induced, such catalytic antibodies could potentially act in vivo to neutralize the pharmacological effects of the drug in an immunized individual. Enzymes and abzymes (otherwise known as catalytic antibodies) apparently employ a similar mechanism for the catalysis of hydrolysis.
Abzymes, as any catalyst, lower the energy required to proceed through the transition state between the starting compound and the respective reaction products. Thus, a catalytic antibody binds to and stabilizes a shape corresponding to the transition state with little or no energy expenditure on the part of the substrate.
Depending on the presence of other factors, the substrate then could proceed to the product or to return to its starting form. In the case of hydrolysis, water must be present, since the hydroxyl group of the water, due to its nucleophilic properties, enters the protransition state and forms the proper transition state for the hydrolysis, and the hydrolysis then takes place. Therefore, a catalytic antibody should be ideally made against such a transition state. However, since transition states are unstable by definition, antibodies have to be made against stable molecules which structurally mimic the transition state (transition state analogs). It has been established that the transition state (ref. 2) for carboxylate ester hydrolysis is centered around unstable formally "pentavalent" carbon, and consequently it can be mimicked by a stable phosphonate ester (ref. 3) since phosphorus is stable pentavalent and shapes and charge distribution of both resemble each other fairly closely. However, esters are among the most common functional groups in living organisms, and thus it is essential that the abzyme is devoid of any general esterase activity and is endowed with very specific benzoyl esterase activity in this context of the cocaine molecule. To achieve this objective, it is crucial that the transition state analog does not disrupt structural features defining specificity of interaction between cocaine and the recognition moiety of the abzyme. If this condition is not met, the antibodies made against such transition state analogs will not be sufficiently specific to be practical.
It is recognized that polar groups in a molecule tend to be the focal point of B-cell (i.e. antibody reactive epitopes. In cocaine, there are three polar groups, namely the bridgehead nitrogen (methylated), the methyl ester, and the benzoyl ester. As explained above, since the benzoyl ester is the target for the hydrolysis by a catalytic antibody, the transition state for the hydrolysis of the benzoyl ester can be mimicked by substituting phenylphosphonate for benzoate in the cocaine molecule. Such a phosphonate has to be linked to a carrier protein, as is conventionally required to enhance the immunogenicity of small molecules. Linkers have to be of appropriate length to maintain the transition state analog at the optimal distance from the antibody binding site. If the linker is too short, the carrier protein could interfere sterically, while, if it is too long, the linker may fold back to the protein, so that the transition state analog would adhere to the protein molecule or its fragments after processing.
Four sites for anchoring the linker on the cocaine molecule are identifiable (listed in order of increasing synthetic difficulty):
(i) a substitution of the N-methyl group by an alkyl chain, the other end of which is bound to a carrier protein (e.g. utilizing the amino group of a lysine in the carrier protein);
(ii) a substitution of the methyl ester by a bifunctional molecule, such as a dicarboxylic acid, the other end of which again is bound to a carrier protein, either directly or through an extension chain;
(iii) p-substitution at the phenyl ring of the phenylphosphonate group with a chain linked again to a carrier protein directly or through an extension chain; and
(iv) a substitution of a ring hydrogen in the ecgonine ring system by a chain of carbon atoms, the other end of which is functionalized so that a bond to a carrier protein can be formed.
Although the third choice (iii) appears to be the best one since it disturbs least of all the important recognition elements of cocaine and remains still within the reach of organic synthetic methodology for a possible future mass production, an attempt was described to link a phenylphosphonate analog of cocaine (ref. 4) via an alkyl chain originating in the nitrogen function utilizing anchoring site (i). Although a number of binding monoclonal antibodies have been isolated, none of them was endowed with the desired catalytic activity, thus confirming the conclusion of the discussion hereinabove.
At least two attempts have been made utilizing the anchoring site (ii). The transition state analog using a specific linker (ref. 5) was described that using the state of the art methodology made possible isolation of two catalytic monoclonal antibodies with small, albeit detectable catalytic activity. Identical transition state analogs using a different linker to BSA or KLH (compounds 5a, 5b, FIG. 1--ref. 6) gave a polyclonal binding antibody in rabbits, and several binding monoclonal antibodies, none of them endowed with catalytic activity. This result could be expected, as it has been outlined hereinabove.
SUMMARY OF INVENTION
The present invention provides certain novel compounds which are methyl ecgonine phosphonate ester derivatives. Accordingly, in one aspect of the present invention, there is provided a novel methyl ecgonine phosphonate ester having the formula: ##STR2## wherein R is selected from:
(a) a functional group,
(b) the group (-Y-functional group), wherein Y is a linker group, including an alkylene radical, and
(c) the group (-Y-carrier molecule), wherein Y is a linker group, including an alkylene radical.
The compounds where R is a functional group are useful intermediates in the preparation of the compounds where R is the group (-Y-functional group), which, in turn are useful intermediates in the preparation of the compounds where R is the group (-Y-carrier molecule). The compounds where R is a functional group also are useful as intermediates in the preparation of the compounds where R is the group (-Y-carrier molecule). The preparation of such intermediate compounds is described below.
The compounds where R is the group (-Y-carrier molecule) are immunogens capable of inducing antibodies which accelerate the hydrolysis of cocaine in an addicted animal, particularly a human.
As noted above, the linkage between the phosphonate ester and the carrier protein should be of sufficient length that the carrier protein does not interfere with the esterase activity of the overall molecule. If the linkage is too short, then the carrier protein may interfere sterically with the phenylphosphonate while, if the linkage is too long, then the carrier protein may fold back and again interfere sterically. The linkage may comprise covalently-bonded functional groups and carbon atoms in an alkylene radical. In general, the linkage may comprise from about 5 to about 15 linearly-linked atoms, preferably about 8 to about 10 atoms.
Accordingly, in another aspect of the invention, there is provided an immunogenic composition useful for the immunization of an animal, comprising an effective amount of the novel methyl ecgonine phosphonate ester provided herein in which R is (-Y-carrier molecule) or an antibody raised thereto, and a pharmaceutically-acceptable carrier. The invention, in a further aspect, provides a method for the treatment of a cocaine-addicted animal, particularly a human, which comprises administering to the animal an immunogenic composition as just described to generate cocaine-neutralizing antibodies in the animal.
The latter compounds, i.e. the compounds where R is the group (-Y-carrier molecule), also are useful in diagnostic applications. In one such diagnostic application, the compounds can be used to screen persons for cocaine use by testing serum taken from a person for the generation of antibodies to the compounds using any convenient assaying technique, such as an ELISA assay.
The latter compounds also are useful in generating antibodies to the compounds in an animal, which antibodies themselves, which may be monoclonal or polyclonal, are useful in diagnostic assays and also in therapy, as a result of their cocaine-neutralizing property. Such antibodies also are useful for research purposes with respect to cocaine addiction.
One therapeutic application, which may have particular application to neonates of cocaine-addicted mothers, involves removing serum from an addicted animal, treating the serum with the cocaine-hydrolyzing antibodies, preferably with the antibodies in an immunobilized form, and returning the treated serum to the animal.
The novel method ecgonine phosphonate esters of the invention may be prepared by any convenient synthesis procedure. However, it is preferred to effect substitution of methyl ecgonine (i.e. 2β-methoxycarbonyltropan-3β-ol) at the free hydroxyl group by an activated phosphonyl substituted phenyl compound which is also substituted by a protected functional group. This procedure is a novel chemical process and constitutes a further aspect of this invention.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 contains a schematic illustration of cocaine and certain derivatives thereof, referred to herein as compounds 1 to 5;
FIG. 2A is a schematic illustration of hydrolysis of cocaine (Scheme 1);
FIG. 2B is a schematic illustration of a synthesis scheme (Scheme 2) for producing cocaine analog conjugate derivatives in accordance with one embodiment of the present invention;
FIG. 3 contains graphical representations of an ELISA titration of mouse anti-hapten response to cocaine analog conjugate derivatives provided in accordance with one embodiment of the invention;
FIG. 4 contains graphical representations of an ELISA titration of rabbit anti-hapten response to cocaine analog conjugate derivatives provided in accordance with one embodiment of the invention;
FIG. 5 contains graphical representation of capillary electrophoresis monitoring of the rate of enzymatic degradation of cocaine into ester hydrolysis products; and
FIG. 6 contains graphical representation of capillary electrophoresis monitoring of the rate of degradation of cocaine by antibodies raised against cocaine analog conjugate derivatives.
GENERAL DESCRIPTION OF THE INVENTION
As described above, in one aspect, we have not discovered how to prepare an immunogen capable of inducing antibodies which accelerate the hydrolysis of cocaine utilizing methyl ecgonine phenylphosphonate p-substituted with a tether or a linker to a carrier protein (=cocaine-based immunogen, or CBI). The cocaine-based immunogen can be prepared from ecgonine methyl ester and phenylphosphinic dichloride substituted in the p-positoin with a carbon-based chain functionalized at its other end. This functionality may comprise, but is not limited to, a carboxylic group. The product of this reaction then can be linked to a carrier molecule comprising, but not limited to, a serum albumin, either directly or by using a carrier molecule containing a tether ending with a functional group capable of forming a linkage with a transition state analog derivative described above. An example of such a group is an amino group. Although we have described the combination of a carboxylic and an amino group to form a linkage, a combination of other two groups, well known in the art, can be utilized.
The cocaine-based immunogen prepared by methods just described may be utilized in the immunization of mice to produce hybridomas capable of making monoclonal anti-cocaine antibodies having esterase activity by methods well established in the field of immunology. Such catalytic mouse anti-cocaine monoclonal antibodies may form the basis for constructing "humanized" monoclonal antibodies of therapeutic value by the application of established genetic engineering technologies. Alteratively, the cocaine-based immunogen may be utilized for immunization of animals suitable for making anti-cocaine polyclonal sera (from which antibodies may be separated by purification, if desired), similarly having esterase activity. The ultimate utilization for the cocaine-based immunogen is foreseen to be immunization of humans with such cocaine-based immunogens containing a carrier suitable for human use. Such immunization would maintain the presence of the anti-cocaine esterase activity in the body so that the use of cocaine by an immunized person would not produce the desired physiological effects but rather the cocaine would be hydrolyzed in the human body.
The present invention provides, in a further aspect thereof, a process for the preparation of cocaine-based immunogens, which comprises the steps of:
a) forming a reaction product of a methyl ecgonine phenylphosphonate p-substituted with a tether or linking group to a carrier protein or other carrier molecule, such as a peptide or polypeptide, or a reaction product having a tether or linking group terminating with a functional group, which permits the formation of a linkage to a carrier protein or other carrier molecule;
b) activating the carrier molecule, if necessary, by, but not limited to, derivatization of the carrier molecule with a suitable group capable of binding to the functional group at the end of the tether or linking group by a covalent bond stable under physiological conditions; and
c) subjecting the reaction product having a tether or linking group terminating with a functional group to a condensation reaction with the activated carrier to form a desired carrier-linked product.
The cocaine-based immunogen produced by these procedures may be usually isolated as a solid. The cocaine-based immunogen then may be used:
(i) for immunization of animals to prepare monoclonal antibodies utilising any convenient protocol;
(ii) for immunization of animals to prepare polyclonal antibodies utilising any convenient protocol;
(iii) for the treatment of humans for cocaine addiction by way of immunization; and
(iv) for the diagnosis of addiction or exposure of a person to cocaine.
The monoclonal antibodies or polyclonal sera and antibodies derived therefrom may be used as is or in humanized form for the treatment of humans for cocaine addiction by in vivo administration or in vitro serum treatment.
DESCRIPTION OF PREFERRED EMBODIMENTS
In order that the invention may be better understood, preferred embodiments now are described by way of example only, with reference to the accompanying reaction schemes and diagrams. In one preferred form of the invention, methyl ecgonine (compound 9) or 2β-methoxycarbonyltropan-3β-ol may be transformed into the cocaine-based immunogen (compounds 12, 14) by a sequence of chemical reactions portrayed in FIG. 2B. Phosphorylation of benzyl 4-bromophenylacetate (compound 6) under nickel chloride catalysis (formation of compound 8 via intermediate compound 7) is of particular importance since it is the crucial step in the reactions scheme not previously known in the art. In all other aspects, the conditions of reactions performed follow protocols generally established in synthetic organic chemistry and any other convenient procedure.
A number of methods known to those skilled in the art may be adapted to follow quantitatively the hydrolysis of cocaine to 2β-methoxycarbonyltropan-3β-ol and benzoic acid by reaction Scheme 1 shown in FIG. 2A. One such method utilizes capillary electrophoresis and detection at λ=200 nm, as described in detail in Example 9 below and illustrated in FIG. 5. Thus, it is possible to quantitatively measure the hydrolysis of cocaine by either following the loss of cocaine itself, or appearance of the cocaine breakdown products benzoic acid and 2β-methoxycarbonyltropan-3-β-ol. The activity of catalytic antibodies and catalytic antisera can be directly related to the activity of naturally occurring esterases, comprising ψ-cholinesterase, or control sera.
Protein conjugates 12a,b and 14a,b (see FIG. 2B) of the analogs of transitions state for the hydrolysis of the cocaine benzoyl ester are used as immunogens in mice and rabbits. Rabbits provide large volume of antisera and mice provide the potential for generating monoclonal antibodies for conventional hybridoma technology. The esterase activity directed against cocaine benzoyl ester of purified antibodies from either control or immunized rabbits, and from selected hybridomas, was assayed by capillary electrophoresis as described hereinabove. The conjugates 12a,b were endowed with this cocaine esterase activity.
EXAMPLES
The following Examples are used to illustrate the present invention. They should not be construed as limiting it in any way. All parts and percentages are by weight unless otherwise indicated. All abbreviations and acronyms have the standard meanings in the art.
General Chemical Procedures
Melting points were determined on a Reichert-Thermovar melting point apparatus and are not corrected. Optical rotations were measured with a Perkin-Elmer polarimeter (Model 243 B) at 26° C. 1 H and 13 C NMR spectra were recorded at 300.13 MHz (75.47 MHz, 13 C) or 500.15 MHz (125.04 MHz 13 C) with Bruker spectrometers at the NMR Spectroscopy Laboratory, Carbohydrate Research Centre, University of Toronto. Spectra were obtained at 20° C. either in CDCl 3 or CD 3 OD containing a trace of TMS (0 ppm, 1 H and 13 C) as internal standard. Fast Atom Bombardment mass spectra (FAB-MS) were recorded with a VG Analytical ZAB-SE instrument at the Mass Spectrometry Laboratory, Carbohydrate Research Centre, University of Toronto. High Resolution Mass Spectrometry (HRMS) is used for exact mass measurements. Thin-layer chromatography (TLC) was performed on silica 6OF (Merck) plastic plates and visualized by spraying with 50% aqueous sulphuric acid and heating at 200° C. Silica gel (230-400 mesh, Toronto Research Chemicals) was used for flash chromatography. All solvents and reagents used were reagent grade.
Examples 1-6
Synthesis of Haptens and Antigens
Example 1
This Example illustrates the preparation of benzyl 4-bromophenylacetate (compound 6, FIG. 2B).
To a suspension of 4-bromophenylacetic acid (2.150 g, 10 mmol) and benzyl alcohol (2.5 mL) in dry dichloromethane (20 mL) was added dicyclohexylcarbodiimide (2.5 g) at 0° C. The mixture was allowed to warm up to room temperature, and stirred overnight. After dilution with dichloromethane (250 mL), the solution was washed with water, dried over sodium sulphate, and dichloromethane was evaporated to give an oily residue. This residue was subsequently subjected to flash chromatography on silica gel using hexane/ethyl acetate (9:1) to give pure compound 6 in 88% yield (3.81 g). 1 H NMR (CDCl 3 ): 7.47-7.42 (m, 2H), 7.31-7.40 (m, 5H), 7.15-7.17 (m, 2H), 5.16 (s, 2H), 3.61 (s, 2H).
Example 2
This Example illustrates the preparation of benzyl 4(diethylphosphonyl-)phenylacetate (compound 7, FIG. 2B).
Triethylphosphite (10 mL) was added dropwise to a mixture of compound 6 (7.51 g, 20 mmol) and nickel chloride (0.5 g) heated at 160° C., and the reaction continued to be heated to this temperature for additional 3 hours. Then the mixture, cooled to room temperature, was diluted with dichloromethane (250 mL) and filtered through a celite bed. The filtrate was washed with water, dried over sodium sulphate and evaporated to dryness. The oily residue was purified by flash chromatography on silica gel using ethyl acetate to give pure compound 7 (7.11 g, 811% yield). 1 H NMR (CDCl 3 ); 7.86-7.77 (m, 2H), 7.45-7.42 (m, 2H), 7.30-7.40 (m, 5H), 5.15 (s, 2H), 4.10-4.20 (m, 6H), 3.70 (s, 2H), 1.38 (t, J=6 Hz 9H). Exact mass measurement (EI): for C 18 H 23 O 5 P calc. 361.1283, found 362.1267.
Example 3
This Example illustrates the preparation of 2β-(methyloxycarbonyl-)tropan-3β-yl 4-(benzyloxycarbonylmethyl-) phosphonate (compound 10, FIG. 2B).
A mixture of compound 7 (2.80 g, mmol) and trimethylsilyl bromide (TMSBr; 2.01 g) was stirred under argon overnight at room temperature. The excess TMSBr was removed in vacuo, and to the residue was added imidazole (25 mg) and oxalyl chloride (1 mL) and the resulting solution was stirred overnight at room temperature. Then both the solvent and volatiles were evaporated in vacuo and the resulting crude dichloride 8 (FIG. 2B) was diluted with pyridine (10 mL) and added to a solution of triazole (1.0 g) in pyridine (20 mL) and stirred for 30 minutes. Then ecgonine methyl ester (compound 9, FIG. 2B; 1.81 g) was added to this solution and the reaction mixture was stirred for 1 hour at room temperature. The reaction mixture was diluted with 1M TEABC buffer (50 mL) and the resulting solution was extracted with chloroform (7×50 mL). The combined chloroform extracts were evaporated to dryness in vacuo to give compound 10 in 71% yield (2.98). 1 H NMR (CDCL 3 ): 7.77-7.62 (m, 27.41-7.12 (m, 7H), 5. 11 (s, 2H), 4.50 (m, 1H), 3.70 (s, 3H), 3.55 (s, 2H),2.40 (s, 3H). 1 H NMR (D 2 O): 7.80-7.70 (m, 2H), 7.50-7.41 (m, 7H), 5.21 (s, 2H), 4.62-4.59 M, 1H), 4.02 (d, J=6.7 Hz, 1H), 3.95 (d, J=7 Hz, 1H), 3.88 (s, 3H), 3.72 (s, 2H), 3.10 (dd, J=9 Hz, 2Hz, 1H), 2.80 (s, 3H). Exact mass measurement (FAB): for C 25 H 31 NO 7 P calc. 468.1838, found 488.1819.
Example 4
This Example illustrates the preparation of 2β-(methyloxycarbonyl-)tropan-3β-yl 4-(methylcarboxyl-) phosphonate (compound 11, FIG. 2B).
To a solution of the compound 10 (750 mg) in glacial acetic acid (15 mL) was added Pd/C (10%; 100 mg) and the mixture was hydrogenated in a Parr instrument overnight. Then the mixture was diluted with dichloromethane (250 mL), the solution was filtered through a celite bed, and the filtrate was evaporated to dryness in vacuo to give compound 11 (600 mg). 1 H NMR (D 2 O): 7.73-7.66 (m, 2H), 7.45-7.40 (m, 2H), 4.65-4.58 (m, 1H), 4.10 (d, J=7.20, 1H), 3.95 (d, J=6.80, 1 H), 3.77 (s, 3H), 3.755 (s, 2H), 3.49 (dd J=11, 1.5 Hz, 1H), 2.80 (s, 3H). Exact mass measurement (FAB): for C 18 H 24 NO 7 PNA calc. 420.1188, found 420.1157.
Example 5
This Example illustrates the preparation of protein conjugates 12a and 12b (FIG. 2B).
Compound 11 (30 mg), KLH (30 mg) and dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (20 mg) was dissolved in water (20 mL) and adjusted to pH=5 by TEABC buffer. After stirring this solution at room temperature for 48 hours, it was filtered through YM-30 (Amicon) membrane filter using 3×10 mL distilled water. The membrane filter was decanted with distilled water 3×10 mL, and the aqueous solution after lyophilization to dryness gave protein conjugate 12a. Using BSA instead of KLH, protein conjugate 12b was obtained.
Example 6
This Example illustrates the preparation of protein conjugates 14a and 14b (FIG. 2B).
A solution of 6-aminocaproic acid (3.0 g), KLH (500 mg) and dimethylamino-propyl-3-ethylcarboiimide hydrochloride (1.0 g) in water (50 mL), adjusted to pH=5 by TEABC buffer, was stirred for 48 hours. Then it was filtered through YM-30 (Amicon) membrane filter using 3×10 mL distilled water. The membrane filter was decanted with distilled water 3×10 mL, and the aqueous solution after lyophilization to dryness gave 6-aminocaproyl KLH (compound 13a, FIG. 2B). Using BSA (0.5 g) instead of KLH, compound 13b, FIG. 2B, was obtained.
A reaction of free carboxyl-containing compound 11 (70 mg) and 6-aminocaproyl KLH (compound 13a) (50 mg) according to the procedure used to synthesize 12A and 12b (as described in Example 5), gave protein conjugate 14a. Under identical conditions, compound 11 reacted with 6-aminocaproyl BSA (compound 13b) to give protein conjugate 14b.
General Immunological Procedures
Antibody Purification Protocol
Antibodies were purified from rabbit sera using Protein A Sepharose chromatography. Briefly, serum was diluted 1/10 with 50 mM Tris/150 mM NaCl (pH=8.6) and loaded slowly onto a Protein A Sepharose column. After all the material was loaded, the column was washed with 3 column volumes of 50 mM Tris/150 mM NaCl (pH=8.6). Bound antibodies were eluted with 50 mM sodium acetate/150 mM NaCl buffer (pH=3.5) after the column had been washed sequentially with 50 mM sodium phosphate/150 mM NaCl buffer (pH=7.0) and 50 mM sodium citrate/150 mM NaCl buffer (pH=5.5). Eluted antibodies were dialyzed against 5 mM sodium borate buffer (pH=8.3) and quantified using extinction coefficient of 1.43 at 280 nm for a 0.1% solution (1 mg/mL).
Enzyme-Linked ImmunoSorbent Assay (ELISA) Protocol
ELISA assays were used to determine by titration the level of hapten-specific antibody in the sera of immunized animals. Ninety-size well ELISA plates (NUNC-MaxiSorp) were coated with 100 μL of 10 μg/mL hapten-conjugate in 20 mL sodium carbonate buffer (pH=9.6) overnight (6 hours). Excess reactants were washed away with 0.05% Tween 80 in phosphate buffer saline (pH=7.2; PBS/Tween) using a Corning plate washer. Residual protein-binding sites on the ELISA plates were blocked by coating the wells with 1% low-fat milk PBS (pH=7.2) for 30 minutes, and washing the plates again. Diluted 1/8→1/16,384 with PBS, pH=8.0! sera (50 μL) were added to the wells and incubated at 37° C. for 1 hour. Then wells were washed 3× with PBS/Tween and stained with either goat anti-rabbit or goat anti-mouse IgG (as appropriate) conjugated to alkaline phosphatase (diluted 1/1,000 from commercial stock with 1% low-fat milk in PBS). Plates were incubated at 37° C. for one hour and washed 3× with PBS/Tween and then stained with substrate (p-nitrophenyl phosphate) at 1 mg/mL in 100 mM diethanolamine with 5 mM MgCl 2 added. Plates were read at 405 nm using a Titertek Multiskan ELISA plate reader. The animals immunized with protein conjugate 14a (KLH long linker) or with protein conjugate 12a (KLH short linker) were assayed against protein conjugate 14b (BSA short linker); likewise animals immunized with either protein conjugate 14b (BSA long linker) or protein conjugate 12b (BSA short linker) were assayed against 14a protein conjugate (KLH long linker).
Capillary Electrophoresis Protocol
Capillary electrophoresis was used to monitor the breakdown of cocaine by separately monitoring the presence of cocaine and its breakdown products, methyl ecgonine and benzoic acid, in the reaction mixture. Using a Beckman P/ACE System 2100 capillary electrophoresis apparatus and a fused silica column (57 cm long) with an internal diameter of 75 μm, all samples were analyzed in either 5 mM or 100 mM borate buffer (pH=8.3). Specimens of cocaine (0.5 mM) were incubated at room temperature with either horse serum ψ-cholinesterase (25 units; Sigma Chemicals), or purified rabbit antibodies. Material was loaded onto the column using low (0.5 psi) pressure injection (4 seconds long) and separated under influence of 24 kV at 25° C. Peaks were read at 200 nm and analyzed using Beckman System Gold software (version 7.01).
Examples 7-10
Preparation of Antisera and Antibodies
Example 7
This Example shows the effect of immunization of mice with the different hapten carrier conjugates.
Twenty BALB/c mice (female; 4-6 weeks old) were each immunized subcutaneously with 50 μg of hapten-conjugates (cf. Table 1 below) in PBS (pH=7.2; 25 μL) emulsified with an equal volume of Freund's complete adjuvant on day 0. All animals were boosted intraperitoneally with an equivalent amount of the corresponding hapten-conjugate emulsified this time with Freund's incomplete adjuvant on day 28. All animals were bled from the retro-orbital plexus on day 42 (2 weeks after boosting) and sera were tested for hapten-specific antibodies by ELISA. The same four different hapten-conjugates, as were used with the rabbits, were tested in each of four different groups of five animals each as summarized in Table 1 below.
FIG. 3 shows graphically the results of the determination by ELISA titration analysis of the level of anti-cocaine analog activity responses in individual mice, with each mouse being indicted by a separate symbol, to immunization by one of the different hapten-carrier conjugates.
The upper panel A illustrates the anti-hapten response to the KLH-long (conjugate 14a) and KLH-short (conjugate 12a) conjugates assayed on the BSA-long (conjugate 14b) conjugate. The lower panel B illustrates the anti-hapten response to the BSA-long (conjugate 14b) and BSA-short (conjugate 12b) conjugates assayed on the KLH-long (conjugate 14a) conjugate.
Collectively, the data presented in FIG. 4 indicate that the cocaine analog hapten-protein carrier conjugates are more effective at inducing anti-hapten responses when the analog is conjugated to the carrier protein by the long linker.
Example 8
This Example shows the effect of immunization of rabbits with the different hapten carrier conjugates.
Eight New Zealand White rabbits (female; 2.5 kg each) were immunized in three sites (one subcutaneous, two intramuscular) with a hapten-conjugate (500 μg) in PBS (pH=7.2; 260 μL), emulsified with an equal volume of Freund's complete adjuvant on day 0. All animals were boosted with an equivalent amount of the corresponding hapten-conjugate emulsified this time with Freund's incomplete adjuvant, again in three different sites (one subcutaneous, two intramuscular) on day 28. All animals were bled from the marginal ear vein on day 42 (two weeks after boosting) and sera were tested for hapten specific antibodies by ELISA. Four different hapten-conjugates were tested, each in two rabbits, as summarized in the following Table 1:
TABLE 1______________________________________Hapten-conjugate Recipients______________________________________14a (KLH long linker) Rabbits #1 & 2; five mice12a (KLH short linker) Rabbits #3 & 4; five mice14b (BSA long linker) Rabbits #5 & 6; five mice14b (BSA short linker) Rabbits #7 & 8; five miceUnimmunized control Rabbit #9; five mice______________________________________
Example 9
This Example illustrates an assay by capillary electrophoresis of the degradation of cocaine by the enzyme ψ-cholinesterase.
Capillary electrophoresis was used to monitor the rate of enzymic degradation by 25 units of horse ψ-cholinesterase (Sigma) of 0.5 mM cocaine at 25° C. in borate buffer pH 8.3 into products of the ester hydrolysis, namely methyl ecgonine and benzoate (Scheme 1, FIG. 2A), by measuring the diminishing area under the cocaine peak and the growing area under benzoate peak. The results obtained are shown in the upper panel A of FIG. 5.
A representative tracing of the capillary electrophoresis pattern for one of these time points illustrated in the lower panel B of FIG. 5.
Example 10
This Example illustrates an assay by capillary electrophoresis of the degradation of cocaine by antibodies from the hapten-conjugate-immunized rabbits.
A capillary electrophoresis analysis of the degradation of cocaine by purified rabbit antibodies isolated from a control unimmunized rabbit and rabbits immunized by the BSA-long conjugate (conjugate 14b), as in Example 8 above. The results obtained are shown in FIG. 6. The upper panel A shows the rate of degradation of 0.5 mM cocaine at 24° C. in borate buffer pH 8.3 for two immunized rabbits and that the breakdown was significantly greater for such rabbits than for the breakdown of cocaine alone in buffer.
In the lower panel B, the immunized rabbit antibodies were also more effective than antibodies from an unimmunized animal, which was not significantly different from buffer alone. These data show that the animals immunized with the BSA-long conjugates of the cocaine analog possessed antibodies which were able to catalyze the breakdown of cocaine.
SUMMARY OF THE DISCLOSURE
While the present invention has been described with reference to specific embodiments thereof, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the true spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation, material or composition of matter, process, process step or steps, or then present objective to the spirit of this invention without departing from its essential teachings.
REFERENCES
1. F. I. Carroll and A. H. Lewin, in Emerging Technologies and New Directions in Drug Abuse Research (R. S. Rapaka, A. Makriyannis, and M. J. Kuhar, Eds.), NIDA Research Monograph #112, Superintendent of Documents, U.S. Government Printing Office, Washington DC 1991, 284-299.
2. K. D. Janda, S. J. Benkovic, and R. A. Lerner, Science 244, 437-440 (1989).
3. S. J. Pollack, P. Hsiun, and P. G. Schultz, J. Am. Chem. Soc. 111, 5961-4962 (1989).
4. N. S. Chandrakumar, C. C. Carron, D. B. Meyer, P. M. Beardsley, S. A. Nash, L. L. Tam, and M. Rafferty, Bioorg. Med. Chem. Lett. 3, 309-312 (1993).
5. D. W. Landry, K. Zhao, G. X.-Q. Yang, M.Gluckman, T. M. Georgiadis, Science 259, 1899-1901 (1993).
6. M. Y. Meah, D. L. Skea, W. A. Corrigall, B. H. Barber, and J. J. Krepinsky, unpublished observations. | Methods are described for the rapid synthesis in satisfactory yield of methyl ecgonine phenylphosphonates as analogues of transition states for the hydrolysis of the benzoyl ester of an ecgonine derivative, namely cocaine, and their linking to carrier proteins, for the purpose of using them as immunogens. The resulting immunogens elicit the formation in experimental animals of antibodies able to promote the hydrolysis of cocaine. Both these catalytic anti-cocaine antibodies and the immunogens themselves are potentially useful for the treatment of individuals seeking to avoid the pharmacological effects of cocaine and in diagnostic applications. | 0 |
This is a divisional of application Ser. No. 08/010,898, filed on Jan. 29, 1993, U.S. Pat. No. 5,336,813, which is a Continuation of Ser. No. 07/611,562, filed Nov. 13, 1990, now abandoned. su
BACKGROUND OF THE INVENTION
The dihydric phenols have achieved significant success in their commercial applications. Dihydric phenols are useful in the commercial manufacture of various polymers including the polyarylates, polyamides, epoxies, polyetherimides, polysulfones and the polycarbonates. Significant attention has been directed to the commercial preparations of the dihydric phenols. For many years it has been well known that the acid catalyzed taction of phenol with specific aldehyde or ketone could prepare the 4,4'-dihydric phenol with specific groups derived from the aldehyde or the ketone connecting the two phenolic rings. In particular when phenol is reacted with acetone, the dihydric phenol 4,4'(hydroxyphenyl)propane-2, hereafter known as bisphenol-A is formed. This has particular utility in polycarbonates, polyarylates and copolyestercarbonates as well as epoxies. In order to make certain polymers, in particular the polycarbonates, the bisphenol-A must be particularly pure, for example, as measured by color. Additionally, the process should be particularly efficient since the dihydric phenol costs contribute substantially to the cost of the final polymer. Therefore much attention has been directed to the recovery of bisphenol-A after preparation. Not only is recovery from the major stream containing primarily bisphenol-A important, but because of the economics involved, various side streams or "purge streams" also contain significant quantities of bisphenol-A and should also be processed in manners which maximize bisphenol-A recovery.
Various catalytic systems for acid catalysis of the reaction between phenol and acetone have been investigated and used commercially. At one time the hydrochloric acid catalyzed process was used in a significant number of commercial facilities. However the corrosion caused by the hydrochloric acid on standard metallic reactors and pre and post reaction equipment left much to be desired as far as replacement economics was concerned. Recently, substantial attention has been placed on using an ion exchange resin catalyst system since it does not have significant acid corrosion problems.
Various tactics have been utilized to maintain the quality and quantity of bisphenol-A which has been recovered from the acidic ion exchange resin catalyzed reaction of phenol and acetone. U.S. Pat. No. 4,847,433 utilizes a carbonate system, specifically the alkaline earth and transition metal oxidation number plus two salts of carbonates, to stabilize the bisphenol-A so that significant quantities of quality bisphenol-A can be recovered from various streams. It was thought that the specific acidic material that was being counteracted by the addition of the carbonate salts were minute quantities of strong acid oligomers which were being leached from the resin catalyst during the processing. It was noted that such carbonate salts should not be recycled to the catalyst system since they would very well bring about eventual neutralization of the catalyst system.
U.S. Pat. No. 4,894,486 specifically states that the presence of metal ions is also thought to have an adverse effect on the color of bisphenols probably by promoting degradation. The British Patent 890432 is then cited to show that various other additives have been employed to inhibit the formation of degradation products of the bisphenols. Thus, alkaline earth phosphates, stannic oxide and oxylate, a mixture of tin powder and tin dioxide, terephthalic and isophthalic acids, oxalic, sebacic and adipic acids and boron or antimony trioxides and their mixtures are taught as useful additives for providing thermal stabilities to bisphenols. Additionally in British Patent 890432 is mentioned the concept of utilizing a neutral or amphoteric compound or compound of weakly acidic character and possibly also possessing the property of forming complexes with metallic ions and ability to react with alkaline reacting impurities in the bisphenols is also mentioned. A further British Patent 1022583 teaches that improved color stability of bisphenols is provided by the incorporation of oxalic, citric or tartaric acids or their alkali metal or ammonium salts during a bisphenol manufacturing process. They may be added with the reactants or after the reaction is complete but before the bisphenol is separated from the reaction mixture. The British patents disclose acidic conditions for preparing bisphenol-A but no mention of acid ion exchange resin catalysis is mentioned.
Recently, U.S. Pat. No. 4,894,486 disclosed the use of the hydroxy acids lactic, malic and glyceric and their ammonium or alkali metal salts as stabilizers for bisphenols. No particular preparation of the bisphenol-A was employed and the only examples utilized the acid per se and measured the APHA color before and after heat treatment.
Weakly basic anion exchange columns have also been utilized to contact bisphenol containing fluids. In U.S. Pat. No. 4,191,843, a weakly basic anion exchange resin is used to contact reactor effluent obtained from an acid ion exchange resin catalyst. Instead of the weakly basic anion exchange resin, strongly acidic ion exchange resin in its salt form can also be used. U.S. Pat. No. 4,766,254, utilizes a weakly basic anion exchange resin to contact the mother liquor of bisphenol-A phenol adduct. Additionally salts of nitric, sulfuric and phosphoric acid (NaH 2 PO 4 ) have been used as bisphenol stabilizers, see Japan 61 12639 and Japan 61 12640. A recent European patent application, EPA 329 075 discloses the use of a polyvinyl pyridine anion exchange column to stabilize bisphenols.
As can be seen from this virtual potpourri of prior art there is very little distinction given to the types of impurities which are being addressed in the manufacturing process of bisphenols, particularly bisphenol-A. The fact that any of acids, salts of acids, certain bases or basic ion exchange resins can be used indicates that both alkaline and acidic impurities are being removed. Therefore there is no real directing nature to the prior art.
It is now been found that when utilizing an acidic ion exchange resin to catalyze a reaction between a phenol and a ketone to produce a bisphenol, particularly phenol and acetone to produce bisphenol-A, it is very advantageous to contact the desired bisphenol produced prior to significantly elevated temperatures such as distillation to separate bisphenol-A from various impurities including phenol as well as the separation of bisphenol-A from bisphenol-A phenol adduct, with certain amines. These amines are selected so they have a boiling point above that of the phenol used in the process. In this manner significant stabilization of the bisphenol, particularly bisphenol-A, is achieved when the bisphenol is subjected to a heat treatment, for example distillation of phenol or the bisphenol or separation from its adduct of bisphenol with phenol. Degradation is significantly inhibited as shown by the substantial quantity of bisphenol which is capable of recovery. Additionally reduced color of the bisphenol is often observed when salts of the acid of this invention are in contact therewith.
SUMMARY OF THE INVENTION
In accordance with the invention, there is a process comprising the addition of a degradation inhibiting effective amount of an amine having a boiling point above that of the phenol used in the process, to a composition comprising a phenol and a bisphenol the addition occurring prior to a procedure which subjects the bisphenol to substantial heat, said bisphenol produced from an acid ion exchange catalyzed reaction of a phenol and a ketone or aidehyde.
A further aspect of the invention is a composition comprising phenol and a bisphenol in admixture with a bisphenol degradation inhibiting effective amount of an amine having a boiling point above that of the phenol.
DETAILED DESCRIPTION OF THE INVENTION
The bisphenol, particularly bisphenol-A, is made by the standard acid catalyzed reaction of a phenol and an aldehyde or ketone. When preparing bisphenol-A, the phenol is phenol and the ketone is acetone. An acidic catalyst is used to increase the efficiency of the reaction. This catalyst system is preferably in the heterogeneous form, that is as an ion exchange resin in its acidic form. The problems using a homogeneous catalyst system such as hydrochloric acid are well known and should be avoided. The ion exchange resin can be for example an Amberlite type resin obtained from Rohm and Haas. This resin has styrenic backbone with pendant SO 3 H groups which provide the acidic character to the resin. Usually the styrene is crosslinked with a small quantity of divinyl benzene or other crosslinking chemical. This addition of a crosslinker appears to provide structural strength and rigidity to the catalyst. Other ion exchange resins can also be used although it is preferable to use the styrenic backbone crosslinked with the difunctional monomer and having SO 3 H groups pendant from the aromatic nucleus of the styrene moiety. The use of these ion exchange resins can bring about certain problems not previously observed with a homogeneous acidic catalyst system. Increased color of the bisphenol-A as well as loss of bisphenol-A during certain heat treatments such as distillation and/or bisphenol-A phenol adduct melting and separation were found to occur.
The group of compounds which inhibit the degradation of the bisphenol is an amine having a boiling point higher than the phenol used in the process. By having the higher boiling point than the phenol, the unreacted amines are present but are not passed back with recycle phenol to the original condensation catalyst wherein neutralization of that acidic catalyst system could rapidly occur. Such unreacted amine and any salt formed during a neutralization is rather passed along with the bisphenol product stream and surprisingly does not seem to cause any undesirable effects. In fact wherein the bisphenol is used in further processing involving the preparation of polymer using an amine catalyst system, for example the interfacial polymerization of aromatic polycarbonate from bisphenol and carbonate precursor, amine is common to the system and is removed at an appropriate point.
Usage of such amines have advantages over other materials used, particularly the carbonates, specifically barium carbonate. Generally the amine has improved solubility in phenolic solutions and water compared to metal carbonates. This provides more efficient use of the additive and the option to easily add the material as a liquid solution rather than a solid powder. Additionally there is no major toxicity problem associated with the amine as there is with the metallic carbonates, particularly barium carbonate.
These salts can be added to the process of preparing the bisphenol prior to any substantial heat treatment for maximum effect. Examples of such heat treatment include distillation, melting the adduct of bisphenol and phenol and like elevated temperature treatments.
As stated previously, the amines should have a boiling point which is significantly higher than the phenol being used. This allows for a substantial separation of the phenol and amine upon distillation of the phenol and allows for the amine to be separated with the bisphenol. When utilizing phenol per se, B.P. 182° C. the following amines are examples of those amines which are effective in the process.
______________________________________Amine B.P. °C.______________________________________p-phenylene diamine 267N,N-diethylaniline 217tributylamine 216N,N-dimethylaniline 193hexamethylene diamine 200tridodecylamine 220-228 @ 0.03 mm Hgdioctylamine 298diphenylamine 3024-dodecylaniline 220 @ 15 mm Hgtrioctylamine 3654-methylbenzylamine 195______________________________________
The amines are preferably either liquid at the process stream temperature or at least substantially soluble in the process stream.
A stabilizing effective or degradation effective amount of the compound(s) should be employed. Generally an effective amount of from about 1 to about 1000 ppm based upon the bisphenol present in the stream is efficient. Below this quantity, effectiveness is difficult to observe. Above this quantity, no additional beneficial results are generally observed. Preferred quantities are generally from about 10 to about 500 ppm can also be employed as well.
Below are examples of the invention. These examples are intended to illustrate and exemplify but not narrow the invention.
EXAMPLES
Bisphenol-A is prepared from the strong acid ion exchange resin catalyzed reaction of acetone and phenol. Lewatit, ion exchange resin from Mobay is used. This is a sulfonic acid substituted cross linked polystyrene. The bisphenol-A is separated as bisphenol-A phenol adduct. Approximately 250 grams of mother liquor of bisphenol-A phenol adduct was placed in a 500 ml pot. The quantity of bisphenol-A present in the mother liquor was analyzed by high pressure liquid chromotography.
The pot is heated with the reflux condenser off and the phenol is collected over head until the pot temperature Irises to 210° C. At that point, the reflux condenser water flow is initiated and the solution is allowed to reflux for four hours. A nitrogen blanket was not used to allow air/oxygen contact during the test.
At the end of four hours, the pot residue is again analyzed by high pressure liquid chromatography to determine the weight of bisphenol-A remaining. This is the control.
The same procedure is carried out as above; however 500 ppm of additive based upon the weight of solution was added to the pot together with the mother liquor. The final quantity of bisphenol-A was reported after four hours of refluxing. Below are the results reported as percent loss of BPA from the initial quantity. 0% loss is total inhibition of degradation.
______________________________________ % Loss % LossAdditive Control Experimental______________________________________1-adamantamine 36.3 0N,N-dimethylaniline 15.4 0Tributylamine 16.6 0______________________________________ | A process comprising the addition of a degradation inhibiting effective amount of an amine having a boiling point above that of the phenol used in the process to a composition comprising the said phenol and a bisphenol, the addition occurring prior to a procedure which subjects the bisphenol to substantial heat, said bisphenol produced from an acidic ion exchange resin catalyzed reaction of the said phenol and a ketone or aldehyde. | 2 |
RELATED APPLICATIONS
The present application is related to U.S. Provisional patent application Ser. No. 60/224,106 filed on Aug. 9, 2000.
GOVERNMENT SPONSORED RESEARCH
The U.S. Government has a paid-up license in this invention and the right in limited circumstances to require the patent owner to license others on reasonable terms as provided for by the terms of Grant No. N00014-99-1-0972 awarded by the Office of Naval Research.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a peristaltic micro-pump fashioned in the column III-nitride material system as well as the broad processing technology used to fabricate suspended micro-devices in this same material system.
2. Description of the Prior Art
In designing the driving system of a biochip, three approaches have been used in the prior art. They are the on-chip mechanical micropump, the on-chip electro-kinetic micropump and the external servo system. An on-chip mechanical micropump may be prepared directly by the micro-machining technology. If this approach is adopted, a moveable part is provided inside the microchannel of the chip. The “electrostatically driven diaphragm micropump” shown by Roland Zengerle et al. in their U.S. Pat. No. 5,529,465 is a typical example. In the Zengerle device, the micropump includes a pressure chamber. Reciprocal pumping power is generated by electrostatics. With the help of two passive check valve, microflows are driven with a 350 mμl/min working velocity.
A simplified “micromachined peristaltic pump” was disclosed by Frank T. Hartley in U.S. Pat. No. 5,705,018. In this device, a series of block flexible conductive strips are positioned in the internal wall of a microchannel. When a voltage pulse passes along the microchannel, the flexible conductive strips are uplifted in sequence by the electrostatics so generated, such that a peristaltic movement is generated. This peristaltic movement drives the microflow along the microchannel. In the Hartley device, the working velocity is about 100 mμ/min.
The on-chip mechanical micropump does not provide the function such that the chip may be repeatedly used for different samples. This is because a microchannel with moveable parts is difficult to clean up residual samples or biochemical reagents after the reaction. Another problem is that the on-chip mechanical micropump, especially the peristaltic pump, involves expensive material costs. These biochips are not suited for disposable applications.
Micro-fluidic pumps fabricated in Column III-nitride materials offer several advantages over existing implementations. For one, Column III-nitride materials offer high chemical inertness and high temperature stability, making the micropumps suitable for harsh or corrosive environments. In addition, these micropumps can be readily integrated on a single chip with the broad spectrum of opto-electronic, high speed and high power devices possible in the Column III-nitride semiconductors. As described below, these micropumps employ a comparatively simple and reliable pumping mechanism. Furthermore, they are fabricated from a versatile processing technology which enables a broad range of device layouts for superior microscopic fluid control.
BRIEF SUMMARY OF THE INVENTION
The invention is a versatile processing technology for the fabrication of micro-electromechanical systems in GaN. This technology, which is an extension of conventional photo-electrochemical (PEC) etching, allows for the controlled and rapid undercutting of p-GaN epilayers. The control is achieved through the use of opaque metal masks to prevent etching in designated areas, while the high lateral etch rates are achieved by biasing the sample relative to the solution. For GaN microchannel structures processed in this way, undercutting rates in excess of 30 μm/min have been attained.
The invention is illustrated in the fabrication of a micropump comprising an electro-deformable membrane and a substrate disposed below the membrane and coupled thereto. A microchannel is defined between the membrane and substrate. The microchannel is formed so as to have a longitudinal axis. An electrode structure is disposed on at least one side of the membrane along side of the microchannel.
The electro-deformable membrane is bowed to form a curvature having a symmetrical axis in the direction of the longitudinal axis of the microchannel.
The micropump further comprises a drive circuit coupled to the electrode structure to apply a sequential voltage along the plurality of opposing electrodes to peristaltically deform the electro-deformable membrane in the direction of the longitudinal axis of the microchannel.
In the illustrated embodiment the electro-deformable membrane is composed of p-type GaN, but any material having the same or similar electro-deformable properties may be employed.
The micropump further comprises two opposing pillars disposed on the substrate between the substrate and the membrane generally aligned in the direction of the longitudinal axis. The two opposing pillars are composed of n-type GaN.
The electrode structure is comprised of two opposing electrode substructures extending parallel to the microchannel. The two opposing electrode substructures each comprise a plurality of discrete electrodes arranged and configured to provide pairs of opposing electrodes on each side of the microchannel. Many equivalent electrode structures to a series of opposing electrodes may be used, including propagation line electrodes in which a traveling wave potential may be placed. It may also be possible for a single electrode rail to be provided to provide the traveling wave potential with the opposing side of the membrane left to float or grounded by an opposing rail or any other conductive means.
The invention is also characterized as a method of micropumping comprising the steps of providing a bowed electro-deformable membrane disposed above a substrate and coupled thereto so that a microchannel is defined between the membrane and substrate. A traveling wave potential is propagated along the electro-deformable membrane in the direction of the longitudinal axis. As a consequence, the electro-deformable membrane is peristaltically deformed by the traveling wave potential and hence fluid is pumped in the microchannel along the longitudinal axis.
The step of providing a traveling wave potential comprises the step of applying a potential across the electro-deformable membrane traverse to the longitudinal axis and sequentially applied along the longitudinal axis. More specifically, in one embodiment the step of providing a traveling wave potential comprises sequentially applying a plurality of discrete potentials across the electro-deformable membrane traverse to the longitudinal axis.
The step of providing a bowed electro-deformable membrane comprises providing p-type GaN membrane and two opposing pillars composed of n-type GaN under the p-type GaN membrane to anchor and space the membrane apart from an underlying substrate. The illustrated method of making the bowed electro-deformable membrane comprises the step of forming the n-type GaN pillars and the p-type GaN membrane by selectively photo-electrochemical etching two adjacent n-type GaN and p-type GaN layers.
In general the step of providing a traveling wave potential is provided by an electrode structure of two opposing electrode substructures extending parallel to the microchannel. The electrode substructures may be continuous or discrete. In the illustrated embodiment the traveling wave potential is supplied by the two opposing electrode substructures comprises across a plurality of discrete electrodes which are arranged and configured to provide pairs of opposing electrodes on each side of the microchannel.
While the apparatus and method has or will be described for the sake of grammatical fluidity with functional explanations, it is to be expressly understood that the claims, unless expressly formulated under 35 USC 112, are not to be construed as necessarily limited in any way by the construction of “means” or “steps” limitations, but are to be accorded the full scope of the meaning and equivalents of the definition provided by the claims under the judicial doctrine of equivalents, and in the case where the claims are expressly formulated under 35 USC 112 are to be accorded full statutory equivalents under 35 USC 112. The invention can be better visualized by turning now to the following drawings wherein like elements are referenced by like numerals.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified diagram of the principle parts of a GaN pump devised according to the invention.
FIGS. 2 a - 2 d are computer simulation perspective net drawings of the membrane in isolation of other elements of the pump shown in a time sequence to illustrate the peristaltic pumping action.
FIG. 3 a is a scanning electron microscopic photograph of a side view of a GN micro-pump of the invention, wherein the shaded region corresponds to the micro-channel for fluid flow.
FIG. 3 b is a scanning electron microscopic photograph which shows an enlarged view of a section of the bowed 1.2μ p-GaN membrane.
FIG. 3 c is a scanning electron microscopic photograph of a top plan view along the channel of a GaN micro-pump. On the left the dark strip running down the center corresponds to the suspended p-GaN film. On the right, a voltage has been applied across the channel causing the membrane to actuate or deflect. The direction of fluid flow is vertical in the images.
FIGS. 4 a - 4 e are simplified cross-sectional side view of one methodology whereby the membrane of the invention may be fabricated.
The invention and its various embodiments can now be better understood by turning to the following detailed description of the preferred embodiments which are presented as illustrated examples of the invention defined in the claims. It is expressly understood that the invention as defined by the claims may be broader than the illustrated embodiments described below.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In recent years, gallium nitride has established its place in the arena of solid-state devices, with applications ranging from light-emitting diodes and visible-blind photodetectors to high power Shottky diodes and ultra-fast high electron mobility transistors (HEMTs). Several material properties of GaN also make it a promising candidate for micro-electromechanical (MEMS) applications. Among the properties which set it apart from silicon, the conventional choice for MEMS, is its large piezoelectric response. This response would provide a powerful means for the excitation and detection of acoustic waves in micro-resonators. In addition, the strong piezoresistive effect in p-GaN is ideal for electrical strain sensing in micro-positioners. Furthermore, chemical inertness and high temperature stability make GaN a suitable choice for MEMS applications in harsh environments. Transparency to visible wavelengths also allows it to feature in optical micro-switches and waveguides. The methodology of the invention allows for the fabrication of a diverse range of suspended GaN microstructures.
The disclosed process exploits the dopant selectivity of photo-electrochemical (PEC) etching to undercut p-GaN layers grown on sacrificial n-GaN layers. PEC etching of GaN is achieved by exposing it to above bandgap radiation while immersed in an aqueous KOH solution. It is believed that band-bending at the n-GaN/electrolyte interface causes photogenerated holes to be swept toward the surface where they participate in the chemical dissolution of the semiconductor. In p-GaN, the bands bend in the opposite sense, creating a barrier for hole migration to the surface. Undercutting of p-GaN layers has also been observed and recently studied using backside illumination through the sapphire substrate. The fabrication of complex microstructures in GaN, however, requires that the undercutting be precisely controlled and optimized. First, etching must be prevented in regions of the n-type underlayer designed to provide mechanical anchoring for the p-type membrane above. Furthermore, for structures with a large undercut span, the lateral etch rate must be high to achieve a practical total etch time.
Photo-electrochemical etching (PEC) of column III-nitride (GaN, AlN, InN and their ternary alloys) can be used according to the methodology of the invention to fabricate a variety of micro-electromechanical devices, including but not limited to the micropump described above. For GaN, the PEC etching process is achieved by exposing the material to above bandgap UV radiation (<365 nm) in an aqueous etchant solution. Under these conditions, n-type doped GaN etches rapidly, while p-type GaN remains unaffected. This dopant selectivity of PEC etching, combined with the UV light sensitivity, allows for the fabrication of p-GaN suspended microstructures as illustrated in greater detail below in connection with FIGS. 4 a - 4 e.
FIG. 4 a is a side cross-sectional view of the beginning step of the method wherein a sapphire substrate 11 is provided. A sacrificial n-GaN base layer 13 is formed on substrate 11 as illustrated in FIG. 4 b . A thin p-GaN layer or membrane 12 is grown epitaxially on sacrificial n-GaN base layer 13 as also shown in FIG. 4 b . During the PEC process illustrated in FIGS. 4 a - 4 e , a portion of n-GaN base layer 13 is selectively undercut or etched away, leaving the upper p-GaN membrane 12 freely suspended. This suspended membrane 12 is formed as follows. A patterned opaque metal mask 22 is deposited on the p-GaN over-layer 12 and is used to prevent UV exposure in certain areas of n-GaN base layer 13 during the etch step in FIG. 4 d . This allows masked regions of the n-GaN base layer 13 to be locally protected from etching in order to leave structural support or pillars 14 for the thin p-GaN film 12 above. Large p-GaN areas can be undercut in this way, with lateral etch rates approaching 100 mm/min.
FIG. 4 d shows the salient features of the etch setup used for controlled undercutting. In the illustrated embodiment, p-on-n bilayer samples 12 , 13 were immersed in 0.1 M KOH and exposed from the front side by a Xenon arc lamp (not shown) with 100 mW/cm 2 in the UV. Prior to the PEC etch, opaque metal masks 22 (Ni/Au—80 nm/20 nm) were patterned onto the samples and then annealed at 500° C. for 5 minutes in Ar to prevent peeling in the corrosive bath. As indicated in the FIG. 4 d , we observed that the n-type epilayer 13 does not etch in the areas immediately below the masks 22 . However, masked regions near the outermost periphery of overlayer 12 undercut very slowly as a result of stray UV radiation that is reflected back through the sapphire substrate 11 directly into the n-GaN layer 13 . To suppress this reflection, the samples 12 , 13 were suspended in solution by a Ni wire epoxied near the side. This problem can be effectively eliminated by using backside polished substrates with a thin SiO 2 anti-reflection coating.
The Ni wire also served as an electrical contact to the p-GaN overlayer 12 during the PEC etch step. It was maintained at a positive 1.5 V bias with respect to a Pt cathode 15 in solution 17 . The application of this bias was seen to dramatically accelerate the undercutting of the unmasked p-GaN areas 13 , with lateral etch rates in excess of 30 μm/min being observed for certain geometries. The origins of this marked increase in etch rate are not well understood at this time. However, observations of the undercutting dynamics suggest that the sample bias gives rise to drift currents of the electrolyte within the narrow etched channels under the p-GaN film 12 . We suspect these currents deliver chemically active OH − radicals to the etch front much more efficiently than diffusion alone.
What results is the microchannel 20 shown in FIG. 4 e which is described in greater detail below. An example of one of the devices that are possible with this processing technology is a micro-fluidic pump 10 depicted in the perspective view of FIG. 1 . The pump 10 is comprised of a p-GaN membrane 12 suspended between two opposing, parallel n-GaN support pillars 14 which are anchored to a rigid substrate 16 below pillars 14 . As depicted in FIG. 1, the p-GaN membrane 12 bows upward between the rigid support pillars 14 to relieve compressive strain in the film resulting from the original epitaxial growth process. This bowing substantially increases the volume of the enclosed micro-channel 20 defined between membrane 12 and substrate 16 below. The amount of bowing and the strain developed in membrane 12 can be varied according to conventional means to assume a wide variety of values. The termination of the longitudinal ends of microchannel 20 may be completed in any one of a number of ways using conventional micromaching techniques, such as chemically assisted ion beam etching (CAIBE), all of which are considered equivalent for the purposes of the present invention. Opposing sets of metallic contact pads 18 a and 18 b can then be patterned above the support pillars on the upper surface of p-GaN membrane 12 using standard lithographic techniques. These metal pads provide electrical contact to the micro-channel for the purpose of electro-actuation of the pump.
The micropump having now been described in general terms, consider the fabrication of the suspended membrane 12 of FIG. 1 in greater detail. An example of the diverse microstructures which can be realized using this etch process is the GaN microchannel shown in FIG. 1 . The microchannel 20 is comprised of an 1 μm thick p-GaN membrane 12 that spans between two long anchoring strips 14 on either side. To fabricate this structure, a series of Ni/Au bars (not shown, but later divided into pads 18 a and 18 b ) with 100 μm spacing between the bars across was to become channel 20 were patterned on a p-on-n bilayer sample 12 , 13 using standard lithographic techniques. The sample was then exposed to the PEC etch described above, during which the unmasked regions between the bars were undercut. Etching of n-GaN underlayer 13 proceeded inward from both sides in the direction of the bars. A total undercut channel length of 5 μm etched to completion in roughly 2 hours. Afterward, the metal masks were removed in places, leaving a series of isolated contact pads 18 a and 18 b along the anchored sidewalls.
The GaN layers 13 used here were grown by molecular beam epitaxy on c-plane sapphire 11 with no buffer layer. Both the n+ (Si) and the p+ (Mg) epilayers are 1 μm thick, and the growth temperature in each case was 800° C. and 700° C. respectively. Both layers are thought to have carrier concentrations in the range of 10 18 /cm 3 .
The surface quality of the p-type film 12 does not appear to degrade as a result of the lengthy PEC etch. Furthermore, the underside of the suspended p-GaN film 12 is smooth and featureless. This is in marked contrast to our observations of MOCVD grown p-on-n samples, for which the undersides are rough and coated with etch-resilient whiskers.
As seen in FIG. 1, the p-GaN membrane 12 bows upward after release to relieve inherent stress. A maximum vertical deflection of 9.2 μm is measured at the center of the 100 μm channel width. We believe the primary origin of this stress is the thermal mismatch between the GaN epilayer 13 and the sapphire substrate 11 , integrated down from growth temperatures. Measurements of the expanded length of the bowed film correspond to a biaxial compressive strain of 1.0×10 −3 in the p-GaN layer prior to release. However, we have observed strong evidence that the stress profile in the p-layer 12 is far more complicated: p-GaN cantilever structures relax into a shape which is uniformly curved away from the substrate 11 . This bending suggests there are vertical stress gradients in the p-layer 12 , perhaps built in at the time of growth as a result of the different lattice constants for Mg and Si doped GaN.
Consider now the method of operating the pump of FIG. 1 . By applying a voltage across a pair of opposing metal contacts 18 a and 18 b , membrane 12 can be made to flatten locally in the intervening region between pillars 14 . Sequential actuation of membrane 12 in this manner will induce a peristaltic wave motion along the length of device 10 , as depicted in FIGS. 2 a - 2 b - 2 c - 2 d , which are computer simulation perspective net drawings of membrane 12 in isolation of other elements of pump 10 shown in a time sequence. FIG. 2 a shows membrane 12 in equilibrium without any applied voltage to it. The remaining images of FIGS. 2 b - 2 d show membrane 12 actuated at successive points along its length by sequential application of a voltage to opposing pairs of contacts 18 a and 18 b along the edges of membrane 12 . A constriction of membrane 12 can be seen in the sequence of FIGS. 2 a - 2 d moving from left to the right end of membrane 12 as seen in the view of the drawings. This wave motion can be used to pump fluids down the length of the micro-channel 20 with a peristaltic wave motion.
Several GaN micro-pumps have been successfully fabricated and tested with varying channel widths and lengths. FIG. 3 a is a scanning electron-microscope perpendicular cross-sectional side-view image of a pump 10 with no applied bias. FIG. 3 b is an enlarged cross-sectional side-view image of a portion of FIG. 3 a . The width of the channel measured between pillars 14 is 200 μm, and the maximum vertical deflection of the p-GaN membrane 12 above the substrate 16 is 10 μm.
Optical microscope images of a top plan view along the length parallel to pillars 14 of device 10 of FIG. 3 a are displayed in FIG. 3 c with the bowed p-GaN membrane 12 viewed from above. On the left half of FIG. 3 c , the membrane 12 is in equilibrium without external bias. On the right half of FIG. 3 c a voltage is applied across the channel 20 has caused membrane 12 to flatten locally. With the aid of a conventional timing circuit to apply voltage sequentially along the longitudinal length of channel 20 , peristaltic motion has been successfully demonstrated in these devices. For the channel depicted in FIG. 3, the voltage required to cause full constriction of the membrane is approximately 20 V. At a fixed point along the longitudinal axis, a complete actuation cycle can be performed at a maximum rate of 100 Hz. With a spacing of 100 μm between contact pads along the longitudinal axis, the peristaltic wave velocity down the channel is roughly 1 cm/s. The corresponding pumping capacity of the channel in FIG. 3 is 0.01 μL/s.
Thus, it can now be readily understood that the versatile PEC processing methodology can be used to create either p or n type nitride suspended membranes of variable bowing or curvature for use in a wide variety of microdevices of which the micropump 10 is only one of a myriad of possibilities. It is to be expressly understood that the method of making the nitride suspended membrane is generally applicable as a fabrication technique for the manufacture of a membrane element in any device now known or later devised.
GaN micro-pump 10 provide a technologically convenient way to control fluid motion in microscopic channels 20 . These pumps 10 could find application in a large range of settings, wherever peristaltic pumping of fluid in a microfluidic device or hydraulic circuit is needed, including without limitation fuel cells, water filtration, blood regulation, and micro-chemical analysis devices.
Many alterations and modifications may be made by those having ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, it must be understood that the illustrated embodiment has been set forth only for the purposes of example and that it should not be taken as limiting the invention as defined by the following claims. For example, notwithstanding the fact that the elements of a claim are set forth below in a certain combination, it must be expressly understood that the invention includes other combinations of fewer, more or different elements, which are disclosed in above even when not initially claimed in such combinations.
The words used in this specification to describe the invention and its various embodiments are to be understood not only in the sense of their commonly defined meanings, but to include by special definition in this specification structure, material or acts beyond the scope of the commonly defined meanings. Thus if an element can be understood in the context of this specification as including more than one meaning, then its use in a claim must be understood as being generic to all possible meanings supported by the specification and by the word itself.
The definitions of the words or elements of the following claims are, therefore, defined in this specification to include not only the combination of elements which are literally set forth, but all equivalent structure, material or acts for performing substantially the same function in substantially the same way to obtain substantially the same result. In this sense it is therefore contemplated that an equivalent substitution of two or more elements may be made for any one of the elements in the claims below or that a single element may be substituted for two or more elements in a claim. Although elements may be described above as acting in certain combinations and even initially claimed as such, it is to be expressly understood that one or more elements from a claimed combination can in some cases be excised from the combination and that the claimed combination may be directed to a subcombination or variation of a subcombination.
Insubstantial changes from the claimed subject matter as viewed by a person with ordinary skill in the art, now known or later devised, are expressly contemplated as being equivalently within the scope of the claims. Therefore, obvious substitutions now or later known to one with ordinary skill in the art are defined to be within the scope of the defined elements.
The claims are thus to be understood to include what is specifically illustrated and described above, what is conceptionally equivalent, what can be obviously substituted and also what essentially incorporates the essential idea of the invention. | A suspended p-GaN membrane is formed using photochemical etching which membrane can then be used in a variety of MEMS devices. In the illustrated embodiment a pump is comprised of the p-GaN membrane suspended between two opposing, parallel n-GaN support pillars, which are anchored to a rigid substrate below the pillars. The p-GaN membrane bows upward between the pillars in order to relieve stress built up during the epitaxial growth of membrane. This bowing substantially increases the volume of the enclosed micro-channel defined between membrane and substrate below. The ends of membrane are finished off by a gradual transition to the flat underlying n-GaN layer in which fluidic channels may also be defined to provide inlet and outlet channels to microchannel. A traveling wave or sequential voltage applied to the electrodes causes the membrane to deform and provide a peristaltic pumping action in the microchannel. | 5 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to computer processors and, more particularly, to queuing and writing store data to cache.
[0003] 2. Description of the Related Art
[0004] Microprocessors have evolved to include a variety of features aimed at improving the speed and efficiency with which instructions are executed. In addition to advances in clock speed and the resulting reduction in instruction execution time, microprocessors may include pipelines, multiple cores, multiple execution units, etc. that permit some degree of parallel instruction execution. Further performance improvements have also been realized through a variety of buffering, queuing, and caching features intended to overcome bottlenecks in the movement of data to and from memory. For example, microprocessors often include multiple memory caches, arranged hierarchically and shared by multiple cores or execution units. Since, cache accesses are faster than memory accesses, various caching techniques are used to increase the likelihood that data is located in a cache when needed by a core or execution unit.
[0005] When multiple cores share memory or cache space, it is necessary to coordinate loading and storing of data in caches and in the shared memory so that a globally consistent view of the data at each location is maintained. For instance, it may be necessary for a given core to obtain exclusive access to a shared memory location before storing cached data in it. In the case where each core has its own level-1 cache but uses a shared, level-2 cache, a similar problem may exist. It may be advantageous to temporarily store data in one or more buffers or queues until exclusive access is obtained in order to permit the core to process additional instructions instead of waiting for the store operation to be completed.
[0006] One approach used to address the above concerns is for each core to have a store queue. A store queue may buffer memory operations that have been executed, but not yet committed to cache or memory. Memory operations that write data to memory may be referred to more succinctly herein as “stores”. A store may target a particular cache line (or portion of a cache line) and include an address identifying the targeted line as well as including data to be stored within the cache line. In order to improve performance, modern microprocessor cores may execute instructions out-of-order or speculatively. These techniques create a need for stores to be held until the order in which they should be presented to memory is determined and exclusive access to the targeted memory location is granted. Once the order of commitment is determined, the store may be retired. A store queue may be used to hold stores until they are retired, after which they may be committed to cache or to memory when exclusive access to the targeted memory location is granted. Moving store operations to the store queue permits a core's instruction execution pipeline to be used to execute other, subsequent instructions. However, even though queuing stores decouples a core from the operations of retiring stores and acquiring exclusive access to memory, a core may still stall if the store queue becomes full. In order to address the above concerns, what is needed is a way to reduce the chances of a store queue becoming full and stalling its associated processor core.
SUMMARY OF THE INVENTION
[0007] Various embodiments of a processor and methods are disclosed. The processor includes at least a first processing core. The first processing core includes a memory cache, a store queue, and a post-retirement store queue. The first processing core is configured to retire a first store in the store queue and convey the first store to both the memory cache and the post-retirement store queue, in response to retiring the first store. In a further embodiment, at least one of the store queue and the post-retirement store queue is a first-in-first-out queue.
[0008] In a still further embodiment, to convey the first store to the memory cache, the first processing core obtains exclusive access to a portion of the memory cache targeted by the first store. The first processing core buffers the first store in a coalescing buffer and merges with the first store, one or more additional stores and/or loads targeted to the portion of the memory cache targeted by the first store prior to writing the first store to the memory cache.
[0009] In another embodiment, the processor further includes a second processing core and a shared memory shared by the first and second processing cores. The memory cache comprises a level-1 cache and the shared memory comprises a level-2 cache. The first processing core conveys the first store from the post-retirement queue to the shared memory. To convey the first store from the post-retirement store queue to the shared memory, the first processing core obtains exclusive access to a portion of the shared memory targeted by the first store.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a generalized block diagram of one embodiment of a computer system.
[0011] FIG. 2 is a detailed block diagram of one embodiment of store logic.
[0012] FIG. 3 illustrates one embodiment of a process that may be used to operate a store queue.
[0013] FIG. 4 illustrates one embodiment of a process that may be used to remove a series of stores from a store queue after retirement.
[0014] FIG. 5 illustrates one embodiment of a process that may be used to coalesce a series of stores.
[0015] While the invention is susceptible to various modifications and alternative forms, specific embodiments are shown by way of example in the drawings and are herein described in detail. It should be understood, however, that drawings and detailed descriptions thereto are not intended to limit the invention to the particular form disclosed, but on the contrary, the invention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the present invention as defined by the appended claims.
DETAILED DESCRIPTION
[0016] FIG. 1 is a generalized block diagram of one embodiment of a computer system 100 . A variety of other embodiments are also contemplated. In the illustrated embodiment, processor 110 is shown coupled to peripherals 120 and to a memory 130 . Peripherals 120 may include any of a variety of devices such as network interfaces, timing circuits, storage media, input/output devices, etc. that may be found in a conventional computer system. Memory 130 may include SDRAM, SRAM, ROM, DRAM and/or other conventional system memory devices. Processor 110 includes cores 140 A and 140 B, write coalescing cache 150 , level-2 cache 160 , and I/O interface 170 . I/O interface 170 may couple each of cores 140 to peripherals 120 . Elements referred to herein by a reference numeral followed by a letter may be collectively referred to by the reference numeral alone. For example, cores 140 A and 140 B may be referred to as cores 140 and an unspecified one of cores 140 may be referred to as a core 140 .
[0017] Each of cores 140 includes a level-1 cache 142 and store logic unit 144 . Store logic unit 144 (alternately referred to as “store unit”) may represent a portion of a load/store unit, a separate logic unit, or a combination thereof. Store logic 144 is coupled to both level-1 cache 142 and level-2 cache 150 to enable core 140 to write to either cache level. More specifically, store logic 144 may convey stores 180 to level-1 cache 142 and stores 182 to write coalescing cache 150 . Write coalescing cache 150 may be further coupled to level-2 cache 160 via fills 186 and evicts 187 . Write coalescing cache 150 may coalesce stores 182 and 183 with fills 186 to produce a reduced number of evicts 187 . Level-2 cache 150 may be further coupled to each level-1 cache 142 . More specifically, level-2 cache 160 may convey fills 184 to level-1 cache 142 A and fills 185 to level-1 cache 142 B. Level-2 cache 160 may also be bi-directionally coupled to memory 130 .
[0018] During operation, core 140 may execute a stream of instructions including loads and stores. When an instruction is decoded to produce a store, the resulting store may be sent to store logic 144 for further processing. In one embodiment, cores 140 may follow a write-through cache policy, according to which any store that is sent to level-1 cache 142 is also sent to level-2 cache 160 via write coalescing cache 150 . Consequently, processing of stores that are received by store logic 144 may be subject to the core gaining exclusive access to the target location in level-2 cache 160 or memory 130 . A detailed description of a process by which store logic 144 handles stores is given below.
[0019] Although system 100 , as shown, include two cores, in alternative embodiments more than two cores may be included and/or each core may represent a cluster of execution units. Additional level-2 caches may also be included in further alternative embodiments in which more than two cores are included. Further, although cache 160 is shown coupled directly to memory 130 and memory 130 is shown as off-processor memory, processor 110 may include a memory controller and/or on-processor memory. Alternatively, an off-processor memory controller may couple level-2 cache 160 to memory 130 . A variety of processor core and memory configurations will be apparent to one of ordinary skill in the art.
[0020] FIG. 2 is a detailed block diagram of one embodiment of store logic 144 . In the illustrated embodiment, store logic 144 includes a store queue 210 , a post-retirement store queue 220 , and a buffer 240 . Store queue 210 may include store locations 211 - 216 . Post-retirement store queue 220 includes store locations 221 - 225 . In one embodiment, store locations 211 - 216 and 221 - 225 may be linked to form first-in-first-out storage queues. Store queue 210 may be coupled to post-retirement store queue 220 and to buffer 240 , which in turn may be coupled to level-1 cache 142 . Although the illustrated store queue 210 includes six locations and the illustrated post-retirement store queue 220 includes five locations, in alternative embodiments the number of locations in store queue 210 or post-retirement store queue 220 may be either more or fewer than illustrated, depending on timing, bandwidth, a latency considerations.
[0021] During operation, store queue 210 may receive one or more decoded stores 252 from a load/store pipeline of a core 140 . Store queue 210 may maintain received stores in a queue until they are ready to be retired. A retirement pointer 230 may be received from core 140 to indicate the least recent store that is retired. Once a store is retired, it is ready to be sent to cache. Store queue 210 may send each retired store to buffer 240 as well as to post-retirement store queue 220 .
[0022] Stores that are sent to buffer 240 become part of stores 254 and may be buffered by buffer 240 until access to a target cache line within level-1 cache 142 is granted. Once access is granted, buffer 240 may send a store to level-1 cache 142 as part of stores 180 . In one embodiment, buffer 240 may be a fill coalescing buffer. For example, buffer 240 may combine stores to the same target cache line prior to sending them to level-1 cache 142 . In a further embodiment, buffer 240 may receive fills from level-2 cache 160 and combine them with stores 254 prior to sending them to level-1 cache 142 . In an alternative embodiment, buffer 240 may be external to store logic 144 , either built into level-1 cache 142 or placed between store logic 144 and level-1 cache 142 . In a further alternative embodiment, store queues 210 and 220 may be combined into a single queue with a tap for removing stores after they have been retired.
[0023] Stores that are sent to post-retirement store queue 220 become part of stores 256 . Stores 256 may be maintained in a queue comprising locations 221 - 225 until access to a target cache line within level-2 or higher cache, memory, or other storage structures associated with other processors is granted. Once access is granted, post-retirement store queue 220 may convey a store as part of stores 182 .
[0024] FIG. 3 illustrates one embodiment of a process 300 that may be used to operate a store queue. In the illustrated embodiment, process 300 includes an input process 302 , a retirement process 304 , and a removal process 306 . Process 300 may execute processes 302 , 304 , and 306 sequentially as shown. In alternative embodiments, two or more of processes 302 , 304 , and 306 may be executed in parallel. Process 300 may execute process 302 , 204 , and 306 in a continuous loop, although for simplicity, a single pass through processes 302 , 304 , and 306 will now be described.
[0025] Process 300 may execute process 302 , which may begin with reception of a store for queuing (decision block 310 ). If a store is received, and if the store queue is not full (decision block 320 ), then the received store may be placed in the queue (block 3330 ). If the queue is full, then process 300 may wait until space is available (block 340 ). If a store is not received, then process 300 may execute retirement process 304 , which may detect a retire signal (decision block 350 ). If a retire signal is received, then a retirement pointer may be advanced (block 360 ). If a retire signal is not received, then process 300 may execute removal process 306 , which may detect that one or more stores are in the retired state (decision block 370 ). Once stores are retired, they may be removed from the queue (block 380 ). If no stores are retired, then process 300 may end.
[0026] FIG. 4 illustrates one embodiment of a process 400 that may be used to remove a series of stores from a store queue after retirement. Process 400 represents one implementation of block 380 as shown in FIG. 3 . Process 400 may begin by getting the next retired store from a store queue (block 410 ). Each store may then be placed in a fill coalescing buffer (block 420 ) while a copy of each store may be placed in a post-retirement queue (block 460 ) in parallel. Stores placed in the fill coalescing buffer may be coalesced (block 430 ) according to a process that will be described further below. Access to a cache line targeted by each store in the fill coalescing buffer may be requested. Until access is granted, stores remain in the fill coalescing buffer (block 445 ). If access is granted (decision block 440 ), a store may be written to the level-1 cache (block 450 ), and flow may return to block 410 to get the next store. Access to a cache line at level-2 or above, targeted by each store in the post-retirement queue may be requested. Until access is granted, stores remain in the post-retirement queue (block 475 ). If access is granted (decision block 470 , a store may be written to the higher level cache (block 480 ), and flow may return to block 410 to get the next store.
[0027] FIG. 5 illustrates one embodiment of a process 500 that may be used to coalesce a series of stores. Process 500 represents one implementation of block 430 as shown in FIG. 4 . Process 500 may begin reception of a store (decision block 510 ). If a store is received, and if the store targets a cache line that is present in the buffer (decision block 520 ), then the received store may be merged with the existing cache line in the buffer (block 530 ). If the received store targets a cache line for which there is not a line stored in the buffer, then the received store may be placed in the buffer (block 540 ). Next, if no store is received, or after placing or merging a received store, then process 500 may receive a load (decision block 550 ). If a load is received, and if the load targets a cache line that is present in the buffer (decision block 560 ), then the received load may be merged with the existing cache line in the buffer (block 570 ). If the received load targets a cache line for which there is not a line stored in the buffer, then the received load may be placed in the buffer (block 580 ). Next, if no load is received, or after placing or merging a received load, then process 500 may end. Although a single pass through process 500 has been described for simplicity, in one embodiment, process 500 may execute in a continuous loop.
[0028] It is noted that the above-described embodiments may comprise software. In such an embodiment, the program instructions that implement the methods and/or mechanisms may be conveyed or stored on a computer accessible medium. Numerous types of media which are configured to store program instructions are available and include hard disks, floppy disks, CD-ROM, DVD, flash memory, Programmable ROMs (PROM), random access memory (RAM), and various other forms of volatile or non-volatile storage. Still other forms of media configured to convey program instructions for access by a computing device include terrestrial and non-terrestrial communication links such as network, wireless, and satellite links on which electrical, electromagnetic, optical, or digital signals may be conveyed. Thus, various embodiments may further include receiving, sending or storing instructions and/or data implemented in accordance with the foregoing description upon a computer accessible medium.
[0029] Although the embodiments above have been described in considerable detail, numerous variations and modifications will become apparent to those skilled in the art once the above disclosure is fully appreciated. It is intended that the following claims be interpreted to embrace all such variations and modifications. | A processor includes at least one processing core. The processing core includes a memory cache, a store queue, and a post-retirement store queue. The processing core retires a store in the store queue and conveys the store to the memory cache and the post-retirement store queue, in response to retiring the store. In one embodiment, the store queue and/or the post-retirement store queue is a first-in, first-out queue. In a further embodiment, to convey the store to the memory cache, the processing core obtains exclusive access to a portion of the memory cache targeted by the store. The processing core buffers the store in a coalescing buffer and merges with the store, one or more additional stores and/or loads targeted to the portion of the memory cache targeted by the store prior to writing the store to the memory cache. | 6 |
FIELD OF THE INVENTION
The present invention relates to a pipe, that is a hollow cylindrical member employing a ceramic superconducting material, and in particular to a pipe for fabricating a coil used in a semiconducting magnet or an electrical accumulator device.
BACKGROUND OF THE INVENTION
Conventionally, a metallic material such as Nb-Ge (for example, Nb 3 Ge) and the like is used as a superconducting material. This material has high ductility, malleability and bending property since it is a metal, and can be used for a coil in a superconducting magnet and also as an electrical accumulator coil.
However, the onset of the superconducting critical temperature (hereinafter referred to as Tc) of this metal is low, that is only 23° K. or lower. Also, if industrial applications of the material are considered, it is extremely important that the Tc be 100° K. or higher, and that the temperature where the electrical resistance becomes zero (hereinafter referred to as Tco) be 77° K. or higher.
Recently, a copper oxide ceramic has been attracting considerable attention as such a superconducting material. However, the copper oxide ceramic material is deficient in ductility, malleability and bending property, and difficult to process after forming.
Accordingly, it is required to develop an application of the copper oxide ceramic material to a coil member for use in the magnet or power accumulator device.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a copper oxide ceramic member of superconducting coil structure which can have a coolant therein for cooling.
Another object of the present invention is to provide a method of producing a copper oxide ceramic member of coil structure.
Accordingly, in the present invention, a copper oxide ceramic member of superconducting coil structure comprises a hollow support body made from a member selected from a metal and a metallic compound and a copper oxide superconducting ceramic material which covers the inner surface of the hollow support body with a space kept therein.
A method of the present invention comprises the steps of providing a hollow support body made from a metal or a metal compound and introducing a solution mixed with a superconducting ceramic material including copper oxide into the inside of the hollow support body.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects, features, and advantages of the present invention will become more apparent from the following description of the preferred embodiments taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a perspective view of a superconducting ceramic pipe of the present invention.
FIG. 2 is a schematic view of an example of an electical storage device using the pipe of the present invention.
FIG. 3 is an end view of an alternate embodiment of a superconducting ceramic pipe in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In order to accomplish the objects mentioned above, a hollow metallic or metallic compound support member is prepared, into which a liquid having a material for the superconducting ceramic material in a mixture, solution or gel is poured from one end of the hollow support member with the other end of the support member temporarily blocked.
A representative superconducting ceramic material used in the present invention is an oxidized ceramic using elements in Gruop IIIa and IIa of the Periodic Table, and copper.
The superconducting ceramic material of the present invention can be generally represented as (A 1-x B x ) y Cu z O w , where x=0.3 to 1, y=2.0 to 4.0 or, preferably, 2.5 to 3.5, z=1.0 to 4.0 or, preferably, 1.5 to 3.5, and w=4.0 to 10.0 or, preferably, 6 to 8. A is one type or several types of elements from among those selected from the yttrium group and those selected from the other lanthanides. The yttrium group is defined as the group containing Y(yttrium), Gd(gadolinium), Yb(ytterbium), Eu(europium), Tb(terbium), Dy(dysprosium), Ho(holmium), Er(erbium), Tm(thulium), Lu(lutetium), Sc(scandium), and other lanthanides (Physics and Chemistry Dictionary, published by Iwanami, Apr. 1, 1963).
One example of the superconducting ceramic material is a copper oxide ceramic material represented by the formula (A 1-x B x ) y CuO z , where x=0.01 TO 0.3, y=1.3 to 2.2, z=2.0 to 4.0, and A is selected from the group of Y(yttrium), Ga(gallium), Zr(zirconium), Nb(niobium), Ge(germanium), Yb(ytterbium), and other lanthanides, and B is a superconducting ceramic material selected from a group of Ba(barium), Sr(strontium), Ca(calcium), Mg(magnesium), and Be(beryllium). The ceramic material can include another elements (referred to as A and B here) depending on its use.
The superconducting ceramic material of the present invention can also be generally represented as (A 1-x B x ) y Cu z O w , where x=0.3 to 1, y=2.0 to 4.0 or, preferably 2.5 to 3.5, z=1.0 to 4.0 or, preferably 1.5 to 3.5, and w=4.0 to 10.0 or, preferably 6 to 8. A is one type of element selected from the elements in Group Vb in the Periodic table, consisting of Bi(bismuth), Sb(antimony), As(arsenic), and P(phosphorous). In addition, B is at least two types of elements, B1, B2--- Bn, for example B1, B2, selected from among Ba(barium), Sr(strontium), Ca(calcium), and Mg(magnesium).
Then, the whole of the hollow member or pipe is heated to evaporate and remove the liquid or solvent, resulting in a hollow pipe coated with the superconducting ceramic material on the inner wall surface thereof.
The resulting product is heated and sintered and subjected to repeated oxidization and reduction processes to produce a superconducting ceramic material.
Next, the entire hollow pipe is heated and the solvent or liquid medium is entirely removed by vaparizarion. This causes the superconducting ceramic material to cover the inner wall of the hollow pipe. By then repeatedly heating the coating to fire it and oxidize or reduce it, a superconducting ceramic material, for example, an oxidized copper ceramic, is formed which has a molecular structure represented by (Al-x Bx)y CuOz, where x=0.01 to 0.3, y=2.0 to 4.0; A is an element selected from a group of elements comprising Y(yttrium), Ga(gallium), Zr(zirconium), Nb(niobium), Ge(germanium), Yb(ytterbium), or other lanthanoids; and B is a superconducting ceramic material selected from a group of elemnents comprising Ba(barium) or Sr(strontium), Ca(calcium), Mg(magnesium), or Be(berylliun).
In the ceramic used in the present invention, elements other than those depicted by A and B can be added.
In the present invention, the superconducting ceramic material is coated as a first layer on the inner wall surface of the hollow support body or pipe, and then a second layer of ceramic material is coated over the first layer by repeating the process after the first layer of the ceramic material is sufficiently solidified. In addition, in this case, a part of the elements of A and B, and the values for x, y and z may be changed.
Of course, in the present invention these steps may be repeated to create a multilayer configuration.
When making the pipe or coil using the metallic superconducting material mentioned above, first a wire can be made by this process, then this wire is wound around a prescribed base to form a coil.
However, it is extremely difficult to form the wire rod of the ceramic superconducting material or wind the ceramic superconducting body around a base.
For this reason, in the present invention a pipe of metal or metallic compound is used, fabricated in the form of a previously prescribed bulb, coil, or endless coil with the starting and terminating points thereof connected to each other. Its interior is filled by the introduction of a liquid in which a superconducting ceramic material is slurried or dissolved. It is therefore possible to essentially create the final form of a pipe of a ceramic material by providing a coating of the superconducting material on the inner wall surface of the metal pipe.
Also, the pipe, when made as a coil or as a wire with the hollow space formed on the inside of this pipe or coil and with the superconducting ceramic material coated onto the the inner surface of the pipe, can be used as a channel for a cooling medium for cooling to the temperature Tco at which the electrical resistance becomes zero.
In addition, by winding a plurality of turns in coil shape using the pipe of the present invention, a superconducting magnet can be formed. Also, by connecting the starting and terminating ends of this coil to each other through the ceramic material the electrical resistance of which is zero, an endless coil is obtained. There is no loss of current in this coil, so it is possible to use it as an elecrtrical energy storage device.
[EXAMPLE 1]
In this embodiment, in the expression (A 1-x B x ) y CuO z , A was yttrium in the form Y 2 O 3 , B was barium in the form BaCO 3 , and copper was used in the CuO form. These chemicals had 99.95% purity or more. Here, x=0.05, x=0.075, and x=0.1, y=1.8, y=2.0, and Y=2.2. By mixing these, 9 types of mixtures were prepared. These were compacted into tablets once at a pressure of 3 kg/cm 2 and fired or sintered in air (called pre-fired), first at 700° C. for 3 hours then at 1000° C. for 10 hours. The resulting product was ground into particles having an average particle diameter not larger than 100 μm- for example, about 10 μm. This mixture was enclosed in a capsule and again compacted at 5 kg/cm 2 to form tablets. These tablets were then fully fired in an oxidizing atmosphere, for example, in air, at 1000° C. for 10 hours. After completion, the structure was seen in the so called perovskeit-like structure, but the transformed K 2 NiF 4 -type structure was observed from X-ray analysis.
Next, the fact that this fired material had a Tc onset greater than 40° K. and preferably 90° K., and a Tco greater than 77° K. was checked from the voltage-current-temperature characteristics.
The tablets were once again ground into a fine powder. The average particle diameter ranged from 100 μm down to 5 μm, for example, 30 μm. In this process, an effort was made during grinding to avoid destroying the basic crystal structure.
This powder was slurried or dissolved in a liquid, for example, freon liquid, or an alcohol such as ethanol, or another liquid.
This liquid was poured into the hollow support body or metal pipe 2 shown in FIG. 1 which is made of, for example, copper or a copper compound (such as a NiCu compound) with the other end of the pipe blocked. The inner wall surface of the pipe 2 was coated to a uniform thickness with the ceramic powder by rotating and turning the pipe 2 from end to end, so that the powder adhered to the wall while the pipe 2 was completely heated to a temperature at 100° C. to 400° C.
In this way, the solvent was removed from the inside of the pipe 2 and the inner wall surface received a ceramic powder coating 3.
To make the coating adhere more tightly to the inner wall surface, a solvent which dissolves epoxy or acrylic resins, for example, toluene or the like, may be used.
After this, oxygen or a mixture of oxygen and argon gas is introduced into the hollow section over the dried ceramic material adhered to the inner wall surface, and the ceramic material is fired while it is being oxidized at 500° C. to 1100° C., for example, at 600° C. for 3 hours, and additionally at 800° C. for 5 hours.
By repeating this type of process 1 to 5 times, the ceramic material was adhered to the inside of the pipe to an average thickness of 50 μm to 1 cm (as a representative figure, 0.5 mm to 5 mm). In this way, the pipe 1 of the present invention comprising a hollow support member 2 and a superconducting ceramic material 3 adhered on the inside of the support member was fabricated forming a space in the inside of the hollow support member 2 as shown in FIG. 1,
In the present invention, the pipe used is a cylindrical hollow support member. However, it may also be a square hollow support member (for example, as shown in FIG. 3, in which like elements are designated with primed numbers), and other shapes can also be used.
In such a superconducting ceramic pipe, Tc had a value 5° K. to 20° K. lower than at the time the tablet was made. However, it is possible to say that this was an improvement and better than the Tc from the initial tablet.
In addition, the length in this design can be changed from several centimeters to several scores of meters. Also, the thickness can be changed from a diameter of several millimeters to one of several centimeters.
[EXAMPLE 2]
This embodiment is an example of an endless coil as shown in FIG. 2 in a perspective view. This endless coil can be used as a battery for electric energy generated by a solar cell and the like.
As can be seen from this diagram, the pipe which has a previously-formed hollow space as in the first embodiment, was formed in the shape of a coil 7. In addition, a starting end 5 and a terminating end 6 were connected in the same way to a hollow pipe 9. This endless coil had a filler opening 8. This filler opening 8 can be used as input and output terminals for electrical energy.
Here, using the same method as in the first embodiment, the superconducting ceramic is slurried or dissolved in a liquid which was poured into the filler opening.
Drying the superconducting ceramic, the unnecessary solvent was driven off in the form of vapor through the openings 8, 8' and the inside of the pipe was dried. Also, in the same way as in the first embodiment, an oxidizing gas was introduced and the ceramic material was dried.
In this way, the endless coil 7 with a hollow interior was fabricated using the pipe 1 of which the inner wall surface was coated with the superconducting ceramic material. Its Tco was experimentally determined to be 45° K. However, by proper selection of the superconducting ceramic material, a higher Tco can be obtained. Also, by introducing liquid hydrogen into the hollow section, an endless coil with a closed circuit of zero resistance can be obtained so that it can be used as an electric energy storage device.
[EXAMPLE 3]
In this embodiment, in the expression (A 1-x B x ) y CuO z , Yb is used as A, and Ba is used as B. Consequently, even after the pipe is formed, the Tco was maintained at 72° K. Other preparation condition of this embodiment was the same as the first example.
In these examples, after such pipes are formed, the hollow inner section is filled with a cooling liquid such as liquid nitrogen or liquid hydrogen, which is a means for continuous and direct cooling of the pipe, specifically the superconducting ceramic material on the inner side, for which temperature is of the most importance.
In addition, using copper or a copper compound for the outside metal makes it possible to weld the pipe for use as part of an electrical device. The use of copper or a copper compound as the metal or metallic compound especially makes it possible to widen the application of this pipe, for example, in the field of electrical parts.
The superconducting ceramic material for use in accordance with the present invention also may be prepared consistent with the stoichiometric formulae (A 1-x B x ) y Cu z O w , where A is one or more elements of Group IIIa of the Periodic Table, e.g., the rare earth elements, B is one or more elements of Group IIa of the Periodic Table, e.g., the alkaline earth metals including beryllium and magnesium, and x=0 to 1; y=2.0 to 4.0, preferably 2.5 to 3.5; z=1.0 to 4.0, preferably 1.5 to 3.5; and w=4.0 to 10.0, preferably 6.0 to 8.0. Also, superconducting ceramics for use in accordance with the present invention may be prepared consistent with the stoichiometric formulae (A 1-x B x ) y Cu z O w , where A is one or more elements of Group Vb of the Periodic Table such as Bi, Sb, and As. B is one or more elements of Group IIa of the Periodic Table, e.g., the alkaline earth metals including beryllium and magnesium, and x=0 to 1; y=2.0 to 4.0, preferably 2.5 to 3.5; z=1.0 to 4.0, preferably 1.5 to 3.5; and w=4.0 to 10.0, preferably 6.0 to 8.0. One example of the former formulae is YBa 2 Cu 3 O x (x=6 to 8), and one example of the latter formulae is BiCaSrCu 2 Ox (the number of x can be substantially smaller than the oxygen amount of the former composition.) | A pipe comprises a hollow support member made from a member selected from copper and copper compounds and a copper oxide superconducting ceramic material which covers the inner surface of the support member with a space kept in the pipe for use in a magnet or power accumulator device. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Application No. 61/710,959 filed on Oct. 8, 2012, entitled “Utility Vehicle Gun Carrier.” The above identified patent application is herein incorporated by reference in its entirety to provide continuity of disclosure.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to mobile storage devices, specifically mobile storage devices that are specially designed to work with ATVs and carry weapons and other equipment.
[0004] ATV flatbeds create a number of unique problems when it comes to transporting certain types of equipment. Fragile equipment, such as fishing rods, can be broken by other objects rolling around in the ATV's flatbed. Even sturdier equipment, such as firearms, can be scratched or otherwise damaged by the abrasive surface of the flatbed or by other objects in the flatbed. Safety is also a major concern when transporting multiple firearms on an ATV. If multiple firearms are stored in the flatbed of an ATV, there is a risk of unintended discharge of the firearms if they collide with each other. Additionally, it may be very inconvenient to access the firearms if they are merely piled on top of each other in the flatbed and are not organized and separated. An equipment rack hanging off the exterior of the ATV also frees up space for the storage of additional equipment in the ATV's flatbed.
[0005] Several types of mobile gun racks have been disclosed in the prior art, but they have several inherent problems. Some types of mobile firearm racks are designed only for use with trucks and are not compatible with ATVs. This is a major disadvantage because often when hunting or participating in sporting events, the terrain is too rough for a pickup truck and an ATV must be used to reach the desired destination. Other types of firearm racks are designed to mount to the floor of a vehicle, which takes up a substantial amount of space that could otherwise be used to store other equipment. Finally, other types of firearm racks that have been specifically designed for ATVs are only capable of storing a single firearm or take up valuable space in the flatbed.
[0006] The present invention addresses all of the problems faced by firearm owners who wish to transport their firearms and other equipment using their ATVs. The present invention mounts on the exterior wall of the ATV's flatbed, thereby freeing up a substantial amount of space for the storage of other equipment in the ATV's flatbed. The present invention mounts to the exterior of an ATV via accessory rail attachments that engage support apertures present along the top edge of some models of ATV flatbed side rails. Engaging these support apertures allows the mobile equipment rack to be held upright and steady, ensuring that equipment will be easy to access and minimally jostled during transport. The present invention also allows for the storage of multiple firearms in a safe and easy-to-access manner by separating them and storing them vertically in order to prevent unintended discharge of the firearms through collisions during transportation on the ATV.
[0007] 2. Description of the Prior Art
[0008] Devices have been disclosed in the prior art that relate to mobile equipment storage. These include devices that have been patented and published in patent application publications. These devices generally relate to weapon racks that are secured at various positions on trucks or ATVs. The following is a list of devices deemed most relevant to the present disclosure, which are herein described for the purposes of highlighting and differentiating the unique aspects of the present invention, and further highlighting the drawbacks existing in the prior art.
[0009] These prior art devices have several known drawbacks. Specifically, U.S. Pat. No. 2,958,422 to Caloiero describes a gun rack that is primarily designed for installation into a cabinet. The gun rack comprises a pair of spaced vertical stiles, a horizontal rail and a vertical rail secured to the stiles, a plurality of oval sockets on the lower rail for receiving the gun butts, and a plurality of spaced openings on the vertical rail corresponding to each of the oval sockets. Although Caloiero discloses a gun rack that stores firearms in an upright position, the gun rack is not specifically designed to be affixed to any type of vehicle.
[0010] U.S. Pat. No. 4,057,183 to Ness is another such device that discloses a gun rack attaching to the wheel well of a rear wheel of a pickup truck. Ness is intended to protect guns, fishing rods, and other such equipment from damage caused by being placed in the body of a truck. Such damage can be caused either by the guns or other equipment colliding with each other, by other objects placed on top of the guns or other equipment, or by virtue of the guns rubbing against the abrasive floor of the truck during transportation. The gun rack discloses an M-shaped frame with two vertical legs that attach to the exterior wall of the wheel well, L-shaped support elements attached to the each of the vertical legs, and at least one clip attached to each support element for securing the guns in place. While Ness has a similar concept to the present invention, Ness is not designed to work with ATVs and does not store the guns in a vertical position. A critical aspect of the present invention is that it is specifically designed to work with ATVs to maximize the types of terrain over which the items can be transported.
[0011] U.S. Pat. No. 5,524,772 to Simmons discloses a firearm rack that attaches to the rear window of a truck. The firearm rack comprises a frame member having an upper and lower end, an upper and lower cradle member capable of receiving a portion of a firearm, and an upper and lower attachment member that secures the frame member to the rear window of the pickup truck. Simmons is designed to be used with a wide array of pickup trucks; however like Ness, it is not suited for use on an ATV due to ATVs' lack of a rear window.
[0012] U.S. Pat. No. 7,137,511 to Crowell discloses a mobile weapon storage system for guns and their accessories that can stand alone or attach to the floor of a vehicle securely. The mobile weapon storage system discloses a variable-width clamp, a weapon shelf, and a frame, which is composed of a left frame member, a right frame member, and a horizontal variable-width member connecting the left and right frames. While this system may adequately secure the firearms and could potentially be adapted for use with an ATV, it takes of valuable space in the ATV's flatbed that could be used to store other equipment. The present invention comprises a vertical gun rack that attaches to the exterior of the ATV's flatbed, thereby freeing up that space to be used to store other objects.
[0013] U.S. Pat. No. 7,770,767 to Bartholdy discloses a gun carrier that mounts to the front of an ATV and may be converted from a horizontal gun rack position to a vertical gun rest position. This gun rest position may be used as a firing rest when the ATV is not in motion. The gun carrier discloses a frame member having two ends, one of which is releasably attached to a first mounting structure on the ATV and the other of which is pivotally attached to a second mounting structure, a clamp that releasably locks the first end of the frame member to the mounting structure, a gas spring between the second mounting structure and the frame member, and a gun cradle attached to the frame member. This gun carrier, like the present invention, is specifically designed for ATVs, but it is only capable of securing a single firearm and it attaches to the front of the ATV, rather than along the exterior of an ATV's flat bed.
[0014] The present invention is a new and improved equipment rack that stores multiple firearms, is adapted specifically and ideally for use with an ATV, and frees up additional storage space in the ATV's flatbed. The present invention has rail accessory attachments, attached to the two vertical frame members, which engage with holes along the top of the exterior wall of the ATV's flatbed. This allows the equipment rack to hang off the exterior wall of the flatbed along the side of the ATV. The present invention substantially diverges in design elements from the prior art and consequently it is clear that there is a need in the art for an improvement to existing ATV equipment storage devices. In this regard the instant invention substantially fulfills these needs.
SUMMARY OF THE INVENTION
[0015] In view of the foregoing disadvantages inherent in the known types of equipment storage devices now present in the prior art, the present invention provides a new ATV equipment rack wherein the same can be utilized for providing convenience for the user when transporting their firearms while hunting or participating in sporting events while using an ATV.
[0016] It is therefore an object of the present invention to provide a new and improved firearm rack device that has all of the advantages of the prior art and none of the disadvantages.
[0017] It is another object of the present invention to provide an equipment rack that frees up space in the ATV flatbed for the storage of other objects.
[0018] Another object of the present invention is to provide an equipment rack that allows individuals to quickly and easily access their firearms, fishing rods, or other equipment.
[0019] A final object of the present invention is to provide an equipment rack that is safe for using during transportation and avoids the risk of inadvertent firearm discharge caused by firearms colliding with each other or other objects during transportation.
[0020] Other objects, features and advantages of the present invention will become apparent from the following detailed description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTIONS OF THE DRAWINGS
[0021] Although the characteristic features of this invention will be particularly pointed out in the claims, the invention itself and manner in which it may be made and used may be better understood after a review of the following description, taken in connection with the accompanying drawings wherein like numeral annotations are provided throughout.
[0022] FIG. 1 shows a front view of a first embodiment of the present invention, not engaged with the support accessory rail apertures of an ATV.
[0023] FIG. 2 shows a front view of the first embodiment of the present invention, focusing on this embodiment's top receiving means.
[0024] FIG. 3 shows a front view of the preferred embodiment of the present invention, focusing on this embodiment's top receiving means.
[0025] FIG. 4 shows a perspective view of the present invention, demonstrating how it engages with the support apertures along the top of the ATV flatbed accessory rails, thereby maintaining the equipment rack in an upright configuration.
[0026] FIG. 5 shows a close-up view of the accessory rail attachment, which engages with an ATV's support apertures to maintain the mobile equipment rack upright and steady during transport.
DETAILED DESCRIPTION OF THE INVENTION
[0027] Reference is made herein to the attached drawings. Like reference numerals are used throughout the drawings to depict like or similar elements of the mobile equipment rack. For the purposes of presenting a brief and clear description of the present invention, the preferred embodiment will be discussed as used for transporting firearms, fishing rods, and other equipment using an ATV model that has support apertures along the top wall of the flatbed side rails. The figures are intended for representative purposes only and should not be considered to be limiting in any respect.
[0028] Referring now to FIG. 1 , there is shown a front view of an embodiment of the mobile equipment rack. The mobile equipment rack comprises a pair of spaced vertical frame members 11 , each with a lower end 20 and an upper end 21 . A horizontal base member 12 extends between and connects to each of the lower ends 20 of the vertical frame members 11 . The horizontal base member 12 has an upper surface 19 , upon which are positioned a plurality of lower receiving means 14 that are adapted to receive the butts of firearms, the handles of fishing rods, or the bases of other such cargo items. In this embodiment, the lower receiving means are a series of V-shaped sockets 22 .
[0029] A horizontal top member 13 spans between and connects each of the upper ends 21 of the vertical frame members 11 . The horizontal top member 13 has a top receiving means 16 that is adapted to receive the barrels of firearms, the shafts of fishing rods, or the tops of other such cargo items. In this embodiment, the top receiving means 16 consists of two components. The first component is a plurality of depressions 17 that are adapted to receive the tops of the cargo items. The number of depressions 17 corresponds to the number of lower receiving means 14 , which in this embodiment are V-shaped sockets 22 . The depressions 17 and the V-shaped sockets 22 are vertically aligned so that firearms may be securely held in place during transportation. The second component is a strap 18 that removably extends between the upper ends 21 of the vertical frame members 11 . The strap 18 keeps the tops of the cargo items secured within the depressions 17 . Although in this embodiment the top receiving means 16 is a two-component system, the top receiving means 16 may consist of any system capable of adequately securing the tops of the cargo items and preventing lateral and tipping movement thereof.
[0030] An accessory rail attachment 15 is attached to each of the vertical frame members 11 between the lower end 20 and the upper end 21 . This accessory rail attachment 15 is adapted such that it is capable of engaging within the support apertures disposed along the upper surface of an ATV flatbed side rail. Certain models of vehicles include a flatbed area with raised sidewalls. The present invention contemplates connection thereto by way of an apertured accessory rail or through-holes in the side rail itself, which are spaced at a given distance to accommodate the first and second accessory rail attachment 15 of the present invention. The accessory rail attachments 15 are angled such that the vertical frame members 11 are not flush against the exterior wall of the flatbed. This angle makes the horizontal base member 12 protrude slightly compared to the horizontal top member 13 , and allows the mobile firearm rack to avoid interfering with the wheel and wheel well of the ATV. This also provides additional stability to the cargo items secured within the equipment rack because it causes the cargo items to comfortably rest within the lower receiving means 14 and the top receiving means 16 .
[0031] Referring now to FIG. 2 , there is shown a front view of one of the contemplated embodiments of the present invention, focusing on this embodiment's top receiving means 16 . In this embodiment, the top receiving means 16 consists of two components. The first component is a plurality of depressions 17 that are adapted to receive the tops of the cargo items. The number of depressions 17 corresponds to the number of lower receiving means 14 . The second component is a strap 18 that removably extends between the upper ends 21 of the vertical frame members 11 . The strap 18 keeps the tops of the cargo items secured within the depressions 17 . The strap 18 may extend between the vertical frame members 11 at any point, as long as it adequately secures the tops of the cargo items within the depressions 17 . In this embodiment, the strap 18 is removably attached on only one of the vertical frame members 11 , but this invention contemplates embodiments where the strap 18 is removably attached to both vertical frame members 11 .
[0032] Referring now to FIG. 3 , there is shown the preferred embodiment of the mobile firearm rack in a similar view as FIG. 2 . In this embodiment, the top receiving means 16 comprises a plurality of U-shaped notches 23 adapted to receive the barrels of firearms, the shafts of fishing rods, or the tops of other cargo items. The U-shaped notches 23 are comprised of a base attached to the horizontal top member 13 , two arms extending from opposite sides of the base, and internally-pointing flanges at the tips of the arms that present a narrow opening for cargo items to enter or leave the notches. The U-shaped notches 23 are composed of a material that is rigid enough that items cannot escape the notches during normal jostling from an ATV trip, but also flexible enough that items that are wider than the narrow opening presented by the U-shaped notches 23 can nonetheless be pushed into the notch via the application of reasonable force.
[0033] The U-shaped notches 23 are intended to relatively easily accept cargo items, but be rigid enough to firmly secure the cargo items during transportation. The number of U-shaped notches 23 corresponds to the number of lower receiving means 14 on the upper surface 19 of the horizontal base member 12 . The U-shaped notches 23 are vertically aligned with the lower receiving means 14 such that cargo items may be securely held in place during transport. Cargo items being firmly secured is paramount to the purpose of the invention because if certain types of cargo items, such as firearms, are improperly secured, then they pose a danger to the user and other individuals in the vicinity. Optionally, bands 24 may be placed around the arms of the U-shaped notches 23 to further ensure that the cargo items are properly secured. The bands 24 decrease the area in the interior of the U-shaped notches 23 , thereby securing the cargo items more tightly against the base of the U-shaped notches 23 and preventing potential damage to cargo items from banging into the walls of U-shaped notches 23 or banging into other cargo items during transportation.
[0034] In the embodiment as shown in FIG. 3 , the U-shaped notches 24 are supported in pairs from a common carrier. Each carrier supports a pair of notches 24 away from the top member while the carrier is mechanically fastened thereto. The notches 24 provide a firm grip of the cargo items by way of a base and a pair of aligned sides that form the U-shape, along with a pair of distal end, inwardly-directed lips that retain the cargo items within the U-shaped notch interior. The notch sides are deformable to allow the cargo items to be inserted into the notch interior, whereby the sides splay outward and the cargo items can be inserted thereinto before the sides and lip of the notches surround the cargo item and retain the same therein.
[0035] Referring now to FIG. 4 , there is shown a perspective view of the mobile equipment rack, demonstrating how the accessory rail attachments 15 engage with the support apertures 25 of the side wall 27 of the ATV's flatbed cargo area to keep the mobile equipment rack vertical. The support apertures 25 , the ATV 26 , and the flatbed side wall 27 should not be construed in anyway to be part of the invention. They are merely provided to show the interaction between the mobile equipment rack and a contemplated ATV structure well suited for supporting the present rack in an upright and stable configuration during transport. This perspective view also demonstrates how cargo items are secured by the lower receiving means 14 and the top receiving means 16 . This vertical storage system keeps the cargo items easily accessible while at the same time ensuring that they will not collide with each other during transport, thus reducing the risk of danger or damage to the cargo items.
[0036] Referring now to FIG. 5 , there is shown a close-up view of the preferred embodiment of an accessory rail attachment 15 . This consists of an angled block 28 affixed to each of the vertical frame members 11 . An elongated attachment member 29 extends from the angled block 28 and curves downwards. The attachment member 29 is an elongated member having a smaller diameter than the diameter of the corresponding support aperture, allowing the attachment member 29 to engage with the support aperture. This is merely one contemplated embodiment of the accessory rail attachment 15 . The accessory rail attachments 15 may be of any configuration that permits the mobile equipment rack to engage with the support apertures of certain ATV models' flatbed side wall. The accessory rail attachments 15 are angled rearward with respect to the vertical frame members 11 such that the horizontal base member 12 protrudes slightly outward from the ATV side wall, whereby the ATV wheel or wheel well does not interfere with the mobile equipment rack and cargo items are tilted backward into the rack during transport. The slight outward angle ensures that the firearms or other equipment sit comfortably within the lower receiving means 14 and the top receiving means 16 .
[0037] In use, the present mobile equipment rack is very well suited for securing and transporting firearms and other similarly sized objects. The rack vertically stores and separates the firearms such that they will not collide with each other or other objects during transportation, thus eliminating the risk of inadvertent discharge of the firearms. Furthermore, the storage rack allows individuals to quickly and easily access their firearms and because it hangs off the exterior wall of the ATV's flatbed wall, it saves space that can be used to store other objects.
[0038] It is therefore submitted that the instant invention has been shown and described in what is considered to be the most practical and preferred embodiments. It is recognized, however, that departures may be made within the scope of the invention and that obvious modifications will occur to a person skilled in the art. With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
[0039] Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention. | Disclosed is a mobile equipment rack suitable for holding firearms, fishing rods, or other equipment. The equipment rack comprises a base portion capable of keeping the lower portion of firearms or other equipment steady, a top portion with notches or other suitable means capable of receiving the upper portion of firearms or other equipment, two members on either side of the base that connect the base portion to the top portion, and two accessory rail attachments adapted to engage with the support apertures of an all-terrain vehicle (ATV) flatbed, such as those vehicles having support apertures along the raised sides of their flatbed cargo area. The mobile utility equipment rack allows multiple guns or other types of equipment to be securely stored in a safe, easy-to-reach fashion, while freeing up space in the ATV's flatbed for storing other items. | 1 |
This is a divisional of application Ser. No. 08/173,009, filed Dec. 27, 1993, now U.S. Pat. No. 5,367,990.
FIELD OF THE INVENTION
The present invention relates to systems and methods of operation thereof for variably controlling internal combustion engine intake and exhaust valves. More specifically, it relates to camless engine valve systems and methods of operation in engines used to eliminate the need for external exhaust gas recirculation and air throttling.
BACKGROUND OF THE INVENTION
Conventional automotive internal combustion engines operate with one or more camshafts controlling the timing and lift of the intake and exhaust valves, according to a predetermined lift schedule. With this type of mechanical structure, the lift schedule is fixed. However, under different engine operating conditions, the optimum lift schedule varies. Thus, the lift schedule must be a compromise of the optimum lift schedule needed for the different operating conditions. To accommodate full throttle engine operation, which requires significant air intake, an aggressive lift schedule must be used. At part load operating conditions, however, the intake air must then be throttled to prevent too much air from entering the cylinder. Consequently, this causes parasitic losses due to the throttling.
It is desirable to eliminate throttling losses by eliminating the need for an air throttle, without losing the effective compression ratio. One possible way to accomplish this is to close the intake valve before piston bottom dead center (BDC) during the intake stroke. However, the gas in the cylinder will then experience expansion during the end of the intake stroke with resultant cooling. Cooling of the gas can be detrimental to engine performance. Therefore, the need arises for a way to maintain the proper temperature of the gas at combustion when it undergoes a cooling due to expansion during the end of the intake stroke. This would improve combustion characteristics and provide better fuel economy.
Further, in internal combustion engines used in vehicles today, some of the exhaust gas is recirculated, by an external exhaust gas recirculation (EGR) system, to control the nitrogen oxide formation and to retain the maximum unburned hydrocarbons in the cylinder and allow for hotter intake gas for better evaporation of fuel. It is desired to eliminate the need for an external EGR system to reduce the cost and complexity that yields increased maintenance requirements. Additionally, for environmental reasons, it is desired to maintain as much of the unburned hydrocarbons in the cylinder as possible rather than allowing them to flow out in the exhaust.
It is understood that the distribution of unburned hydrocarbons in the cylinder charge at the beginning of the exhaust stroke is uneven. A substantial part of the unburned hydrocarbons that come out of the piston ring crevices at the end of the expansion stroke remain concentrated in the bottom part of the cylinder near the piston. If this part of the cylinder charge can be prevented from being discharged into the exhaust port, a substantial reduction in hydrocarbon emissions can be achieved. Thus, in order to maintain the greatest amount of unburned hydrocarbons within the cylinder, it is desired that the part of the exhaust charge with the highest concentration of unburned hydrocarbons be prevented from flowing out through the exhaust port. Furthermore, if some hot gas can temporarily reside in the intake port, it will increase the intake air temperature, which promotes better evaporation of fuel injected into the port, especially during engine cold start and warm-up. This, too, improves hydrocarbon emissions.
The enhancement of engine performance attainable by varying the acceleration, velocity and travel time of the intake and exhaust valves in an engine is well known and appreciated in the art. The increasing use and reliance on microprocessor control systems for automotive vehicles and increasing confidence in hydraulic and electric as opposed to mechanical systems is now making substantial progress possible. The almost limitless flexibility with which the intake and exhaust events (timing strategy) can be varied in an engine with a camless valvetrain can lead to substantial improvements in engine operation.
However, none of the present systems and methods of operation provide a variable engine valve control system that substitutes for the external EGR system in today's engines to reduce harmful emissions by returning a portion of unburned hydrocarbons back to the cylinder while at the same time promoting better evaporation of fuel, while also eliminating air throttling losses without reducing the effective compression ratio and while avoiding problems caused by low air temperature resulting from early intake valve closure. The present system optimizes engine performance, especially at part load engine operation.
SUMMARY OF THE INVENTION
In its embodiments, the present invention contemplates an electrohydraulically operated valve control system cooperating with a piston and cylinder in an internal combustion engine. The valve control system includes an intake port, coupled to the cylinder, having an intake valve operatively associated therewith, with the intake valve selectively closable before and after piston bottom dead center, and an exhaust port, coupled to the cylinder, having an exhaust valve operatively associated therewith. The valve control system further includes a heat exchanger having a heat exchange mechanism, an exhaust gas inlet and an exhaust gas outlet, and an intake air inlet and an intake air outlet, with the exhaust inlet being coupled to the exhaust port and coupled through the heat exchange mechanism to the exhaust outlet. The intake outlet is coupled to the intake port and is selectively coupled to an intake inlet though the heat exchange mechanism and around the heat exchange mechanism. The heat exchanger further has a means for selectively routing intake air through the heat exchange mechanism whereby the amount of intake inlet air that passes through the heat exchange mechanism is a function of the closing of the intake valve relative to the piston's bottom dead center position.
The present invention further contemplates a method of operating an engine valve control system in an internal combustion engine. The method includes the steps of opening an intake valve of a cylinder, selectively heating ambient intake air prior to entry into the engine cylinder, and closing the intake valve prior to a piston's bottom dead center position during an intake stroke within the cylinder whereby the intake air will be at an ambient temperature when the piston reaches a position of bottom dead center.
Accordingly, an object of the present invention is to provide a camless valvetrain system capable of eliminating the need for intake air throttling while still maintaining the effective compression ratio and adequate ignition characteristics.
It is a further object of the present invention to achieve the above noted object of the present invention and further to eliminate the need for an external EGR system by returning the portion of exhaust gas in the cylinder with the highest concentration of unburned hydrocarbons to the intake port during the exhaust stroke.
It is an advantage of the present invention that the need for air throttling will be eliminated without reducing the effective compression ratio and without adversely affecting ignition characteristics.
It is a further advantage of the present invention that nitrogen oxide and hydrocarbon emissions will be reduced while eliminating the need for an external EGR system and allowing for better fuel evaporation.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram showing a single valve assembly of an electrohydraulic camless valvetrain in accordance with the present invention;
FIG. 2 is a circular diagram illustrating the duration and timing of intake and exhaust events of engine valves in accordance with the present invention;
FIGS. 3A and 3B show a schematic diagram of an engine cylinder and engine valves in two stages of an exhaust stroke in accordance with the present invention;
FIGS. 3C and 3D show a schematic diagram of an engine cylinder and engine valves in two stages of an intake stroke in accordance with the present invention; and
FIG. 4 is a schematic diagram of an intake air heat exchanger in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a single engine valve assembly 8 that forms part of a valvetrain controlled by a electrohydraulic camless valve system (not shown). While this figure is the preferred embodiment for the valvetrain, other hydraulic and electrical systems can also be used to variably control engine valves. An electrohydraulic valvetrain is shown in detail in U.S. Pat. No. 5,255,641 to Schechter, which is incorporated herein by reference.
A single engine valve assembly 8 of an electrohydraulically controlled valvetrain is shown in FIG. 1. An engine valve 10, for inlet air or exhaust as the case may be, is located within a cylinder head 12. A valve piston 26, fixed to the top of the engine valve 10, is slidable within the limits of a piston chamber 30.
Fluid is selectively supplied to volume 25 above piston 26 from a high pressure oil source 40 and a low pressure oil source 42 hydraulically connected through a high pressure line 44 and a low pressure line 46, respectively, to a high pressure port 48 and a low pressure port 50, respectively.
Volume 25 can be connected to high pressure oil source 40 through a solenoid valve 64 or a check valve 66, or no low pressure oil source 42 through a solenoid valve 68 or a check valve 70. A volume 27 below piston 26 is always connected to high pressure oil source 40. A fluid return outlet 72 provides a means for returning to a sump (not shown) any fluid that leaks out of piston chamber 30. High pressure solenoid valve 64 and low pressure solenoid valve 68 are activated and deactivated by signals from a microprocessor controller 74.
Engine valve opening is controlled by high-pressure solenoid valve 64 which opens, causing valve acceleration, and closes, causing deceleration. Opening and closing of low pressure solenoid valve 68 controls engine valve closing.
During engine valve opening, high pressure solenoid valve 64 opens and the net pressure force acting on piston 26 accelerates engine valve 10 downward. When high pressure solenoid valve 64 closes, pressure above piston 26 drops, and piston 26 decelerates pushing the fluid from volume 27 below it back into high pressure oil source 40. Low pressure fluid flowing through low pressure check valve 70 prevents void formation in volume 25 during deceleration. When the downward motion of engine valve 10 stops, low pressure check valve 70 closes and engine valve 10 remains locked in its open position.
The process of valve closing is similar, in principle, to that of valve opening. Low pressure solenoid valve 68 opens, the pressure above piston 26 drops and the net pressure force acting on piston 26 accelerates engine valve 10 upward. When low pressure solenoid valve 68 closes, pressure above piston 26 rises, and piston 26 decelerates pushing the fluid from volume 25 through high-pressure check valve 66 back into high-pressure oil source 40.
The flexibility with which the timing and lift of intake and exhaust valves can be continuously varied allows great flexibility in optimizing engine performance for many different engine operating conditions, including part load engine operating conditions.
FIGS. 2, 3A, 3B, and 3C show variable valve timing in which early intake valve opening and exhaust valve closing aids engine operation for certain engine operating conditions by eliminating the need for an external EGR system. The variable timing for closing 101 of an exhaust valve 100 and opening 103 of an intake valve 102 in a cylinder 112 is shown such that, at part-load, closing 101 and opening 103, respectively, takes place substantially in advance of a piston 110 reaching top dead center (TDC) 104 so that the exhaust charge is split into two parts. Exhaust valve 100 and intake valve 102 are preferably each electrohydraulically controlled in the same manner as engine valve 10 shown in FIG. 1, although other camless engine valve systems can also be used.
As a result of the timing of the valve closings and openings, a first part of the exhaust gasses, comprising the upper part of the cylinder content, is expelled into an exhaust port 106 during the first portion of the exhaust stroke, as shown in FIG. 3A. A second part of the exhaust gasses, comprising the lower part of the cylinder content, is expelled into an intake port 108, as shown in FIG. 3B. The second part will contain a higher concentration of unburned hydrocarbons than the first part since a substantial portion of the unburned hydrocarbons are concentrated in the bottom part of the cylinder 112.
When piston 110 begins its intake stroke, the gas previously expelled into intake port 108 returns to cylinder 112 as part of the intake charge, as shown in FIG. 3C. This assures that a substantial amount of the unburned hydrocarbons produced during each cycle will be introduced back into cylinder 112 from intake port 108 and can then participate in the next combustion cycle. The quantity of the exhaust gas thus retained in the cylinder can be controlled by varying the timing of exhaust valve closing 101 and intake valve opening 103. The second part of exhaust charge returned to the cylinder restricts the quantity of nitrogen oxide produced in the next cycle, thus reducing harmful emissions and eliminating the need for an external EGR system.
As an additional benefit, the temporary residence of the second part of the exhaust charge in intake port 108 preceding each intake stroke will also promote better evaporation of the fuel injected into port 108 due to the high temperature of the gas. This is especially beneficial during engine cold start and during engine warm-up.
As an alternative, it should be noted that retention of some of the exhaust gas in cylinder 112 in the gas splitting strategy can also be accomplished by delaying exhaust valve closing significantly past TDC 104. In this case, practically the entire exhaust charge is expelled into exhaust port 106, and some of it returns to cylinder 112 at the beginning of the intake stroke. There is, however, no assurance that the gas that returns represents what was previously in the lower part of cylinder 112, and, hence that the highest concentration of unburned hydrocarbons is maintained in cylinder 112.
FIGS. 2, 3C, and 3D show intake valve closing 113 in which the variable timing of closing 113 is such that, at part-load, intake valve closing 113 takes place substantially before piston bottom dead center (BDC) 114, trapping a variable volume of intake air in cylinder 112 initially at approximately barometric pressure. This facilitates unthrottled engine operation at part load, eliminating the need for intake air throttling. To restrict the quantity of air inducted into cylinder 112, intake valve 102 is closed far in advance of BDC 114, thus reducing the volume of the trapped intake charge. The mixture of intake air, fuel and exhaust gas that was inducted at near barometric pressure will then be subjected to expansion during the remainder of the intake stroke. The intake air expansion after intake valve closure will cause an associated cooling. The drop in intake charge temperature associated with its expansion may lead to excessively low temperature at the end of the compression stroke, which can be deleterious to the combustion process.
To prevent this, the intake air can be heated. One way to accomplish this heating is through heat exchange with the exhaust gas. The intake air, then, is subjected to heating in advance of its induction into cylinder 112. This heating of intake air will assure that, after the expansion caused cooling in the cylinder, the temperature of the intake charge is approximately equal to the ambient temperature of the air before the expansion.
FIG. 4 illustrates a heat exchanger 116 that selectively preheats the intake air prior to entering intake port 108. Heat exchanger 116 includes intake inlet 122 for receiving ambient air, with a mass air flow sensor 124 mounted at inlet 122. Mass air flow sensor 124 monitors the total mass of inlet air flowing into intake inlet 122. Intake inlet 122 divides into a bypass duct 126 and a heat exchange inlet duct 128. The intake air can be routed through a heat exchange mechanism 118 via heat exchange inlet duct 128, where the air temperature is increased. A heat exchange outlet duct 130 connects to the bypass duct 126, which leads to an air intake outlet 132.
Heat exchanger 116 further includes an exhaust gas inlet 134, connected between exhaust port 106 and heat exchange mechanism 118, and an exhaust gas outlet 136 also connected to heat exchange mechanism 118. A directional control valve 120 can be rotated to vary the percentage of the total mass air flow that is directed through the heat exchanger from 0 to 100%, and, in this way, control the temperature of the air inducted into cylinder 112.
Air flowing through heat exchange mechanism 118 is heated so that, after expansion, the temperature of the intake charge is not below the ambient temperature. Thus, the heating of the air before induction into cylinder 112 cancels the cooling effect of expansion, so that at the start of the compression stroke, the gas in cylinder 112 is below atmospheric pressure but at approximately ambient atmospheric temperature. These are the same conditions that would prevail in cylinder 112 at this point in the cycle if the intake air was throttled, except that there was no throttling and consequently, no pumping loss.
During the subsequent compression stroke, the intake charge is subjected to full compression determined by the geometric compression ratio. Since the effect of expansion cooling was cancelled out by the air heating, the charge expansion during the intake stroke has no detrimental affect on the rest of the cycle.
As an alternative to early intake valve closure, it should be noted that the air flow control at part-load can also be accomplished by closing intake valve 102 late after BDC 114 rather than before BDC. The effect of reduced effective compression ratio can still be alleviated by air heating, but the loss of heat to cylinder walls can be substantial. Thus, early intake valve closing is the preferred arrangement.
While certain embodiments of the present invention have been described in detail, those familiar with the art to which this invention relates will recognize various alternative designs and embodiments for practicing the invention as defined by the following claims. | A variable engine valve control system and method of operation thereof wherein each of the reciprocating engine valves is hydraulically or electrically controlled and can vary its lift schedule for various engine operating conditions. During part load operation of the engine, the intake valve is opened and the exhaust valve is closed during the exhaust stroke, prior to a piston's top dead center position, so that the intake port receives exhaust gas, which is then returned to the cylinder during the intake stroke to eliminate the need for an external exhaust gas recirculation system and to improve fuel evaporation into the intake air. Further, during part load, the intake valve is closed before the end of the intake stroke and the intake air is heated by a heat exchanger prior to entry into the cylinder to eliminate the need for air throttling without compromising the compression ratio and ignition characteristics. | 5 |
TECHNICAL FIELD
This invention relates generally to power supplies for supplying power to portable electronic devices having a rechargeable battery, and more specifically to a power adapter including a rechargeable adapter battery.
BACKGROUND
Rechargeable batteries may be found in a variety of portable electronic devices, including laptop computers, personal digital assistants (PDAs), cell phones, digital media players, cameras, etc. The rechargeable battery in such devices is typically charged using power supplied from a power adapter connected to an external power source. The power adapter may also be configured to provide power to run the device, in conjunction with charging the internal battery.
Existing adapters do not include an battery source for powering electronic devices and/or powering an internal battery. As such, users desiring additional battery power will typically purchase an external battery that can be separately connected to the portable electronic device. However, such external batteries are generally cumbersome to use, at least because they must be unpacked for use and then repacked for storage. In addition, many users may forget to bring the external battery in addition to the adapter while in transit.
What is needed is a way to combine a power adapter and a battery so that a user does not have to carry an additional external battery while traveling with a portable electronic device.
SUMMARY
Generally, embodiments discussed herein provide power to an electronic device from a battery external to the device but associated with a power adapter. The power adapter typically includes the battery as an integral component that is connected to a plug or other interface capable of mating with a power source, such as a wall socket. Thus, presuming the adapter is plugged into the electronic device, the adapter battery may provide power either to operate the device or charge a battery within (or otherwise associated with) the device even if the adapter is not connected to a power source.
Further, the adapter may include a processor, such as a microcontroller, that may execute logical operations to intelligently determine how to distribute charge between the adapter battery and device battery, based at least in part on an operating state of the device. The adapter processor may communicate with a processor inside the device and, in some embodiments, the device processor may assist in such logical operations or may perform the operations and instruct the adapter processor accordingly. Thus, the adapter may vary its charging function depending on operating variables not only of the adapter itself, but also those of the device to which it is connected.
One embodiment takes the form of an apparatus for providing power to an electronic device, including: a processor; a battery operatively connected to the processor; a power output operatively connected to the battery and configurable to be connected to the electronic device; a relay operatively connected to the battery and the processor; and a power input operatively connected to the battery and the relay.
Another embodiment takes the form of a method for powering an electronic device from an adapter having an internal adapter battery The method may include the following operations: determining if the adapter is connected to a power source; in the event the adapter is connected to the power source, determine if the device is connected to the adapter; in the event the device is connected to the adapter, operating the device from the power source; and in the event the device is not connected to the adapter, charging the internal adapter battery.
These and other embodiments and features will be apparent to those of ordinary skill in the art upon reading this disclosure in its entirety, along with the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates an embodiment of a power adapter having a rechargeable battery coupled to an electronic device.
FIG. 2 is a block diagram of the embodiment of the power adapter and electronic device shown in FIG. 1 .
FIGS. 3A-3B are a flow diagram illustrating the power adapter and electronic device of FIG. 1 in various stages of use.
FIG. 4 is a block diagram of another embodiment of an electronic device having multiple rechargeable batteries.
DETAILED DESCRIPTION
A portable electronic device, such as a laptop computer, may include an internal battery to provide power for several hours of operation while the laptop computer is not connected to an external power source. Generally, in order to continue operation once the internal battery is depleted, one must recharge the battery, replace it, or connect the portable electronic device to a power source such as an electrical outlet. Further, many portable electronic devices are sealed and so a user cannot replace the internal battery, or at least cannot do so easily.
An adapter having its own internal battery may be connected to a portable electronic device to provide power to operate the device once its battery is depleted. In some embodiments, the adapter and the electronic device may each include respective microcontroller units that are configured for sharing information, such as battery charge and power source information, between the various internal hardware components, as well as between the electronic device and the adapter.
It should be noted that an adapter with an internal battery, as described herein, may be used with any appropriately-configured portable electronic device or non-portable device, for that matter. Suitable electronic devices include, but are not limited to, mobile telephones, portable computers, tablet computing devices, input/output devices, portable video players, portable televisions, personal digital assistants, headphones, and so on.
As shown in FIGS. 1 and 2 , in one embodiment, an electronic device 12 having a rechargeable internal battery 38 may be connected to a power adapter 10 having a rechargeable adapter battery 11 . The power adapter 10 may also be connected to a power source 17 via a plug 20 . The sample electronic device 12 shown in FIG. 1 and discussed herein is a portable computer, but it should be understood that any of the aforementioned devices may be appropriately configured and substituted. In addition, the power source 17 may be any source of electrical power, including a direct current (DC) power source, although an alternating current (AC) source is illustrated in FIG. 1 .
The adapter 10 may include an output connector 24 connecting the adapter 10 to the electronic device 14 , as well as an input power line 16 connecting the adapter 10 to the external power source 17 . In some embodiments, the adapter may further include an outer housing 18 for protecting the internal components of the adapter 10 , and the input power line 16 may include a cord coupled to a plug 20 configured for plugging into the external power source 17 . In other embodiments, the plug 20 may extend directly from the housing 18 , rather than from a cord.
The output connector 24 may include a plug that may be received by a receiving port on the electronic device 14 (port not shown). In some embodiments, the plug may include a quick release mechanism that enables the plug to disengage from the receiving port if it is tugged on, for instance by someone tripping over the output cord. In addition, the output connector 24 may further include a light indicator, such as a light-emitting diode (LED), configured to indicate the battery charge state, e.g., charging or fully charged, of the adapter battery 11 and/or the internal rechargeable battery 38 in the electronic device 12 . One connector that may be used in conjunction with an embodiment of the power adapter 10 is the MAGSAFE connector manufactured by Apple Inc.
FIG. 2 is a block diagram schematically illustrating some of the internal components of the power adapter 10 and electronic device 12 shown in FIG. 1 . As shown in FIG. 2 , the electronic device 12 may include an internal device microcontroller unit 34 and an internal charger 36 , as well as an internal rechargeable internal battery 38 . The device microcontroller unit 34 may be connected to the internal charger 36 and the internal battery 38 , as well as to the adapter microcontroller unit 32 of the adapter 10 . In some embodiments, the device microcontroller unit 34 may also be connected to a wireless control device 37 configured to receive and transmit information to the adapter microcontroller unit 32 of the adapter 10 . The internal charger 36 may be connected to the internal rechargeable battery 38 , as well as to the adapter 10 through a power line 24 configured to supply voltage from the adapter 12 to the charger 36 .
Additionally, the internal charger 36 may be connected, either wirelessly or through physical communication channels, to the other components of the electronic device 12 in order to direct power to these components when the adapter 10 is connected to an external power source 17 (as shown in FIG. 1 ). The internal battery 38 may also be connected to the other components of the electronic device 12 to supply battery power to these components when, for example, the electronic device 12 is not connected to the adapter 10 and/or the adapter 10 is not connected to an external power source.
In one embodiment, the device microcontroller unit 34 may include one or more inputs that receive data from the internal battery 38 and the adapter microcontroller unit 32 of the adapter 10 . For example, in one embodiment, the device microcontroller unit 34 may be configured to receive information from the internal battery 38 indicating the charge level of the battery 38 . Continuing the example, the charge level may be reported in various states indicating if the battery 38 is very low, low, adequate or fully charged. As will be described more fully below, the device microcontroller unit 34 may also be configured to receive information from the adapter microcontroller unit 32 indicating the level of charge of the adapter battery 11 and/or whether the adapter 10 is connected to an external power source. As shown in FIG. 2 , this information may be sent via a physical communication channel 17 or through a wireless control device 37 . Additionally, the device microcontroller unit 34 may include one or more sensors for measuring and monitoring the power being supplied from the adapter 10 to the electronic device 12 via power line 24 .
The device microcontroller unit 34 may likewise include one or more outputs for transmitting information to the adapter microcontroller unit 32 . For example, the device microcontroller unit 34 may be configured to transmit the charge level received from the internal battery 38 to the adapter microcontroller unit 32 of the adapter 10 , either through a physical communication channel 17 or a wireless control device 38 .
The device microcontroller unit 34 also may include a control line outputting a control signal to the internal charger 36 ; the microcontroller 34 typically generates this control signal. The control signal may enable the charger 36 to either begin or stop charging the internal battery 38 . The control signal may be based on the charge level information received from the adapter microcontroller unit 32 regarding the adapter battery 11 , whether the adapter 10 is connected to an external power source and/or the charge level information received from the internal battery 38 .
As shown in FIG. 2 , the power adapter 10 may include a converter 22 , a relay 26 , a charger 30 , a rechargeable internal battery 11 , a adapter microcontroller unit 32 , a boost converter 13 , a power switch 14 , a voltage regulator 15 , and/or one or more universal serial buses 18 (USB).
In one embodiment, the converter 22 is connected to the external power source 17 (as shown in FIG. 1 ) via an input power line 16 , which may include a cord and an associated plug 20 . The converter 22 may convert AC voltage received from the power source 17 into DC voltage that is usable by the other components in the adapter 10 , as well as by the electronic device 12 . Additionally, the converter 22 may be connected to a relay 26 that is configured to supply voltage either from the converter 22 to the charger 30 to charge the adapter battery 11 or directly from the converter 22 to the power switch 14 , bypassing the charger 30 and the battery 11 . As will be discussed in more detail below, the determination as to whether voltage is supplied directly to the power switch 14 or through the charger 30 , battery 11 and the boost converter 13 is made by the adapter microcontroller unit 32 .
In some embodiments, the power adapter 10 may include an additional input configured to receive power from a trickle power source 21 , such as a solar or photovoltaic cell, supplying a trickle voltage. As shown in FIG. 1 , the trickle power source 21 may be connected to the charger 30 so as to supply voltage to the charger 30 and/or the power switch 14 , while bypassing the converter 22 .
As shown in FIG. 2 , relay 26 may be set so that voltage is supplied from the converter 22 to the charger 30 . In one embodiment, the charger 30 may be configured to supply a current to the adapter battery 11 to charge the battery 11 . The charger 30 may also be configured to supply voltage from the battery 11 to a boost converter 13 , which in turn may be configured to convert the voltage received from the battery 11 to output a higher DC voltage. The boost converter 13 may, in turn, be connected to the power switch 14 .
The power switch 14 may be configured to receive voltage directly from the converter 22 (via relay 26 ) or from the boost converter 13 . Further, the power switch 14 may be connected to the internal charger 36 of the electronic device 12 by the power connector 24 , initially discussed with respect to FIG. 1 . The power switch 14 may further be configured to supply voltage to an additional port provided in the adapter 10 , such as a USB port 18 configured to receive a secondary portable electronic device, such as a cellular phone and/or a portable media player. Examples of suitable such devices include an iPod or an iPhone, as currently manufactured by Apple Inc. A voltage regulator 15 may regulate the voltage outputted by the power switch 14 in order to maintain a constant voltage level, thereby preventing or minimizing damage to the secondary device caused by sudden voltage increases in the external power source (as well as ensuring the voltage level is sufficient to operate or charge the secondary device).
Still with respect to FIG. 2 , a adapter microcontroller unit 32 may be electrically connected to various components of the power adapter, including the power switch 14 , the boost converter 13 , the charger 30 , the adapter battery 11 , the relay 26 and/or the converter 22 . The adapter microcontroller unit 32 may also be connected via a control line 17 to the internal device microcontroller unit 34 of the electronic device 12 . In some embodiments, the adapter microcontroller unit 32 may also be wirelessly connected via a wireless control device 37 to the internal device microcontroller unit 34 of the electronic device 12 .
The adapter microcontroller unit 32 may include a microprocessor, a program memory in the form of a NOR flash or ROM, as well as an EEPROM (or other erasable storage mechanism). Additionally, the microcontroller unit may further include other functional components, such as a crystal oscillator, timers, watchdog, serial and analog I/O, etc. As would be appreciated by one of skill in the art, the microcontroller 32 may be fabricated on a single integrated chip, or may include components located on multiple chips.
The adapter microcontroller unit 32 may include a plurality of inputs and/or outputs for receiving information regarding various components within the adapter 10 and/or controlling these components. For example, in one embodiment, the adapter microcontroller unit 32 may be configured to receive information from the converter 22 indicating whether the converter 22 is receiving voltage from the input power line 16 , i.e., whether the adapter 10 is receiving power from an external power source. Additionally, the adapter microcontroller unit 32 may be configured to receive information from the adapter battery 11 indicating the charge level of the battery 11 , for example, whether the battery is very low, low, adequate and/or fully charged. The adapter microcontroller unit 32 may further include an additional input for receiving information from the internal device microcontroller unit 34 of the electronic device 12 , such as the charge level of the internal battery 36 of the electronic device 12 .
The adapter microcontroller unit 32 may also control and/or monitor various functions of the adapter 10 . For example, the device microcontroller unit 34 may be configured to transmit the charge information received from the adapter battery 11 to the internal device microcontroller unit 34 , either through a physical communication channel 17 , or through a wireless control device 38 . In addition, the adapter microcontroller unit 32 may transmit control signals to the charger 30 , boost converter 13 , relay 26 and/or power switch 14 based on information received from the converter 22 , the adapter battery 11 , and/or the internal device microcontroller unit 34 of the electronic device 12 .
Continuing the discussion, the adapter microcontroller unit 32 may be connected to the adapter charger 30 by a control line. The adapter microcontroller may generate and transmit a control signal instructing the charger 30 to either begin or stop charging the adapter battery 11 , as necessary or desired. In addition, the adapter microcontroller unit 32 may also control operation of the boost converter 13 , the relay 26 and power switch 14 . Thus, opening and closing of relay 26 and power switch 14 is generally under the control of the adapter microcontroller, which may thus direct power to flow directly from the converter 22 to the device 12 or through the charger 30 , battery 11 , and boost controller 13 .
FIG. 3A is a flowchart illustrating one method for supplying power between an electronic device and an adapter having a battery if the adapter is connected to a power source, but the electronic device is not connected to the adapter. Initially, in operation 302 the embodiment may determine whether the adapter has been connected to an external power source. Referring to FIG. 2 , this operation is typically performed by the adapter microcontroller unit 32 of the adapter 10 , which receives information from the converter 22 indicating whether the adapter 10 is connected to the external power source 17 .
If, in operation 302 , the embodiment determines that the adapter is connected to an external power source, it may determine whether the electronic device is connected to the adapter in operation 304 . This determination may be made by either the device microcontroller unit 34 , which receives information from the internal charger 36 indicating whether the electronic device 12 is connected to the adapter 10 via the power line 24 , or the adapter microcontroller unit 32 . It should be noted that operation 304 may be optional in certain embodiments or may occur prior to operation 302 , in which case operation 320 may be omitted.
If in operation 304 the embodiment determines that the electronic device is not connected, then operation 314 is executed and the embodiment will charge the adapter battery from the external power source. This operation is generally performed via the adapter microcontroller unit 32 which is configured to transmit a control signal to the relay 26 to supply voltage from the converter 22 to the adapter charger 11 . The adapter microcontroller unit 32 is further configured to transmit a control signal to the adapter charger 30 enabling the charger 30 to charge the adapter battery 11 . Following operation 314 , the method ends in end state 346 .
Continuing the discussion of FIG. 3A , as previously mentioned, in operation 304 the embodiment determines if the electronic device is connected to an external power source. If the embodiment determines that the electronic device is connected to an external power source, then operation 306 is accessed and the embodiment will run the electronic device from the external power source.
Referring back to FIG. 2 , if the adapter microcontroller unit 32 receives an indication that the adapter 10 is connected to a power source and the device microcontroller unit 34 of the electronic device 12 receives an indication that the electronic device 12 is connected to the adapter 10 , the adapter microcontroller unit 32 may transmit a control signal to the relay 26 to supply voltage from the converter 22 directly to the power switch 14 , bypassing the charger 30 and the boost converter 13 . The adapter microcontroller unit 32 may also transmit a control signal to the power switch 14 to supply voltage received from the relay 26 to the adapter 12 .
Turning back to FIG. 3A , operation 308 is executed after operation 306 . In operation 308 , the embodiment will determine whether there is excess power available in light of the power requirements necessary to operate the device. This determination is made by the device microcontroller unit 34 of the electronic device 12 , which may include sensors for monitoring the power supplied to the internal charger 36 from the adapter 12 via the power line 24 . If there is insufficient power for any operation beyond supplying power to the device, then operation 318 is accessed and the embodiment will not charge the internal battery. Accordingly, the embodiment and will continue to only run the computer from the external power supply. Referring to FIG. 2 , if the device microcontroller unit 34 of the electronic device 12 determines that there is insufficient power to charge the internal battery 36 , the microcontroller 34 will transmit a control signal to the internal charger 36 to disable charging of the internal battery 36 , and to provide power received from the adapter 10 to power the other components of the electronic device 12 .
Following the execution of operation 315 , the method ends in end state 346 .
It may alternately be determined in operation 308 that the available power is sufficient to charge the internal battery. If so, the embodiment proceeds to operation 310 and the internal battery is charged.
Next, in operation 312 , the embodiment determines if there is still sufficient available power to charge the adapter battery. This determination may be made by the device microcontroller unit 34 or the adapter microcontroller. If, in operation 312 , there is sufficient available power to charge the adapter battery, then in operation 314 the embodiment will charge the adapter battery. As mentioned above, this operation is performed via the adapter microcontroller unit 32 which is configured to transmit a control signal to the relay 26 to supply voltage from the converter 22 to the adapter charger 11 , as well as transmit a control signal to the adapter charger 30 to charge the adapter battery 11 .
If, in operation 312 , if there is not sufficient available power to charge the adapter battery, then in operation 315 the embodiment will not charge the adapter battery. Referring to FIG. 2 , if the device microcontroller unit 34 of the electronic device 12 determines that there is insufficient power to charge the adapter battery 11 , the microcontroller 34 will transmit this information to the adapter microcontroller unit 32 , which in turn will transmit control signals to relay 26 and power switch 14 to supply voltage directly from the converter 22 to the charger 36 of the electronic device 12 , bypassing the charger 30 and boost converter 13 .
After either operation 314 or 315 , the method terminates in end state 346 .
The discussion of FIG. 3A now returns to operation 302 . If the embodiment determines that the adapter is not connected to an external power source in this operation, then, in operation 320 , the embodiment determines whether the electronic device is connected to an external power source. Referring to FIG. 2 , this may be accomplished by the microcontroller 34 of the electronic device 12 , which may receive information from the charger 36 indicating whether the charger 36 is connected to the adapter 10 . It should be noted that operation 320 may be optional in certain embodiments or may occur prior to operation 302 .
If, in operation 320 , the embodiment determines that the adapter is not connected to an external power source, then operation 322 is executed and the embodiment will conserve power of both the adapter battery 11 and the internal battery 38 . This may be accomplished in the embodiment shown in FIG. 2 by the microcontroller units 34 , 32 of the electronic device 12 and the battery 12 , which may transmit respective control signals to the chargers 36 , 30 to disable charging of the batteries 11 , 38 . After operation 322 , the method ends in operation 346 .
FIG. 3B is a flowchart illustrating another portion of the method initially discussed with respect to FIG. 3A . A positive determination in operation 320 of FIG. 3A , as discussed above, results in the embodiment entering operation 324 of FIG. 3B . In operation 324 , the embodiment determines whether the internal battery is at a low charge level. For example, referring to FIG. 2 , operation 324 , the microcontroller 34 of the electronic device 12 may be configured to receive a signal from the internal battery 38 indicating a level of charge of the battery 38 . The value of a “low charge level” may be set by the manufacturer or may, in certain embodiments, be user-specified. As one example, a 25% charge level may be considered low.
If, in operation 324 , the embodiment determines that the internal battery is not at a low charge level, then operation 326 is performed. In operation 326 , the embodiment determines whether the adapter battery is at a low charge level. As previously mentioned, this operation may be performed by the microcontroller 32 of the adapter 10 , which is configured to receive a signal from the adapter battery 11 indicating a level of charge of the battery 11 .
If, in operation 326 , the embodiment determines that the adapter battery is at a low charge level, then in operation 332 , the embodiment will run the electronic device from its internal battery. Referring to FIG. 2 , this may be accomplished by the device microcontroller unit 34 of the electronic device 12 , which may transmit a control signal to the charger 36 to disable charging, as well to the internal battery 38 to supply power to the other components of the electronic device 12 . Following operation 332 , the method terminates in end state 346 .
If, however, in operation 326 , the embodiment determines that the adapter battery is not at a low level, then in operation 328 , the embodiment will run the electronic device from the adapter battery. Although this may not be the most efficient use of power, since power will be lost as it is transferred from the adapter battery to the computer battery, this operation provides a practical benefit, in that internal battery power of the electronic device is preserved. Referring to FIG. 2 , this operation may be performed by transmitting a control signal from the device microcontroller unit 34 of the electronic device 12 to the internal charger 36 to supply voltage to the internal battery 38 . The adapter microcontroller unit 32 of the adapter 10 may also transmit a control signal to the adapter charger 30 enabling the charger 30 to supply voltage from the battery 11 to the boost converter 13 . In addition, the adapter microcontroller unit 32 may further transmit additional control signals to the boost converter 13 and the power switch 14 to perform their respective functions. Following operation 328 , the method terminates in operation 346 .
Returning to operation 324 , the embodiment may determine that the internal battery is at a low charge level. If so, operation 330 is accessed and the embodiment determines if the internal battery is at a very low charge level. Again, this may be determined by the microcontroller 34 of the electronic device 12 , which receives information from the internal battery 38 indicating the charge level of the battery 38 . As with the low battery level, the “very low” battery level may be specified by a third party such as a manufacturer or may be user-specified. As one example, a 10% charge may be a very low battery charge level.
If, in operation 330 , the embodiment determines that the internal battery is at a very low level, then operation 334 is executed and the embodiment determines if the adapter battery is also at a low level. This may be determined by the microcontroller 32 of the adapter 10 , which may receive information from the adapter battery 11 indicating whether the charge level of the battery 11 is very low.
If, in operation 334 , the embodiment determines that the adapter battery is at a low level, then operation 336 is accessed and the embodiment will force the adapter and the electronic device to go into sleep mode, or to shut down. This may be accomplished in the embodiment shown in FIG. 2 by transmitting a control signal from the adapter microcontroller unit 32 to the adapter charger 30 to disable charging of the adapter battery. Similarly, the device microcontroller unit 34 of the electric device 12 may also transmit a signal to the charger 36 to disable charging of the internal battery 38 . Further, the microcontroller unit may transmit a control signal to the other components of the electronic device 12 to initiate shut down or power off procedures for the electronic device 12 . After operation 336 , the method terminates in end state 346 .
On the other hand, if the embodiment determines in operation 334 that the adapter battery is not at a low level, then in operation 338 , the embodiment will charge the internal battery from the adapter battery. As previously described with respect to operation 328 , this may be accomplished via the device microcontroller unit 34 of the electronic device 12 , which may transmit a control signal to the internal charger 36 to supply voltage to the internal battery 38 . Following operation 338 , end state 346 is entered.
Returning to operation 330 , the embodiment may determine that the internal battery is not at a very low level. In this case, the embodiment executes operation 340 and determines if the adapter battery is at a low level. As previously described, this may be accomplished by the adapter microcontroller unit 32 of the adapter 10 , which is configured to receive information indicating a charge level of the adapter battery 11 .
If, in operation 340 , the embodiment determines that the adapter battery is at a low level, then in operation 336 , the embodiment will force the adapter and the electronic device to go into sleep mode, or to shut down. By contrast, if the embodiment determines that the adapter battery is not at a low level in operation 340 , then the embodiment will run the electronic device from the adapter battery in operation 328 . The implementation of these operations, for example, in the embodiment illustrated in FIG. 2 , may be the similar to that previously discussed with respect to steps 334 , 336 and 338 .
Generally, the foregoing methods of operation have been described and indication has been provided as to what components execute certain operations. It should be appreciated that either microcontroller unit 34 , 36 may accomplish or execute functionality described herein that is ascribed to the other unit with appropriate configuration. Likewise, various other operations ascribed to particular hardware elements may be carried out by different elements. Accordingly, the foregoing discussion of particular operations being carried out by particular hardware is provided for illustration only.
FIG. 4 illustrates another embodiment of an electronic device 700 having two batteries 703 , 705 that are located inside the housing 701 of the device 700 . Each battery 703 , 705 , may be connected to a charger 707 configured to charge the batteries 703 , 705 . In other embodiments, there may be more than one charger 707 provided in the electronic device 700 for example, the device 700 may include one charger 707 provided for each battery 703 , 705 of the device 700 . A microcontroller unit 709 may be connected to the charger 707 and configured to enable the charger 707 to charge the batteries 703 , 705 by supplying voltage received through an input power line 16 that may include a cord and a corresponding plug 20 connected to a power supply 17 . Although an electronic device 700 is illustrated in FIG. 7 , one of ordinary skill in the art will appreciate that the present invention also encompasses an adapter having multiple battery packs.
Although the present invention has been described with respect to particular embodiments and methods of operation, it should be understood that changes to the described embodiments and/or methods may be made yet still embraced by alternative embodiments of the invention. For example, certain embodiments may omit or add operations to the methods and processes disclosed herein. Accordingly, the proper scope of the present invention is defined by the claims herein. | An adapter including an associated battery capable of powering an electronic device. The power adapter typically includes the battery as an integral component that is connected to a plug or other interface capable of mating with a power source, such as a wall socket. Thus, the adapter battery may provide power either to operate the device or charge a battery within (or otherwise associated with) the device even if the adapter is not connected to a power source. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of Korean Application No. 2002-18377, filed Apr. 4, 2002, in the Korean Patent Office, the disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to microwave ovens, and more particularly to an apparatus and a method of controlling a microwave oven, which can cook foods under optimal cooking conditions regardless of surrounding humidity conditions by compensating for variation of cooking conditions due to the surrounding humidity conditions.
2. Description of the Related Art
Generally, when rice is cooked in a conventional microwave oven, a first heating is performed until rice water reaches a boiling point of 100° C., and then a second heating is performed for a predetermined period of time after the rice water reaches the boiling point using an output power of a magnetron lower than that of the first heating.
The microwave oven is not equipped with a temperature sensor and thus, detects the boiling of the rice water using a detection value from a humidity sensor, which senses a humidity value of water vapor discharged from a cooking chamber so as to detect the boiling point of the rice water.
FIG. 1A is a waveform diagram showing a relationship between sensing voltages of a humidity sensor and time in the conventional microwave oven. FIG. 1B is a waveform diagram showing a relationship between output powers of a magnetron and time in the conventional microwave oven. FIG. 1C is a waveform diagram showing a relationship between boiling temperatures of water and time in the conventional microwave oven. As shown in FIG. 1A, at a beginning of heating food, the output power of the magnetron is maximized to rapidly heat the food, and then, the output power is gradually lowered while continuing to heat the food. If the rice water boils, rice continues to be heated using low output power suitable for steaming boiled rice, so the rice is cooked. Accordingly, the humidity value sensed by the humidity sensor is a constant value at the start of cooking, rapidly increasing when rice water reaches the boiling point, and gradually decreasing thereafter.
A sensing voltage graph of the humidity sensor, as shown in FIG. 1A, shows a variation of the humidity value. A reference value (T1 FACTOR) of the humidity sensor, corresponding to the boiling point (100° C.) of the rice water, is estimated on a basis of sensing voltage values. Generally, the reference value is uniformly set at a value of, for example, 85% of a maximum voltage MAX of the sensing voltages on a basis of a normal surrounding humidity condition.
However, a sensor for sensing relative humidity, not absolute humidity, is mainly used as the humidity sensor due to problems such as cost, etc. Then, if the surrounding humidity condition of the microwave oven is lower than that of a normal state, that is, a dry state, such as during Winter, the maximum voltage MAX sensed by the humidity sensor is relatively increased. Therefore, the voltage at 85% of the maximum voltage does not reflect the boiling point of rice water. Consequently, the output power of the magnetron is decreased to output a low output power suitable for steaming the rice before the rice water boils, thus causing rice to be half-cooked.
SUMMARY OF THE INVENTION
Various objects and advantages of the invention will be set forth in part in the description that follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Accordingly, the present invention has been made keeping in mind the above problems occurring in the related art, and an object of the present invention is to provide a method of controlling a microwave oven to cook foods under optimal cooking conditions regardless of a surrounding humidity condition, by compensating for a variation of cooking conditions due to the surrounding humidity condition.
To achieve the above and other objects, the present invention provides a method of controlling a microwave oven, including: performing a first heating until detection values of a humidity sensor reach a reference value, wherein the humidity sensor senses humidity of water vapor discharged from a cooking chamber; performing a second heating, lower than the first heating, after the detection values reach the reference value using an output power from a magnetron; determining a surrounding humidity condition of the microwave oven; and resetting the reference value of the first heating so as to cook food appropriately
Further, to achieve the above and other objects, the present invention provides a method of controlling a microwave oven, including: performing a first heating until detection values of a humidity sensor reach a reference value, wherein the humidity sensor senses humidity of water vapor discharged from a cooking chamber; performing a second heating, lower than that of the first heating, for a set period of time after the detection values reach the reference value using an output power from a magnetron; determining a surrounding humidity condition of the microwave oven; and resetting a period of time for the second heating so as to cook food appropriately according to the determined humidity condition.
To achieve the above and other objects, the present invention provides a control method of a microwave oven, including: maximizing an output power; counting a first heating time; reading sensing voltages from a humidity sensor during the first heating time; comparing the sensing voltages sensed by the humidity sensor with each other to determine a maximum voltage; setting a first reference value at a predetermined voltage level from the maximum voltage; determining whether a current sensing voltage sensed by the humidity sensor has reached the first reference value; decreasing the output power to a low power; determining whether the current mode is in a dry mode or a normal mode; setting a preset time as a reference period of time for a second heating time corresponding to the counted heating time; outputting the low power for a predetermined period of time of the second heating time; increasing the output power of the microwave oven to perform a cooking operation after the predetermined period of time of the second heating time elapses; and stopping the cooking operation of the microwave oven after the second heating time has elapsed.
To achieve the above and other objects, the present invention provides an apparatus to control a microwave oven, including: a control unit counting a time from a start of heating to a time point when a first reference value is detected, comparing the counted heating time with a predicted heating time preset; and determining a current mode as a dry mode when the counted heating time is shorter than the predicted heating time.
To achieve the above and other objects, the present invention provides an apparatus to control a microwave oven, including: a control unit determining a surrounding humidity condition of the microwave oven, and compensating for a variation of heating time due to the surrounding humidity of the microwave oven according to seasons or areas in which the microwave oven is used to provide an optimal heating time enabling the microwave oven to optimally cook food, regardless of surrounding conditions.
To achieve the above and other objects, the present invention provides a method of controlling a microwave oven, including: counting a time from a start of heating to a time point when a first reference value is detected; comparing the counted heating time with a predicted heating time preset; and determining a current mode as a dry mode when the counted heating time is shorter than the predicted heating time.
To achieve the above and other objects, the present invention provides a method of controlling a microwave oven, including: determining a surrounding humidity condition of the microwave oven; and compensating for a variation of heating time due to the surrounding humidity of the microwave oven according to seasons or areas in which the microwave oven is used to provide an optimal heating time enabling the microwave oven to optimally cook food, regardless of surrounding conditions.
These together with other objects and advantages, which will be subsequently apparent, reside in the details of construction and operation as more fully hereinafter described and claimed, reference being had to the accompanying drawings forming a part thereof, wherein like numerals refer to like parts throughout.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and other advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1A is a waveform diagram showing a relationship between sensing voltages of a humidity sensor and time in the conventional microwave oven when a surrounding humidity of the microwave oven is in normal and dry states;
FIG. 1B is a waveform diagram showing a relationship between output powers of a magnetron and time in the conventional microwave oven when the surrounding humidity of the microwave oven is in the normal and dry states;
FIG. 1C is a waveform diagram showing a relationship between boiling temperatures of water and time in the conventional microwave oven when the surrounding humidity of the microwave oven is in the normal and dry states;
FIG. 2 is a top sectional view showing a construction of a microwave oven according to an embodiment of the present invention;
FIG. 3 is a block diagram of the microwave oven of FIG. 2;
FIG. 4 is a flowchart of a method of controlling the microwave oven according to an embodiment of the present invention;
FIGS. 5A and 5B are graphs showing first and second reference values of FIG. 4;
FIG. 6 is a flowchart of another microwave oven control method to change a second heating time in a dry mode, according to another embodiment of the present invention; and
FIG. 7 is a waveform diagram showing sensing voltages of a humidity sensor to describe a method of determining a mode of FIGS. 4 and 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Hereinafter, embodiments of the present invention will be described in detail with reference to the attached drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein; rather, these embodiments are provided so that the present disclosure will be thorough and complete, and will fully convey the concept of the invention to those skilled in the art.
FIG. 2 is a top sectional view showing the construction of a microwave oven according to an embodiment of the present invention. Referring to FIG. 2, the microwave oven of the present invention includes a body 10 , which constitutes an external shape of the microwave oven and defines a cooking chamber 12 and a machine room 11 separately partitioned. A door 13 is connected to the body 10 by a hinge to open and shut the cooking chamber 12 , a control panel 14 is installed on a front of the body 10 and provided with a plurality of functional buttons thereon, and a humidity sensor 17 senses a humidity of the cooking chamber 12 .
The cooking chamber 12 opens at the front of the body 10 , where a cooking tray 12 a in a form of a turntable is installed on a bottom portion of the cooking chamber 12 and a motor is installed under the cooking tray 12 a to rotate the cooking tray 12 a. Further, an inlet 15 a, communicating with the machine room 11 to suck the external air into the cooking chamber 12 , is formed on a front portion of one sidewall 15 of the cooking chamber 12 . Further, an outlet 16 a is formed on a back portion of another sidewall 16 of the cooking chamber 12 to discharge the air in the cooking chamber 12 to the outside.
Further, in the machine room 11 , a magnetron 1 a is installed to oscillate microwaves, a cooling fan 11 b is installed to suck the external air to cool the machine room 11 and the cooking chamber 12 , and a guide duct 11 c is installed to guide the air in the machine room 11 to the inlet 15 a. The cooling fan 11 b is disposed between a magnetron 11 a and a back wall of the machine room 11 . A plurality of suction holes 11 d are formed on the back wall of the machine room 11 to suck the external air into the machine room 11 .
The humidity sensor 17 is mounted on the sidewall 16 of the cooking chamber 12 adjacent to the outlet 16 a to be disposed along the air discharging path of the cooking chamber 12 . Therefore, the humidity sensor 17 senses the humidity of the air being discharged from the cooking chamber 12 through the outlet 16 a. The humidity sensor 17 is electrically connected to a control unit formed on the control panel 14 , as will be described later.
FIG. 3 is a block diagram of the microwave oven according to an embodiment of the present invention. Referring to FIG. 3, the microwave oven includes a control unit 30 to control operations of the microwave oven. The control unit 30 is connected to an input unit 14 a arranged in the control panel 14 to allow a user to input operation commands, such as rice cooking for one person and two persons. Further, the control unit 30 is connected to the humidity sensor 17 to sense humidity.
Further, the microwave oven has a storage unit 20 electrically connected to the control unit 30 , to store various data for cooking. Furthermore, the control unit 30 is electrically connected to a magnetron driving unit 41 to drive the magnetron 11 a, a fan driving unit 42 to drive the cooling fan 11 b, a motor driving unit 43 to drive a motor 12 b for rotating the cooking tray 12 a, and a display driving unit 44 to drive a display unit 14 b arranged on the control panel 14 to display information. When the user manipulates the input unit 14 a of the control panel 14 to operate the microwave oven, the microwave oven according to an embodiment of the present invention cooks food placed on the cooking tray 12 a by radiating microwaves that are oscillated by the magnetron 11 a to the cooking chamber 12 .
Further, the external air is sucked into the machine room 11 through the suction holes 11 d to cool the machine room 11 by the action of the cooling fan 11 b during a cooking operation of the microwave oven, and is provided to the cooking chamber 12 through the guide duct 11 c and the inlet 15 a. Then, the air in the cooking chamber 12 is discharged to the outside through the outlet 16 a, together with water vapor generated from the food, as shown by an arrow in FIG. 3 . Accordingly, odor and water vapor can be eliminated from the cooking chamber 12 . In this case, the air in the cooking chamber 12 is discharged to the outside while being brought into contact with the humidity sensor 17 , so the humidity sensor 17 senses water vapor contained in the discharged air and transmits the sensed water vapor to the control unit 30 as electrical signals. The control unit 30 recognizes such electrical signals as voltage values. The control unit 30 drives the magnetron 11 a, the motor 12 b and the cooling fan 11 b to automatically cook the food based on the electrical signals received from the humidity sensor 17 .
Hereinafter, a method of controlling a microwave oven to cook rice according to an embodiment of the present invention will be described in detail. FIG. 4 is a flowchart of a method of controlling the microwave oven according to an embodiment of the present invention. Referring to FIG. 4, the user places a bowl, in which rice and a suitable quantity of water are mixed, in the cooking chamber 12 so as to cook the rice. The user then selects a cooking course for one person or two persons through the input unit 14 a. At S 10 , the control unit 30 heats the food by driving the magnetron 11 a to maximize its output power. At S 11 , the control unit 30 counts a first heating time.
At S 12 , the control unit 30 reads sensing voltages from the humidity sensor 17 for a predetermined period of time of the first heating time. At S 13 , the control unit 30 compares the sensing voltages sensed by the humidity sensor 17 with each other and determines a maximum voltage.
If the maximum voltage is determined, at S 14 , the control unit 30 sets a voltage at 85% of the maximum voltage as a first reference value. At S 15 , the control unit 30 determines whether a current sensing voltage determined from the humidity sensed by the humidity sensor 17 has reached the first reference value. In this case, the first reference value is a humidity value when the temperature of water reaches the boiling point (100° C.), the humidity value being obtained through experiments to determine the humidity and the temperature of water when a surrounding humidity condition of the microwave oven is normal.
At S 15 , if the current sensing voltage has reached the first reference value, at S 16 , the control unit 30 determines whether a current mode is in a dry mode or a normal mode by a mode determining method to be described later.
If it is determined that the current mode is in the normal mode, at S 19 , the control unit 30 decreases the output power of the magnetron 11 a to a low power suitable for steaming boiled rice, and stops the counting of the heating time. Then, at S 20 , the control unit 30 sets a preset time as a reference period of time for a second heating (second heating time) corresponding to the counted heating time.
If the second heating time is set, during the second heating time, at S 21 , the control unit 30 operates the magnetron 11 a to output the low power required to steam boiled rice for a predetermined period of time of the second heating time, while the control unit 30 increases the output power of the magnetron 11 a to perform a cooking operation after the predetermined period of time of the second heating time elapses. At S 22 , after the second heating time has elapsed, the control unit 30 stops the driving of the magnetron 11 a. At S 23 , the control unit 30 finishes the cooking.
Further, at S 16 , if the current mode is in the dry mode, at S 17 , the control unit 30 sets a second reference value (a voltage at 83% of the maximum voltage) lower than the first reference value, instead of the first reference value, so as to heat the food a little longer, as shown in FIGS. 5A and 5B. Accordingly, as shown in FIGS. 5A and 5B, a reference value is decreased to a voltage at 83%, lower that the previous 85%, of the maximum voltage, such that a time taken for the sensing voltage to reach the reference value is lengthened, thus allowing the food to be heated a little longer.
At S 17 , if the second reference value is set, at S 18 , the control unit 30 determines whether the current sensing voltage has reached the second reference value. At S 18 , if the current sensing voltage has reached the second reference value, at S 19 , the control unit 30 decreases the output power of the magnetron 11 a to the low power suitable to steam boiled rice, and stops the counting of the heating time. At S 20 , the control unit 30 sets a preset time corresponding to the counted heating time as the second heating time.
During the second heating time, at S 21 , the control unit 30 operates the magnetron 11 a to output the low power required to steam boiled rice for a predetermined period of time of the second heating time, while the control unit 30 increases the output power of the magnetron 11 a to perform the cooking operation after the predetermined period of time of the second heating time elapses. At S 22 , after the second heating time has elapsed, at S 23 , the control unit 30 stops the driving of the magnetron 11 a and finishes the cooking.
FIG. 6 is a flowchart of another microwave oven control method of changing the second heating time in a dry mode instead of the reference value during the first heating, according to another embodiment of the present invention.
Referring to FIG. 6, at S 100 , the control unit 30 heats the food by driving the magnetron 11 a to maximize the output power, and, at S 101 , counts the first heating time. At S 102 , the control unit 30 reads the sensing voltages from the humidity sensor 17 for a predetermined period of time of the first heating time. Further at S 103 , the control unit 30 compares the sensing voltages sensed by the humidity sensor 17 with each other, and sets the maximum voltage.
If the maximum voltage is set, at S 104 , the control unit 30 sets a voltage at 85% of the maximum voltage as a first reference value. At S 105 , the control unit 30 determines whether the current sensing voltage determined from the humidity sensed by the humidity sensor 17 has reached the first reference value.
At S 105 , if the current sensing voltage has reached the first reference value, at S 106 , the control unit 30 decreases the output power of the magnetron 11 a to a low power suitable for steaming boiled rice, and stops the counting of the heating time. Then, at S 107 , the control unit 30 determines whether the current mode is in the dry mode or the normal mode by a mode determining method to be described later If the current mode is in the normal mode, at S 108 , the control unit 30 sets a preset time as the second heating time corresponding to the counted heating time.
If the second heating time is set, at S 109 , during the second heating time, the control unit 30 operates the magnetron 11 a to output low power required to steam boiled rice for a predetermined period of time of the second heating time, while the control unit 30 increases the output power of the magnetron 11 a to perform a cooking operation after the predetermined period of time of the second heating time elapses. After the second heating time has elapsed, at S 110 and S 111 , the control unit 30 stops the driving of the magnetron 11 a and finishes the cooking.
Further at S 106 , if the current mode is in the dry mode, at S 120 , the control unit 30 sets the second heating time to be longer than the preset time. If the second heating time is set, at S 109 , during the second heating time, the control unit 30 operates the magnetron 11 a to output low power required to steam boiled rice for a predetermined period of time of the second heating time, while the control unit 30 increases the output power of the magnetron 11 a to perform a cooking operation after the predetermined period of time of the second heating time elapses. After the second heating time has elapsed, at S 110 and S 111 , the control unit 30 stops the driving of the magnetron 11 a and finishes the cooking.
Hereinafter, the dry mode determining method of FIGS. 4 and 6 is described. There are two methods to determine the dry mode of FIGS. 4 and 6.
A first method is performed by determining the current mode as the dry mode if a voltage waveform between points A and B ascends as shown in FIG. 7, and by determining the current mode as the normal mode if the voltage waveform is constant or descends. That is, sensing voltages sensed by the humidity sensor 17 for a predetermined period of time are compared with each other, such that the current mode is determined as the dry mode if the sensing voltages are gradually increased. Alternatively, the maximum voltage is set by comparing sensing voltages sensed by the humidity sensor 17 for a predetermined period of time with each other, and if a voltage at the start of heating is less than the maximum voltage, the current mode is determined as the dry mode. This determination is due to a phenomenon where if the surrounding humidity of a microwave oven is decreased, the humidity within the cooking chamber is affected to cause the waveform of the sensing voltages of the humidity sensor 17 to ascend.
A second method is performed by counting a time from the start of heating to a time point when the first reference value is detected, comparing the counted heating time with a predicted heating time preset for a case where the surrounding humidity of the microwave oven is normal, and determining the current mode as the dry mode if the counted heating time is shorter than the predicted heating time. The second method considers that, when the surrounding humidity of the microwave oven is in the dry mode, heating time becomes shorter than that of a normal mode.
As described above, the present invention provides a method of controlling a microwave oven, which provides an optimal heating time by compensating for a variation of heating time due to surrounding humidity of the microwave oven according to seasons or areas in which the microwave oven is used, thus enabling the microwave oven to optimally cook food, regardless of surrounding conditions.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. | An apparatus and a method of controlling a microwave oven includes performing a first heating until detection values of a humidity sensor reach a reference value, wherein the humidity sensor senses humidity of water vapor discharged from a cooking chamber. A second heating is performed, lower than the first heating, after the detection values reach the reference value using an output power from a magnetron. A surrounding humidity condition of the microwave oven is determined. The reference value of the first heating is reset so as to cook food appropriately according to the determined humidity condition. | 7 |
SUMMARY
[0001] The present invention provides method and apparatus for a linear sensor integrated circuit (IC) that provides output signals to control a motor, such as a coil motor, to control a lens in auto focus digital camera applications. The current in the coil to drive the motor changes until the position of the external lens assembly or CCD array results in a sensor, such as a Hall effect sensor, having a voltage that matches the input signal position command. With digital RC filter operation, which enables resource sharing, a cost effective device and compact device is provided.
[0002] In one aspect of the invention, an integrated circuit comprises: a position sensor to sense the position of a ferromagnetic target and generate a target position signal, a scaling block to receive the target position signal, a digital RC filter to receive the target position signal, a reference position, and a scale factor, and generate an output, the RC filter including: a multiplier to multiply the scale factor and a difference of the reference position and the target position signal, and a bit shifter for dividing by some factor of two, wherein all division for computations in the RC filter are performed by bit shifts, a PID controller coupled to the RC filter to receive the output from the RC filter, and an output driver to provide a position output signal.
[0003] The integrated circuit can further include one or more of the following features: computations in the RC filter and computations in the scaling block share a multiplier, the target includes a lens having a ferromagnetic material for camera auto focus, the position sensor includes a Hall element, the PID controller receives position information from the position sensor, wherein the digital filter computes y[n+1]+(y[n]*2 z +k*(x−y[n]))/2 z , where x is a position value, k is a scaling value, z is a positive integer, and y is the output to the PID, and/or the output driver is configured to generate the position output signal to an actuator coil.
[0004] In another aspect of the invention, a system comprises a camera having auto-focus capability, the camera comprising: a position sensor to sense the position of a ferromagnetic target and generate a target position signal, a scaling block to receive the target position signal, a digital RC filter to receive the target position signal, a reference position, and a scale factor, and generate an output, the RC filter including: a multiplier to multiply the scale factor and a difference of the reference position and the target position signal, and a bit shifter for dividing by some factor of two, wherein all division for computations in the RC filter are performed by bit shifts, a PID controller coupled to the RC filter to receive the output from the RC filter, and an output driver to provide a position output signal.
[0005] The system can further include one or more of the following features: computations in the RC filter and computations in the scaling block share a multiplier, the target includes a lens having a ferromagnetic material for camera auto focus, the position sensor includes a Hall element, the PID controller receives position information from the position sensor, wherein the digital filter computes y[n+1]=(y[n]*2 z +k*(x−y[n]))/2 z , where x is a position value, k is a scaling value, z is a positive integer, and y is the output to the PID, and/or the output driver is configured to generate the position output signal to an actuator coil.
[0006] In a further aspect of the invention, a system comprises: a camera having auto-focus capability, the camera comprising: means for sensing a position of a ferromagnetic target; a digital RC filter means coupled to the means for sensing a position for generating an output, the digital RC filter including: a multiplier to multiply the scale factor and a difference of the reference position and the target position signal, and a bit shifter for dividing by some factor of two, wherein all division for computations in the RC filter are performed by bit shifts, a PID controller means coupled to the RC filter to receive the output from the RC filter; and an output driver means coupled to the PID controller means.
[0007] In another aspect of the invention a method comprises: employing a position sensor to sense the position of a ferromagnetic target and generate a target position signal, employing a scaling block to receive the target position signal, employing a digital RC filter to receive the target position signal, a reference position, and a scale factor, and generate an output, the RC filter including: a multiplier to multiply the scale factor and a difference of the reference position and the target position signal, and a bit shifter for dividing by some factor of two, wherein all division for computations in the RC filter are performed by bit shifts, employing a PID controller coupled to the RC filter to receive the output from the RC filter, and employing an output driver to provide a position output signal.
[0008] The method can further include one of more of: computations in the RC filter and computations in the scaling block share a multiplier, the target includes a lens having a ferromagnetic material for camera auto focus, and/or the digital filter computes y[n+1]=(y[n]*2 z +k*(x−y[n]))/2 z where x is a position value, k is a scaling value, z is a positive integer, and y is the output to the PID.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The foregoing features of this invention, as well as the invention itself, may be more fully understood from the following description of the drawings in which:
[0010] FIG. 1 is a schematic representation of a position sensor and driver in accordance with exemplary embodiments of the invention;
[0011] FIG. 2 is a schematic representation of a PID controller;
[0012] FIG. 3 is a schematic representation of a RC filter and scaling block;
[0013] FIG. 3A is a schematic representation of scaling block operation for the implementation of FIG. 3 ;
[0014] FIG. 3B is a schematic representation of RC filter operation for the implementation of FIG. 3 ;
[0015] FIG. 4 is a schematic representation of a PID block for the implementation of FIG. 2 ; and
[0016] FIG. 5 is an exemplary implementation of a camera having an integrated circuit position sensor and driver.
DETAILED DESCRIPTION
[0017] FIG. 1 shows a system 100 having digital auto-focus in accordance with exemplary embodiments of the invention. A sensor 102 , such as a Hall effect sensor, determines a position of a magnet on the target, e.g., lens, that is provided to a digital proportional-integral-derivative (PID) controller 104 . The PID controller 104 is connected to an output driver 106 that provides output signals 106 a,b that can be coupled to an actuator coil 10 for moving the lens. A controller 108 controls overall operation of the device and an interface 110 provides serial, for example, communication with a processor, microcontroller or other device.
[0018] In an exemplary embodiment, the sensor 102 signal is amplified 120 , filtered 122 , and converted by an ADC 124 from an analog to a digital signal, which is input to the PID controller 104 . The output of the PID controller 104 is converted by a DAC 126 from a digital to an analog signal before being sent to the output driver 102 .
[0019] A series of registers 130 are coupled to the controller 108 and output driver 102 to store various information including position information, PID information, such as coefficients, ADC/DAC information, calibration information, bit shift information, etc. The registers 130 are available for read/write operations via the interface 110 over the serial SDA, SCL lines. An EEPROM and controller 132 are coupled to the registers and to the SCL line for programming operations. It is understood that any suitable memory device can be instead of, or in addition to, an EEPROM.
[0020] FIG. 2 shows further detail for the PID controller 104 of FIG. 1 . In general, the PID controller 104 calculates an error value between the Hall effect sensor 102 ( FIG. 1 ) and a target 10 , e.g., lens, location programmed by the user, for example. In exemplary embodiments, coefficients for the PID controller 104 are selected to minimize controller error and reduce settling time.
[0021] Position information, shown as ten bits, is provided to a calibration scaling block 150 , which provides scaled lens position information to a RC filter 152 . The PID block 154 receives an output from the digital RC filter 152 and processes the filtered signal to provide an output control signal to adjust the lens position.
[0022] The calibration scaling block 150 receives positive register 152 and negative register 154 information during calibration. The lens can be driven to a first maximum position and the location stored, such as in a PREG register, and then driven to a second maximum position, opposite the first, and this location stored in a DREG register. This aligns the range of travel across the resolution of the device.
[0023] The scaled position information is provided to a digital RC filter 152 , which outputs filtered and signed position information to the PID block 154 . The RC filter provides a smooth change in the reference position on the PID controller. Information, e.g., voltage, is provided from the Hall sensor to the PID block 154 , which outputs control information that can be used to move the lens.
[0024] FIG. 3 shows an exemplary implementation of the calibration scaling block 150 and RC filter 152 of FIG. 2 . A programmable digital approximation of an RC filter is used as the input filter to a ND (proportional, integral, derivative) controller, such as the PID block 154 of FIG. 2 . An exemplary position update implementation is set forth below:
[0000] y[n+ 1]= y[n]+k* ( x[n]−y[n] )
[0000] where, x is the desired input position to the PID controller, y is the reference position sent to the PID controller, and k is a scale value between 0 and 1. When x is abruptly changed, y will move toward x with an exponential behavior similar to an RC analog filter response to a step input. The effective time constant of this digital RC approximation can be programmed by changing either k and/or the update rate.
[0025] In an exemplary embodiment, space expensive division is avoided by modifying the equation to require division only by a factor of two, which can be accomplished with bit shifts. An exemplary transformed equation is set forth below:
[0000] y[n+ 1]=( y[n]* 2 z +k* ( x−y[n] ))/2 z
[0000] which provides division by 2̂z, Where z is a positive integer and k is an integer between 0 and 2̂z. This digital RC could be used as the input filter for any controller, including both analog and digital.
[0026] After running calibration, PREG and NREG contain the actual maximum and minimum values needed for full lens travel. In one embodiment, only the most significant 8 bits out of the 12 bit ADC are stored in PREG and NREG, effectively rounding the saved calibration values. In the illustrated embodiment, the user input position value POS is ten bits and should represent the full lens travel range. Thus, a user POS value of 0x0 needs to map to the rounded, twelve bit NREG value and a user POS value of 0x3FF needs to map to the rounded, twelve bit PREG value, To rescale the POS values the following can be used:
[0000] X =(( P REG− N REG)×POS)/1024+ N REG
[0000] where PREG and NREG are 12 bits wide with the top 8 bits being those in the PREG and NREG registers and the bottom 4 bits being zero for minimized multiplier size. Then X is the 12 bit output which is provided as input for the RC filter. In one embodiment, there is a small approximation since POS should be divided by 1023. However, dividing by 1024 allows for the division to be done by a bit shift. The order of operations requires that the multiplication of POS by (PREG−NREG) is done before the division to improve accuracy.
[0027] It is understood that the resealing event may only need to occur when a new POS, PREG, or NREG value is loaded. Other than that, the multiplier is an available resource that will be shared with the RC Filter logic described below.
[0028] There is a need to allow any changes of the POS value to be implemented as an RC curve. In an exemplary embodiment, the following is used:
[0000] y[n+ 1]=( y[n]* 2 10 +k* ( x−y[n] ))/2 10
[0000] where x is the 12 bit resealed user POS value, k is a scaling value, and y is the output to the PID. The order of operations requires that the downshift be performed at the end allowing for a multiplier to be of a smaller size and still retain the accuracy in the equation.
[0029] It should be noted that the effective value of k is scaled down by 1024 due to the ‘2 10 ’ scaling terms in the equation. The selectable scaling ranges allows for k to be represented by a 1 to 8 bit number which allows for easy sharing of the multiplier with the resealing logic, In FIG. 3 , it is shown that for this embodiment, k was chosen to be 6 bits wide with the top two bits of the 8 bit value going into the multiplier being fixed at zero.
[0030] FIG. 3A shows the path during calibration scaling. In accordance with
[0000] X= (( P REG− N REG)×POS)/1024+ N REG,
[0000] NREG( 7 : 0 ) is subtracted from PREG( 7 : 0 ) at summer 302 having an output which passes through a multiplexer 304 to a multiplier 306 , which receives POS( 9 : 0 ) via multiplexer 308 . The multiplier 306 output passes through demultiplexer 310 to summer 312 , which has NREG( 7 : 0 ) as in input. The output of the summer 312 is twelve bit POS scaling information.
[0031] FIG. 3B shows the RC filter implementation path. Scaling value k RC_scale[ 5 : 0 ] passes though multiplexer 304 to the multiplier 306 . Value y[n]*2 z , which is stored from the last update in RC filter register 314 and bit shifted 315 to achieve division by 2̂10 is provided to summer 316 for subtraction from the scaled position value (x in the equation). The output of the summer 316 (x-y[n]) is provided to the multiplier 306 via multiplexer 308 . The multiplier 306 output (k*(x-y[n])) passes through demultiplexer 310 to summer 318 for addition with the value in the RC filter register) (y[n]*2 10 ). The summer 318 output is then provided to the RC filter register 314 and then to a bit shift module 320 to provide the RC filter output (y[n+1]), which is sent to the PID block.
[0032] With this arrangement, the multiplier 306 is used for scaling and RC filter operations. As can be seen, division by a factor of 2 is achieved by bit shifts. By implementing division in bit shift operations, significant space savings are achieved as compared with divisions which cannot be performed with bit shifting alone.
[0033] FIG. 4 shows an exemplary PID implementation 400 in which the RC filter output 402 and the Hall sensor output 404 are provided as PID inputs. The PID output provides a control signal for the coil to control the target, e.g., lens, movement. It is understood that PID blocks are well known in the art.
[0034] FIG. 5 shows an exemplary circuit diagram of a camera 500 having a position sensor and driver integrated circuit 502 to sense a position of a target, such as a lens, and to generate a drive signal to actuate a motor until a desired position for the target is achieved. In one embodiment, the sensor is provided as a Hall effect sensor to generate a voltage corresponding to a ferromagnetic target location on a lens in an auto-focus module 504 . In one embodiment, the ferromagnetic target comprises a hard ferromagnetic material, such as a permanent magnet.
[0035] It is understood that a position sensor can include a variety of magnetoresistive devices, such as giant magnetoresistance (GMR), anisotropic magnetoresistance (AMR), and the like. In one embodiment, the integrated circuit includes a Hall effect sensor and a magnetoresistive sensor.
[0036] Having described exemplary embodiments of the invention, it will now become apparent to one of ordinary skill in the art that other embodiments incorporating their concepts may also be used. The embodiments contained herein should not be limited to disclosed embodiments but rather should be limited only by the spirit and scope of the appended claims. All publications and references cited herein are expressly incorporated herein by reference in their entirety. | Methods and apparatus for providing a position sensor to sense the position of a ferromagnetic target and generate a target position signal, a scaling block to receive the target position signal, and a digital RC filter to generate an output using bit shifting for dividing by some factor of two, wherein all division for computations in the RC filter are performed by bit shifts. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains to a carbonated water dispenser having an improved carbonated water distribution manifold connected to several post-mix dispensing valves, to an improved carbonated water distribution manifold, and to a method of making an improved carbonated water distribution manifold.
2. The Prior Art
A post-mix carbonated beverage dispensing system makes its own carbonated water from a supply of municipal or well water, and then distributes the carbonated water to a plurality of post-mix valves. Each post-mix valve mixes carbonated water with syrup and effects dispensing of a complete beverage. These dispensers are typically found in fast food retailers, theatres, convention centers, sports facilitates and the like, and are most often used to fill cups with beverage.
Most of all these plural flavor post-mix dispensers have some type of structure to distribute carbonated water from a single or plural carbonator to a plurality of dispensing valves. There typically will be a minimum of four dispensing valves and it is common to see up to eight dispensing valves being supplied from a single carbonator.
The structure that distributes the carbonated water has been a continual source of problems and a cause of decarbonation and foaming during dispensing. One structure for distributing carbonated water was a molded plastic housing with metal ferrules for an inlet and plural outlets.
These devices had to be located remote from the cooling structure and during stand by time, carbonated water in the housing would warm up and decarbonate. Leakage, ferrule breakage, stress cracks and sanitation were also continually reoccurring problems.
A metal block with a bored out center section, with bored and tapped transverse aperture with adapter fittings has also been used. These are expensive, heavy, bulky, leaky, very difficult to sanitize and are not an effective solution.
The most recently commercially used structure for distributing carbonated water is a manifold made of a elongate length of stainless steel tubing forming an elongate plenum.
At least one end of the tube is closed and the other end may be an inlet or may be closed. Several transverse fittings are welded into apertures drilled transversely into the plenum tube. The transverse fittings are then welded into the plenum tube. This structure has been in use for several years and is the least costly, and most structurally efficient known device for distributing carbonated water in a dispenser.
The problem is that it may or may not properly dispense carbonated water and beverage; you really don't know until the dispenser has been in use for a period of time. The problem results from the welding of the transverse fittings to the plenum tube. The weld usually breaks through at least one of the transverse tubes and causes an obstruction in the tube. Carbonated water flowing over the obstruction then decarbonates and the dispensing valve foams. A given manifold may have five good outlets and one bad outlet; it may have three bad outlets, it may have a bad inlet, it may be perfectly good. Whether the manifold is a good one or a defective one can't be visually determined. Consequently the quality control and quality repeatability of these manifolds is very poor. These manifolds are also a sanitary problem because of crevices in the weld, and/or crevices where the weld has not completely penetrated. The welds in this manifold cannot be viably inspected from the inside. The retailer or beverage entity that ends up with a defective manifold has to go through all kinds of exercise to determine the manifold is defective. Usually dispensing valves will be changed, sanitizing will be done, and a serviceman will attempt to adjust the dispenser.
This is a serious irritant and quality problem for the food and beverage industry. Carbonated water is a very unique and delicate substance to handle, convey and distribute, while preventing decarbonation and resultant foaming of beverage.
The existing manifolds are not good enough to be cast into aluminum cold plates for ice cooled dispensers because of poor welds, cracking, leaking, and the poor quality previously referred to may lead to the loss of a quite valuable casting because of a defective weld.
OBJECTS OF THE INVENTION
It is an object of the present invention to provide an improved cold carbonated beverage dispenser having consistent delivery of highly carbonated water equally to all dispensing valves with a predictable, constant and repeatable level of quality, and a multiple flavor post-mix dispenser which dispenses post-mix carbonated beverage without foaming decarbonation or bubbling from any one or more of the dispensing heads.
It is an object of the present invention to provide an improved carbonated water distribution manifold that is welded from the inside and which will predictably and consistently deliver carbonated water without decarbonation or pressure drop to each and every dispensing valve.
It is an object of the present invention to provide a method of making an improved carbonated water distribution manifold wherein unpredictable welding obstructions and crevices which cause pressure drop, decarbonation, obstructed flow, and sanitation problems are eliminated.
It is an object of the present invention to provide a dispensing tower having a manifold pack with an improved carbonated water distrubtion manifold.
It is an object of the present invention to provide a cold plate for an ice cooled beverage dispenser wherein the cold plate has an improved cast-in carbonated water distribution manifold.
SUMMARY OF THE INVENTION
According to the principles of the present invention, an improved cold carbonated beverage dispenser has a carbonator, a plurality of post-mix beverage dispensing heads each of which is connectible to the carbnator, and a carbonated water distribution manifold fluidly between the carbonator and the dispensing heads; the manifold has a tubular inlet fitting, tubular outlet fittings, a carbonated water distribution plenum between the inlet and outlet fittings, a planar inlet wall with the inlet fitting being welded to the inlet wall from inside the plenum, and planar outlet wall with the outlet fittings being welded to the outlet wall from inside the plenum; this manifold assures delivery of carbonated water without decarbonation equally to each and every dispensing head on the dispenser.
An improved carbonated water distribution manifold has a tubular inlet fitting, a plurality of discrete tubular outlet fittings, and a distribution plenum between the inlet and outlet fittings, the plenum has an inlet wall with an aperture into which the inlet fitting extends, an outlet wall with a plurality of outlet apertures into which the outlet fittings extend, and additional plenum walls welded to the inlet and outlet walls, with the inlet and outlet fittings being welded from inside of the plenum chamber, with there being no weld obstructions or crevices to cause decarbonation during flow of carbonated water through the manifold and out any one of the outlet fittings.
A method of making an improved carbonated water distribution manifold has the steps of making an elongate tubular stainless inlet fitting, making a plurality of elongate tubular stainless outlet fittings, making a planar stainless inlet wall, making a planar stainless outlet wall, making additional stainless plenum walls, welding the inlet and outlet fittings to the inlet and outlet walls respectively from a future inside of a carbonated water plenum, and welding the walls together forming the plenum chamber between the inlet and outlet fittings, with all of the fittings being unobstructed by weld and devoid of crevices, so that carbonated water will flow through the manifold and out any outlet fitting without decarbonation or pressure drop, and without sanitation problems.
Many other advantages, features and additional objects of the present invention will become manifest to those versed in the art upon making reference to the detailed description and accompanaying drawings in which the preferred embodiment incorporating the principles of the present invention is set forth and shown by way of illustrative example.
BRIEF DESCRIPTION OF THE DRAWINGS:
FIG. 1 is a perspective view showing schematically the pertinent structure of a an improved beverage dispenser with the present invention therein;
FIG. 2 is a cross-sectional elevational view of the structure of FIG.1;
FIG. 3 is a cross-sectional view taken through lines A--A;
FIG. 4 is an alternative cross-sectional view taken through lines A--A;
FIG. 5a and FIG. 5b show a detailed view explaining fabrication of the improved manifold of the present invention;
FIG. 6 is a cross sectional view of the prior art;
FIG. 7 is a diagramic view of a beverage dispensing tower having a an improved manifold pack with the improved manifold of the present invention;
FIG. 8 is an elevational cross section of a an improved cold plate having the present invention therein; and
FIG. 9 is a plan view of the structure of FIG. 8.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The principles of the present invention are particularly useful when embodied in an improved cold carbonated post-mix beverage dispenser such as is shown schematically in FIGS. 1 & 2 and generally indicated by the numeral 10.
The dispenser 10 has a cooling tank 12 which is filled with ice water to level 14 with the ice water being cooled and having an ice bank of several pounds built therein by an electromechanical refrigeration chassis (not shown) which has an evaporator coil (not shown) normally immersed in the ice water and about which the ice bank reservoir is frozen and held in the water bath.
An important feature of the present invention is the carbonated water distribution manifold shown in FIGS. 1 & 2 and generally indicated by the numeral 20. A water inlet line 22 is connectible to a municipal or other bulk source of palatable sweet water and supplies a water pre-cool coil 24 in the cooling tank 12. The pre-cool coil 24 serves to cool incoming water to close to 32 degrees F. (0 degrees C.) and is connected to supply this cooled water to a carbonator 26. The carbonator is also appropriately connected to a source of carbon dioxide gas (not shown) which effects carbonation of the water in the carbonator 26 to a carbonation level in the range of 4.5 to 5.0 volumes. A carbonated water outlet line 28 extends from the carbonator 26 to an inlet fitting 30 of the carbonated water distribution manifold 20. The inlet fitting 30 leads to a carbonated water distribution plenum 32 which has a plurality of discrete carbonated water outlet fittings 34. Each of the outlet fittings 34 are discretely fluidly connected to the carbonated water inlet of a respective carbonated beverage dispensing head 36. Each dispensing head 36 is for a specific flavor, such as Cola, Diet Cola, Lemon-Lime, Diet Lemon-Lime, Cherry Cola, Orange, and so forth, and a discrete syrup supply line 38 is connected to each dispensing head 36; the syrup supply lines 38 each include a discrete syrup cooling coil 40 which is also immersed in the cooling tank 12.
As shown in FIGS. 1 & 2, the plenum 32 preferably lies on the bottom of the cooling tank 12 along and transversely spanning a front side of the tank. The elongate tubular inlet fitting 30 has a horizontal length 42 extending rearward on the bottom of the tank 12 to an upward extending length 44 leading to an inlet end 46 which is above the water level 14. The elongate tubular outlet fittings 34 each have an upright length 48 which extends upward and out of the water bath to an outlet end 50 which is above the water level 14. Thus the inlet 46 and every outlet 50 is well above the water level 14 enabling easy access, connection, disconnection, sanitation, and minimum probability of contamination.
In FIG. 3, a first preferred cross section and construction of the water manifold 20 is shown. An inlet wall 52 and an outlet wall 54 are formed of a single L-shaped piece. Additional plenum walls 56 are formed and welded to the inlet and outlet walls 52, 54 to form the plenum 32 with an interior carbonated water distribution chamber 58. The ends of the plenum 32 and water chamber 58 are closed by end caps 60. An outlet end 62 of the inlet fitting 30 is inserted into an inlet aperture 64 of the inlet wall 52 and is welded to the inlet wall 52 from inside of the plenum 32.
A convex and smoothly radiused toroidal outlet ring 57 is formed around the outlet end 62 and inside the plenum 32. The outlet ring 57 has a minor diameter with is substantially the same as the inside diameter of the outlet end 62 as shown, and the smooth convex radius of the outlet ring 57 enables smooth carbonated water flow out of the unobstructed inlet fitting 30 and into the water distribution chamber 58. An inlet end 66 of each outlet fitting 34 is inserted into a discrete respective outlet aperture 68 in the outlet wall 54 and each outlet fitting 34 is welded to the outlet wall 54 from inside of the plenum 32.
A convex and smoothly radiused toroidal inlet nose 67 is formed around each inlet end 66 and inside the plenum 32. The inlet nose 67 has a minor diameter which is substantially the same as the inside diameter of the inlet end 66 as shown, and the smooth radiused inlet nose 67 enables smooth carbonated water flow into the unobstructed and bell mouthed inlet end 66 of each outlet fitting 34.
In FIG. 4 the inlet aperture 64 and all outlet apertures 68 are provided with an inwardly formed weld ring 70 that projects inwardly into the plenum 32 and the water distribution chamber 58. The inlet end 66 of each outlet fitting 34 is inserted into and through a respective weld ring 70. The inlet end 66 and weld ring 70 are welded together at their inner ends from inside of the eventual plenum 32 and water distribution chamber 58. A convex smoothly curved and radiused bell-shaped toroidal entry nose 72 is formed by the weldment of the inlet end 66 and weld ring 70 with a minor or smallest diameter of the toroidal inlet nose 72 being substantially the same as the inner diameter of the inlet end 66 as clearly shown. The inlet end 66 and weld ring 70 are welded together at their inner ends from inside of the eventual plenum 32 and water distribution chamber 58. The inlet 66 inner diameter is the diameter of the carbonated water passageway extending through the outlet fitting 34 and there is no obstruction whatsoever to entry of water into each and every outlet fitting 34. The inlet nose 72 provides a relatively gentle and close to laminar inlet flow of carbonated water that does not cause decarbonation or undesirable pressure drop. An outlet ring 73 of FIG. 4 is structurally identical to the inlet nose 72. The material thickness of the weld ring 70 provides the majority of the toroidal inlet nose 72 and outlet ring 73 as clearly shown in FIG. 4.
FIG.5a and FIG. 5b further illustrate the componentry of the manifold 20 and enable further explanation of the improved method of fabricating this carbonated water distribution manifold 20. The manifold 20 is constructed completely of stainless steel and after completion of fabrication is chemically passivated and pressure tested to a nominal proof pressure well in excess of the 125 PSI maximum working pressure. A first stainless steel sheet metal blank 74 is fabricated having the inlet aperture 64 and outlet apertures 68. The flanged in weld rings 70 are also formed and extend to one side of the blank 74. The blank 74 is formed along its length into an L-shape to define the planar inlet wall 52 and planar outlet wall 54. The inlet fitting 30 is inserted into the inlet aperture 64 and welded to the weld ring 70 or inner surface of the inlet flange 52 from the concave side of the L-shaped blank 74F; this concave side being the future inside of the plenum 32. The outlet fittings 34 are then inserted into respective outlet apertures 68 and are likewise welded to the weld rings 70 or inner surface of the outlet flange 54 from the concave side of the L-shaped blank 74F. The welds of the fittings 30, 34 to the walls 52, 54 are now 100% visually inspected. This inspection can be done easily and without instruments. A completely reliable determinatiton is made that the welds are good and that there is no blockage of the inlet or outlet fittings 30, 34, that the welds are complete and that there are nonsanitary crevices or inclusions. The metal used for the blank 74 is about 0.060 inch (1.5 mm) thick and the tubular fittings 30, 34 have a metal wall section in the range of a 0.020-0.025 inch (0.50-0.60 mm) thick. The inlet and outlet walls 52, 54 are thicker and preferably at least twice as thick as the walls of the fittings 30, 34 which assists in producing high quality welds that do not protrude into the fittings 30,34. The outlet from the inlet fitting 30 and the inlets to the outlet fittings 34 are now nicely rounded surfaces which enhance proper fluid flow through the manifold 20. Upon completion of the welded assembly of the fittings 30,34 and inlet and outlet wall blank 74, the plenum 32 is ready to be completed and closed up. A second wall blank 76 has the additional plenum walls 56 and end caps 60 and is formed into the configuration shown as 76F in FIG. 5b. The formed additional wall blank 76F is then placed against and welded to the formed inlet and outlet wall blank 74F to form the completed plenum 32 and manifold 20. The tubular inlets and outlet fittings will typically have 0.250 to 0.312 inch (6-8 mm) inside diameter and the plenum 32 will typically have an internal cross section in the range of 0.5 to 0.75 inches (12.5-19 mm) square or rectangular so that the distribution chamber 58 has a cross section which is always larger than a cross-section of the fittings 30,34. The exterior weld of the plenum wall blanks 74F, 76F is easily repaired if it leaks without effecting the welds of the fittings 30,34 to the inlet and outlet walls 52,54.
This improved method of fabrication and improved manifold 20 enable consistent and high quality distribution of carbonated water in absolutely sanitary conditions.
The prior art is clearly shown in FIG. 6 wherein weld protrusions 78 can be seen obstructing flow of carbonated water. It is these obstructions that cause decarbonation and foaming at one or more of the dispensing heads 36. Also shown are weld voilds 80 that cause sanitation problems. These protrusions 78 and voids 80 are completely unpredictable and cannot be visually ascertained of the fabrication and they have caused significant problems in the past.
FIG. 7 illustrates a further useful alternative embodiment of a dispenser wherein a dispensing tower generally indicated by numeral 100 has a frame 102 which supports a plurality of dispensing heads 36 and a manifold pack 104 for connecting beverage supply lines (not shown) to the heads 36. The manifold pack 104 has a carbonated water distribution manifold 20T embedded within a block of thermal insulation 106. This particular manifold 20T has a pair of inlet fittings, 30T. A remote refrigeration and carbonated water supply device (not shown) has a circulating pump and motor which continualy circulates cold carbonated water through the plenum 32T by pumping one inlet 30T and extracting out of the second inlet 30T or vice versa. The insulation 106 is molded insitu around and to the plenum 32T and at least portions of the inlet and outlet fittings, and the welds of the manifold 20T are no longer accessible for examination or repair.
FIGS. 8 & 9 illustrate an alternative manifold 20CP being utilized at a cast aluminum cold plate generally indicated by the numeral 110, and which when used will have ice cubes loaded on its upper surface 112 for cooling carbonated water and/or syrup in the cold plate liquid circuits to be described.
The manifold 20CP has its plenum 32CP preferably located just under and parallel to the top surface 112 and adjacent to periphery edge 114 of the cold plate 110. The water outlet fittings 34CP extend upward for connection to lines leading to dispensing heads 36 or for connection directly to dispensing heads 36. The plenum is supplied by at least one and possibly two inlet fittings 30CP which is this case are also the water cooling coils in the cold plate 110. The inlet fitting coils 30CP will preferably be wound into involute spirals as seen in FIG. 9 and will be fed warm water at the center and then the outer most coil will be conencted directly to the plenum 32CP to feed cold carbonated water into the plenum. If there are two coils 30CP, they will be one above the other and they will connect into the ends of the plenum 32CP as shown; they may also be counter flow wherein the upper one feeds clockwise and the lower one feeds counter-clockwise or vice versa. If there are two inlet fitting coils 30CP, they will be fluidly connected in parallel to a supply of carbonated water. Syrup cooling coils 116 are embedded underneath and spaced from the water inlet fitting coils 30CP.
The use of the improved manifold 20, 20T, 20CP in dispenser 10, tower 100 or cold plate 110 enables the addition of considerable value to these structures, upon based reliability of the manifold 20, 20T, 20CP with complete confidence that the finished high value product will not be defective or scrap, and that it will work properly and dispense cold carbonated beverage without pressure and flow drop, decarbonation, or foaming. The manufacturing process becomes much more effective because there is negligible scrap and vastly increased quality at a lesser cost.
Although other advantages may be found and realized, and various and minor modifications suggested by those versed n the art, be it understood that I wish to embody within the scope of the patent warranted hereon, all such embodiments as reasonably and properly come within the scope of my contribution to the art. | A carbonated beverage dispenser has an improved carbonated water distribution manifold for evenly and reliably distributing carbonated water from a single carbonator and cooling structure to a plurality of post-mix dispensing valves without decarbonation, flow restriction, foaming or other deficiencies. The improved carbonated water distribution manifold is fabricated of stainless steel and has a tubular inlet fitting, a plurality of tubular outlet fittings, a distribution plenum in between the inlet and outlet fittings with the plenum having a generally planar inlet wall into which the inlet fitting extends, a generally planar outlet wall into which the outlet fittings individually extend, additional plenum walls adjoining the inlet and outlet walls and jointly forming the plenum with there being an interior carbonated water distribution chamber inside the plenum, and in which all of the inlet and outlet fittings are welded to the inlet and outlet walls respectively from inside of the distribution chamber. | 8 |
DISCLOSURE
The United States Government has rights in this invention pursuant to Contract No. DE-AC09-89-SR18035 between the U.S. Department of Energy and Westinghouse Savannah River Company.
CROSS REFERENCE
This application claims the benefit of U.S. Provisional Application No. 60/023,406, filed Aug. 14, 1996, entitled "Tandem Microwave Waste Remediation System".
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to use of microwave energy to treat waste materials. The invention incorporates a dual microwave chamber system. A first chamber is used to treat the waste material housed within a crucible. As the waste is exposed to direct microwave energy and to heat, off-gas emissions from the waste material are transferred to a second chamber where additional microwave energy is used to treat the off gas emissions. It has been found that a significant qualitative and quantitative reduction in off-gas emissions can be achieved.
2. Description of Related Art
It is known in the art to use microwaves to treat waste. U.S. Pat. No. 4,940,865 to Johnson et al. provides an apparatus for the melting of materials using microwaves. U.S. Pat. No. 5,166,488 to Peppard teaches an apparatus using microwaves to melt hypodermic syringes. Johnson vents gaseous and airborne particulates outside the apparatus. Peppard uses a conventional filtering system to retain/treat off-gas emissions. Accordingly, there is room for improvement within the art of microwave processing of wastes.
SUMMARY OF THE INVENTION
It is an object of this invention to provide an apparatus and process which uses microwave radiation to physically transform a waste material.
It is a further object of this invention to provide an apparatus and a process to treat gaseous emissions with a combination of direct microwave radiation and with elevated temperatures such that the treated emissions can be discharged into the atmosphere.
It is a further and more particular object of this invention to provide a dual chamber microwave treatment apparatus and process whereby a first chamber is used to treat a solid or liquid waste material and a second chamber in communication with the first chamber is used to treat off-gases generated during the waste material microwave treatment process.
It is a further and more particular object of this invention to provide an off-gas treatment apparatus and process which uses a conventional microwave oven.
It is still a further and more particular object of this invention to provide an apparatus and process for microwave treatment of solid or liquid waste and gaseous emissions which provides for an inert gas microwaving environment.
It is still a further and more particular object of this invention to provide an apparatus and process for microwave treatment of off-gases and similar emissions in which a gas emission microwave treatment zone can provide an ion exchange medium for the capture and retention of hazardous materials which are impervious to a microwave treatment protocol.
These and other objects of the invention are accomplished by an apparatus and process that provides for a tandem hybrid microwave waste disposal system comprising: a first combustion chamber in communication with a source of microwaves; a second combustion chamber in communication with a source of microwaves, the second combustion chamber having an input region in communication with a first end of a hollow conduit, a second end of the conduit in communication with the first combustion chamber, the second combustion chamber further comprising a susceptor defining a gas-permeable matrix; an exhaust port in communication with an output region of the second combustion chamber, wherein evolved combustion off-gases from the first combustion chamber pass through the conduit into an input region of the second combustion chamber whereby the susceptor matrix is maintained at an effective temperature for further treating the off-gases, the treated off-gases exiting through the exhaust port. Such an apparatus enables a process of treating waste comprising: providing a supply of waste material within a combustion chamber; passing a fluid stream through said combustion chamber; exposing the waste material to a combination of microwave energy and radiant energy, the radiant energy supplied by a susceptor in proximity to the waste material; directing off-gases from the first combustion chamber to a second combustion chamber; radiating the off-gases in the combustion chamber with microwave energy; retaining the off-gases within the second combustion chamber until an effective amount of the off-gases are destroyed, thereby providing treated off-gases; and, venting the treated off-gases.
The invention is an improvement over prior utilizations of microwave energy because the treatment and sterilization of a heterogeneous broad range of materials is possible without extensive pretreatment. Treatment is provided for solid and liquid waste mixtures including plastics, radioactive materials, florescent tubes, rubber materials, oils, solvents, resins, volatile organic compounds and carbon filter media, etc. The microwave units are compact and portable. The second chamber provides treatment, detoxification and sterilization of off-gases emitted from the first chamber. The treated waste is a decontaminated and sterilized material, with an off-gas treated stream which requires little or no additional remediation.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings,
FIG. 1 depicts a schematic of a tandem microwave waste processing apparatus in accordance with this invention; and
FIG. 2 depicts an alternative configuration of the microwave waste processing apparatus of this invention.
DETAILED DESCRIPTION
The tandem microwave waste treatment system provides for the physical and chemical alteration of waste using a two-stage treatment protocol, whereby each stage of waste treatment is carried out in a separate microwave chamber. Relevant background information can be found in the following publications which are incorporated herein by reference: Wicks, G. G., Clark, D. E., Schulz, R. L. and Roboski, R. A., "Hybrid Microwave Technology for Treatment of Hazardous Wastes, Including Electronic Circuitry with Reclamaration of Precious Metals", presented at the 1997 Global Demilitarization Symposium & Exhibition, Reno, Nev., May 5-8, 1997; Wicks, G. G., Clark, D. E., and R. L. Schulz "Microwave Technology for Waste Management Applications: Treatment of Discarded Electronic Circuitry", Microwaves Theory and Applications in Materials Processing IV, D. E. Clark, W. H. Sutton and D. A. Lewis, eds., Vol. 80, pp. 627-637 (1997); Schulz, R. L., Folz, D. C., Clark, D. E., Schmidt, C. J. and Wicks, G. G., "Microwave Waste Treatment System", presented at the First World Congress on Microwave Processing, Lake Buena Vista, Fla., Jan. 5-9, 1997; Schulz, R. L., Folz, D. C., Clark, D. E., Schmidt, C. J. and Wicks, G. G., "Microwave Treatment of Emissions from Waste Materials", Microwave Processing of Materials V, M. F. Iskander, J. O. Kiggans, Jr., C. Bolomey, eds., Materials Research Society Symposium Proceedings, Vol. 430, pp. 549-554 (1996); Wicks, G. G., Clark, D. E., Schulz, R. L. and Folz, D. C., "Microwave Technology for Waste Management Applications Including Disposition of Electronic Circuitry", Microwaves: Theory & Application in Materials Processing III, Ceramic Transactions, D. E. Clark, D. C. Folz, S. J. Oda and R. Silberglitt, eds., Vol. 59, pp. 79-89 (1995); Schulz, R. L. Folz, D. C., Clark, D. E., Wicks, G. G., and Hutcheon, R. M., "Applications of Microwave Energy for Waste Remediation", in Proceedings of the 28th Microwave Power Symposium of the International Microwave Power Institute Symposium, Montreal, Quebec, pp. 9-18 (1993); Schulz, R. L., Folz, D. C., Clark, D. E., and Wicks, G. G., "Microwave Destruction/Vitrification of Electronic Components", Ceramic Transactions, Microwaves: Theory and Application in Materials Processing II, D. E. Clark, W. R. Tinga and J. R. Laia, eds., Vol. 36, pp. 81-88 (1993); Schulz, R. L., Folz, D. C., Clark, D. E., Hutcheon, R. M. and Wicks, G. G., "Microwave Processing of Simulated Nuclear Waste Glass II", Ceramic Transactions, Microwaves: Theory and Application in Materials Processing II, D. E. Clark, W. R. Tinga and J. R. Laia, eds., Vol. 36, pp. 89-97 (1993); Schulz, R. L., Fathi, Z., Clark, D. E., and Wicks G. G., "Microwave Processing of Simulated Nuclear Waste Glass", presented at the Symposium on Microwaves: Theory and Application in Materials Processing, Apr. 28-May 2, 1991, Cinn. Ohio, Ceramic Transactions, Nuclear Waste Management IV, G. G. Wicks, D. F. Bickford and L. R. Bunnell, eds., Vol 23, pp. 779-786 (1991), also published in, Microwave Processing of Materials, D. E. Clark, F. D. Gac, W. H. Sutton, eds., Ceramic Transactions, Vol. 21, pp. 451-458 (1991).
As seen in reference to FIG. 1, a tandem microwave waste treatment apparatus 1 is illustrated. A first primary chamber 2 is defined by the interior of a 900 watt, 2.45 GHz microwave unit 3 which has been lined along interior surfaces with a refractory lining 5. An air inlet 7 has been provided along a bottom surface of the microwave unit 3. Inlet 7 is in communication through feed line 9 with a supply of compressed gas. Preferably, the compressed gas is an inert gas such as argon or nitrogen and can be introduced to the primary chamber at a controlled rate. The use of inert gases is useful to control the combustion rate and to avoid explosive operating conditions. However, it has been demonstrated that for some materials, a simple air stream will suffice.
In a preferred embodiment, a walled, covered box-like enclosure 11 of susceptor material such as SiC is placed over crucible 13 within chamber 2 of the combustion chamber, crucible 13 containing the waste material which is to be processed. An upper surface of the susceptor enclosure 11 defines an opening 15 in communication with an interconnect tube 17.
As seen in FIG. 1, interconnect tube 17 is in communication with an interior of a second microwave unit 19, positioned a spaced distance above unit 3. Similar to unit 3, a refractory lining 5 surrounds an interior 21 of microwave unit 19. A terminal end of tube 17 is interconnected to a combustion chamber 23. Filters 18 may be provided to control particulate emmissions. Combustion chamber 23 is provided by a mullite or alundum (Saint Gobain/Norton Industrial Ceramics Corp.) tube 24 partially filled within its interior with a SiC bed of 16 grit size material 25 . Alternatively, chamber 23 can be filled with a plurality of stacked reticulated SiC filters as well as other appropriate susceptor materials and mixtures thereof. Chamber 23 and material 25 provide operating temperatures of between 1000-1200 degrees C. Reticulated phosphate bonded alumina (pba) filters 27 are placed at either end of chamber 23 to maintain the stability of the bed and to increase the gas emission residence time within the chamber.
An exhaust port 29 exits microwave unit 19. Port 29 is in communication at a first end with a terminal end 31 of chamber 23. Sampling ports 33 are provided on both exhaust port 29 and exhaust tube 17 to facilitate collection of gas stream samples for analyses. Thermocouples 35 are provided on both the combustion chamber 23 as well as crucible 13 to provide displayed operating temperature conditions.
In operation, the material to be treated is placed within crucible 13 of microwave unit 3. Microwave unit 19 is operated to bring the Si--C susceptor material 25 within chamber 23 to an operating temperature of between 1000-1200 degrees C. Once the operating temperature conditions are obtained, the microwave unit 3 is used to treat the material inside crucible 13 with a combination of direct microwave energy as well as indirect infrared energy which radiates from the susceptor. The microwave energy input of both units 19 and 3 can be easily controlled to achieve a desired combustion rate of the solid material as well as an effective operating temperature for the treatment of off-gases within chamber 23.
The process can be further controlled by the use of inert gases to provide a regulated fluid flow through the system. The sampling ports 33 provide the operator the ability to sample the off-gas streams following both the material waste treatment and the off-gas treatment. The present data was collected by using Tenax-TA filled glass air traps (Analytical, College Station, Tex.) which are highly absorbent for C6-C20 compounds. Following collection, the air traps were submitted for gas chromatography and mass spectrometer (GC-MS) analysis of the retained off-gases. It is envisioned that sampling ports 33 can be equipped with in-line monitors to provide real time data collection with respect to the off-gas constituents. As seen in FIG. 2, a valve 41 can be used to control the venting of treated off-gases. Should on-line monitors detect unacceptable levels of materials in the off-gas stream, the off-gas pathway can be diverted for retreatment (directional arrows) to the off-gas combustion chamber.
EXAMPLE 1
Set forth in tables 1 and 2 are the conditions and results of seven 30 minute test runs (SR-1 through SR-7) using crushed and pulverized printed electrical circuit boards as the waste material. The data was collected using a side-by-side microwave unit configuration as disclosed in the related provisional application referenced above and as discussed in Schulz, R. L., Folz, D. C., Clark, D. E., Schmidt, C. J. and Wicks, G. G., "Microwave Treatment of Emissions from Waste Materials", Microwave Processing of Materials V, M. F. Iskander, J. O. Kiggans, Jr., C. Bolomey, eds., Materials Research Society Symposium Proceedings, Vol. 430, pp.549-554 (1996).
The gaseous organic compounds that vaporize during treatment of the material in the primary chamber, were sampled at the gas sampling port 33 at the exit of the primary chamber. These values are provided in column A in Table 2. The gases were sampled following treatment in the off-gas combustion chamber and the values reported in column B of Table 2. The results demonstrate reduction of certain organic chemical off-gas concentrations to non-detectable (ND) concentrations, and reductions of other organic chemical off-gas concentrations to more than 1 order of magnitude.
TABLE 1______________________________________ Processing/ Off-gas Duty Sample Initial Final % Collection Cycle* ID Weight (g) Weight Wt Loss Time (min) (%)______________________________________SR1 69.96 41.15 41.2 30 50 SR2 70.09 40.66 41.9 30 50 SR3 69.99 45.75 34.6 30 50 SR4 70.05 41.16 41.2 30 100 SR5 70.01 42.27 39.6 30 50 SR6 70.00 40.85 41.6 30 50 SR7 70.03 44.49 36.4 30 50______________________________________ *Percent of time interval magnetron was activated
TABLE 2__________________________________________________________________________A Summary of the GC mass Spectroscopy Results of Emissions Resulting fromCombustion of Printed Circuit Boards. (A = before microwave off-gas treatment; B = after microwave off-gastreatment) SR-1 (ppb) SR-2 (ppb) SR-3 (ppb) SR-4 (ppb) SR-5 (ppb) SR-6 (ppb) SR-7 (ppb)Compound A B A B A B A B A B A B A B__________________________________________________________________________Benzene* 16.9 1.1 14.2 nd 19.8 nd 115.3 5.2 119.6 8.1 176.6 14.7 165.4 13.5 Toluene 28.7 2.7 24.4 nd 32.6 nd 67.5 6.1 78.7 6.9 159.1 18.1 115.7 5.9 Ethylbenzene* 18.7 nd** 19.0 nd 7.8 nd 13.9 nd 26.7 nd 142.9 5.0 91.8 nd Styrene* 38.7 1.2 66.6 nd 15.0 nd 165.2 2.9 167.7 2.6 472.3 27.2 482.9 6.5 Napthalane* 1.2 nd 11.0 nd nd nd 75.1 1.3 35.2 1.3 6.8 3.4 47.6 2.4 m/p Xylene* 17.5 nd 1.9 nd nd nd 27.5 nd 23.8 nd 53.3 1.6 60.0 nd 1,3,5 9.5 nd 12.4 nd 1.3 nd 15.6 1.6 18.4 nd 12.8 2.4 46.2 1.7 Trimethyl- benzene 1,2,4 17.5 nd 1.7 nd nd nd nd nd nd nd 15.1 nd 6.1 1.8 Trimethyl- benzene__________________________________________________________________________ *Listed in the Clean Air Act (as amended, 1990) as hazardous air pollutants [14]. **nd = not detected (<1 ppb)
EXAMPLE 2
Set forth in Table 3 is data from two additional runs using crushed and pulverized circuit boards and following the general protocol set forth above in an upper/lower tandem microwave system as seen in FIG. 1. As set forth in Table 3, the results of the emissions analysis is set forth in nanograms. Again, significant reductions and/or elimination of certain emission waste has been obtained.
TABLE 3______________________________________Gas Chromatography Data Collected Before and After Microwave Treatment of Emissions Resulting From the Combustion of Unreinforced Circuit Boards SR-8 EMISSIONS (ng) SR-9 EMISSIONS (ng)COMPOUND A B A B______________________________________Benzene* 5838.9 22.2 1415.6 139.5 Toluene* 8146.6 15.7 4215.9 158.7 Ethylbenzene* 1147.4 nd 4557.0 5.2 Styrene* 1666.9 6.2 20012.0 38.4 Naphthalene* 355.5 nd 2403.6 27.9 m/p Xylene* 2259.0 nd 510.6 nd 1,3,5 1564.0 nd 378.7 64.3 Trimethylbenzene 1,2,4 904.7 nd 171.8 nd Trimethylbenzene______________________________________ A = before microwave offgas treatment; B = after microwave offgas treatment *Listed in the Clean Air Act (as amended, 1990) as hazardous air pollutants.
The reductions in off-gas constituents is significant and has applications for a variety of off-gas emission sources, regardless of origin. Further, the data is from a combustion treatment chamber having a simple cylindrical shape and a length of approximately 8 inches. By varying the geometry and length of the treatment chamber, is should be possible to increase the volume of introduced off-gases along with enhanced efficiency of the treatment process.
An important feature of the present invention is the use of the hybrid microwave system. As used herein, hybrid refers to the combination of a direct microwave energy bombardment of the waste material along with the radiant infrared heating which occurs through the use of the susceptor materials. For specialty waste applications, it is possible to tune or vary the frequency of the microwave source so as to selectively target a waste constituent. Such targeting is possible in both the primary waste treatment step as well as the treatment of off-gas emissions.
It is known in the art that microwaves can be transmitted substantial distances from a remote magnetron 51 (FIG. 2) via wave guides 53 . As a result, the magnetron can be shielded from reflected microwaves which permits innovative designs for combustion chambers to be constructed. Such abilities are significant in that the present process can be commercially scaled up in ways compatible with conventional off-gas emission source designs.
As set forth in Table 1, there is a significant reduction in the weight of the treated material. Further, as best described in co-pending patent application having Ser. No. 08/605/293 entitled "Methods for Recovering Metals from Waste", and incorporated herein by reference, microwave heating of the electronic, metal-containing waste enables precious metals to be separated and collected from the remaining solid waste material after volatilization. As such, significant amounts of precious and nonprecious metals can be removed from the waste stream and recycled.
The treated residue is more friable than the untreated waste and can be compacted and compressed for waste volume reductions of over 50% of the starting material. Further, the high temperatures of the initial combustion chamber can destroy any bacterial or viral pathogens which may be present on or within the waste. As an additional benefit, the extreme heat transforms material such as medical waste into a decontaminated, sterile product which has been rendered into an unrecognizable, nonhazardous inert waste product. As a result, disposal of the residue of nonradioactive medical waste a the normal sanitary waste stream is possible.
Where significant ceramic and glass materials are present in the waste, the high temperatures will produce a molten glass product without the need for additional additives. Where needed, additional glass formers can be added to the waste to create a vitrified waste product. The vitrified product has been found to immobilize difficult to destroy constituents in a leach-resistant, glass-like matrix while permitting the simultaneous separation and reclamation of precious metals such as gold and silver.
All solid and liquid material microwave treatment processes generate off-gases. The present invention provides for an apparatus and process to further treat off-gases with microwaves to substantially reduce and/or eliminate harmful constituents in the off-gas emissions. However, the off-gas treatment capabilities are not limited to tandem microwave processes. Numerous off-gas emission sources, independent of a microwave waste treatment origin, are capable of being treated with the microwave off-gas process of the present invention. For instance, traditional incinerator off-gases could serve as an off-gas source which is passed through a microwave off-gas unit to destroy additional volatile organic compounds (VOCs). Emission sources as diverse as dry cleaners, university and research fume hood operations, industrial emissions, off-gas from remediation treatments, etc. could be further treated with a microwave off-gas system.
The microwave off-gas treatment system can be customized for particular waste streams. For instance, waste which is contaminated with radioactive materials, including mixed waste, is often vitrified into a solid waste material. The off-gasses from the vitrification process will also contain traces of the radioactive material. By incorporating a ion exchange material specific for the radioactive isotope(s) into the Si--C matrix material or elsewhere in the combustion chamber, the isotopes can be retained within the treatment chamber. As a result, less costly emission systems can be used where mixed waste combustion and/or vitrification is involved.
Finally, it should be noted that the described embodiments and data provided were obtained using modified versions of conventional household microwave units. Such units are useful for small volume waste generators which may treat waste on site as opposed to transporting waste for off-site treatment. Such units are easily transported and can be readily assembled and disassembled.
For commercial waste handling facilities and/or recycling operations, it would be desirable to scale-up the size and output of the equipment so that commercial quantities of waste may be processed. Such modifications are well within the capabilities of one skilled in the art.
Many variations will undoubtedly become apparent to one skilled in the art upon a reading of the above specification with reference to the drawings. Such variations, however, are within the spirit and scope of the invention as defined by the following appended claims. | The invention discloses a tandem microwave system consisting of a primary chamber in which microwave energy is used for the controlled combustion of materials. A second chamber is used to further treat the off-gases from the primary chamber by passage through a susceptor matrix subjected to additional microwave energy. The direct microwave radiation and elevated temperatures provide for significant reductions in the qualitative and quantitative emissions of the treated off gases. The tandem microwave system can be utilized for disinfecting wastes, sterilizing materials, and/or modifying the form of wastes to solidify organic or inorganic materials. The simple design allows on-site treatment of waste by small volume waste generators. | 5 |
TECHNICAL FIELD The present invention relates to a method for making a structure with cellular cores for use in a structural panel for a turbojet nacelle.
[0001] The invention also relates to a panel and a nacelle including such a structure with cellular cores.
BACKGROUND
[0002] Airplane turbojet engines are surrounded by a nacelle to protect them and ensure the operation thereof. The nacelle is made up of walls composed of non-structural panels and structural panels. The latter parts ensure a sufficient stiffness of the nacelle. To that end, structural panels usually have one or more layers of cellular core structures (commonly called “honeycomb” structures). These layers are generally covered with a skin on their so-called outer face, i.e. the face radially furthest from the axis of the engine, and on their inner face, i.e. the face radially closest to the axis of the engine.
[0003] The structural panel is then assembled by arranging the different skins and layers, which are then pasted on a mold with the required shape. The assembly is cured in a furnace so as to grip the layers and polymerize the adhesives.
[0004] In parallel, turbojet engines generate substantial noise pollution. There is therefore a strong demand aiming to reduce this pollution, and even more so given that the turbojet engines used are becoming increasingly powerful.
[0005] To that end, some of the panels used are acoustic structural panels whereof the layers are generally covered on the outer face with an air-impermeable skin, called “solid,” and on the inner face with an air-permeable perforated skin, called “acoustic.”
[0006] The structural acoustic panel can also comprise several layers of cellular core structures between which a multi-perforated skin, called a “septum,” is located. This skin is adhered between the cellular core structures by heating during the assembly/gluing phase of the panel.
[0007] Such panels constitute acoustic resonators able to “trap” the noise and therefore attenuate the sound emissions towards the outside of the nacelle.
[0008] In a known manner, a cellular core structure comprises at least one cellular core block comprising a central part having core honeycomb cells and two lateral parts each having a plurality of honeycomb joining cells.
[0009] The acoustic properties of the acoustic structural panel, i.e. its noise absorption rate as a function of the frequency and sound level of the noise, depend in particular on the joining of the cellular core block(s).
[0010] The join of the cellular joining cells is commonly done using a foaming adhesive, such as the FM410® adhesive, which has a significant expansion capacity. The adjacent edges of the cellular core block(s) are coated with the adhesive, which, when it expands, blocks the honeycomb cells by creating overthicknesses.
[0011] The use of adhesive requires too long a placement and cutout time of the overthicknesses from an industrial perspective.
[0012] Furthermore, these overthicknesses have the drawback of decreasing the effective acoustic surface of the cellular core structure as well as causing abrupt impedance interruptions, which contributes to decreasing the acoustic performance of the acoustic panel during the operation of the turbojet engine.
[0013] Also known from application WO2008/113904 is a structure with cellular cores whereof the honeycomb edge cells situated on the edges of several blocks with cellular cores making up said structure have been sectioned, then fitted together to join said blocks.
[0014] However, such a structure with cellular cores requires maintenance by stressing the cellular core structure, which makes production more complex.
[0015] Moreover, this embodiment does not make it possible to obtain optimal bending strength.
BRIEF SUMMARY
[0016] One aim of the present invention is therefore to provide a cellular core structure that is easy to manufacture and has good bending strength.
[0017] Another aim of the present invention is to provide a cellular core structure able to effectively absorb the noise from the turbojet engine in an acoustic panel.
[0018] To that end, according to a first aspect, the invention relates to a method for manufacturing a structure with cellular cores that can be used in the structural panel of a turbojet nacelle, including at least one block of cellular cores having a central portion with core honeycomb cells and at least two side portions each including side honeycomb cells, wherein said method includes the following steps:
[0019] A) forming junction walls on the side honeycomb cells, the junction walls being capable of interacting for forming a junction area;
[0020] B) unfolding the junction walls thus formed; and
[0021] C) joining the walls thus unfolded and belonging to two different side portions end-to-end so that said junction walls are fitted together so as to form a junction area.
[0022] The joining of one or more cellular core blocks by fitting junction walls together makes it possible to avoid stressing the structure obtained using the inventive method. Indeed, the junction is made by simply interweaving said walls without the latter necessarily being in contact.
[0023] The bending strength is improved. In fact, the majority of the junction walls not being in contact with each other, they can each deform freely without impacting the other walls. Moreover, the stresses pass through the outer skins from one outer skin to the other, which makes it possible to prevent the concentration of forces in the axis of the joint.
[0024] Furthermore, the cellular core structure obtained using the inventive method has the advantage of not obstructing the honeycomb cells at the joints of the cellular core blocks. As a result, the cellular core structure very effectively absorbs the noise from the operation of the turbojet engine.
[0025] According to other features of the invention, the inventive method comprises one or more of the following optional features, considered alone or according to all possible combinations:
the length (e) of each junction wall is greater than or equal to the largest length of the side and/or core honeycomb cells, which makes it possible to improve the bending strength; the side parts belonging to cellular core blocks whereof the side and core honeycomb cells have different sizes are joined end-to-end, which makes it possible to adapt the mechanical strength of the structure as needed; in step A, one opens the edge honeycomb cells situated on the edges of a side part of a block intended to be joined and honeycomb cells adjacent to the edge honeycomb cells so as to form the junction walls, which allows a simple and effective formation of the junction walls; the edge and adjacent honeycomb cells are opened by section to a lateral side and/or a wall of a honeycomb cell; the inventive method comprises an additional step D in which the fitting done in step C is maintained by fastening members, in particular by clamps or staples, which makes it possibly to durably maintain the cellular core structure without stress.
[0031] According to a second aspect, the invention relates to a structural panel for a nacelle surrounding a turbojet engine, characterized in that it is equipped with at least one cellular core structure obtained using the inventive method.
[0032] Preferably, the panel according to the invention is an acoustic panel whereof the cellular core structure(s) are coated on one of their faces with an outer skin impermeable to air and on their other face with a perforated inner skin, which makes it possible to benefit from the advantages of said structure in an acoustic structural panel.
[0033] According to one preferred alternative, the inventive panel includes at least two cellular core structures superimposed one on the other, which makes it possible to strengthen the mechanical rigidity of the panel according to the invention.
[0034] According to another aspect, the invention relates to an aircraft engine nacelle, characterized in that it comprises at least one panel according to the invention.
[0035] Preferably, the structural panel(s) are situated in the air intake zone of said nacelle.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] The invention will be better understood upon reading the following non-limiting description, done in reference to the appended figures.
[0037] FIG. 1 is a cross-sectional view of a single-layer structural panel according to the present invention;
[0038] FIG. 2 is a cross-sectional view of a dual-layer structural panel according to the present invention;
[0039] FIG. 3 is a diagrammatic view of the inventive method;
[0040] FIG. 4 is a top view of a structure obtained at the end of the inventive method;
[0041] FIG. 5 is a front view of a honeycomb cell used in the present invention;
[0042] FIG. 6 is an alternative of the embodiment of FIG. 3 .
DETAILED DESCRIPTION
[0043] As shown in FIG. 1 , the structural panel 1 according to the invention can be a single-layer acoustic panel comprising a cellular core structure 2 according to the invention formed by one or more, and in this case two cellular core blocks A and B joined together. In the event a single cellular core block is used, it is joined on itself to form a cellular core structure, for example by forming a substantially cylindrical structure that can be used in a nacelle air intake.
[0044] The cellular core block(s) A and B used can have any geometric shape, such as square, or any other suitable shape.
[0045] In the event the inventive structure includes a plurality of cellular core blocks A, B defining a plurality of junction zones, it is then possible to choose each block to obtain the desired mechanical strength and, if applicable, the desired acoustic absorption.
[0046] The cellular core structure 2 is sandwiched between an inner skin 3 and an outer skin 4 , which allow the transition of mechanical stresses. Furthermore, the presence of these skins 3 and 4 makes it possible to keep the cellular core structure 2 in a single element.
[0047] These two cellular core blocks A, B include a central portion 5 comprising core honeycomb cells 7 a , 7 b and typically several, in this case two side portions 9 a , 9 b each comprising a plurality of side honeycomb cells 11 a , 11 b . A block can for example include at least four side portions. The side honeycomb cells 11 a , 11 b of each block A and B are adjacent to the junction zone 13 , the features of which will be detailed below.
[0048] As shown in FIGS. 3 and 4 , the core honeycomb cells 7 a , 7 b and the side honeycomb cells 11 a , 11 b in this case have hexagonal sections, thereby forming so-called honeycomb structures. It is possible for said honeycomb cells 7 a , 7 b and 11 a , 11 b to have sections with any geometric shape other than hexagonal. As shown in FIG. 1 , the section of the core 7 a and side 11 a honeycomb cells of the block A can for example be smaller than that of the core 7 b and side 11 b honeycomb cells of the block B, so as to meet the acoustic and/or mechanical stresses imposed by the manufacturer's specifications.
[0049] Preferably, the side 11 a , 11 b and core 7 a , 7 b honeycomb cells are made of metal, an alloy, or a composite material so as to facilitate the production of the core 7 a , 7 b and side 11 a , 11 b honeycomb cells and to impart good mechanical strength to the latter. The material forming the inner skin 3 can be made in a metal material, such as aluminum or titanium, or fabric, and the material forming the outer skin 4 can be a multi-layer composite material or a metal material such as aluminum or titanium.
[0050] The structural panel 1 as shown in FIG. 1 is an acoustic panel. In this case, the inner skin 3 includes perforations 15 located facing the core 7 a , 7 b and side 11 a , 11 b honeycomb cells. In this way, the structural panel 1 can absorb the sound annoyance created by the operation of the turbojet engine.
[0051] In an alternative shown in FIG. 2 , the structural panel 101 is a dual-layer panel according to the invention comprising two layers of cellular core blocks, respectively formed by blocks A, B and A′, B′. Said layers are assembled together by known means and sandwiched between an inner skin 103 and an outer skin 104 similar to those of FIG. 1 . The other elements forming the structural panel 101 are identical to those of the structural panel 1 shown in FIG. 1 , the corresponding references being the same.
[0052] According to one alternative, it is possible to obtain a structural panel including a number of layers of cellular core blocks greater than 2, in particular greater than or equal to 3.
[0053] In this dual-layer panel, the cellular core blocks A, B on the one hand, and A′, B′ on the other are joined together in one or more joint zones 113 .
[0054] The operating principle of an acoustic panel like those 1 and 101 shown in FIGS. 1 and 2 is known in itself; the panel 1 , 101 is intended to be mounted in the inner wall of an aircraft nacelle, preferably in the air intake zone of said nacelle, so that the inner skin 3 , 103 is located opposite the engine located in said nacelle.
[0055] The noise emitted by this engine penetrates the honeycomb cells A, B via orifices 15 situated in the inner skin 3 , 103 , and vibrates inside these core 7 a , 7 b and side 11 a , 11 b honeycomb cells that make up the acoustic resonators. In this way, a dissipation of the acoustic energy and subsequent reduction of the noise level are possible. In order to improve the acoustic absorption, it is possible to apply a perforated skin, also called septum, between the two layers of blocks with a cellular core A, B and A′, B′ of the structural panel 101 so that the core 7 a ′, 7 b ′ and side 11 a ′, 11 b ′ honeycomb cells of the blocks A′ and B′ also make up acoustic resonators.
[0056] According to the embodiment shown in FIGS. 3 and 4 , the cellular core structure 202 used in the structural panel according to the invention is obtained using the inventive method, which includes a step A, symbolized by the arrow 30 , a step B, symbolized by the arrow 31 , and a step C (not shown).
[0057] In step A, junction walls 36 are formed on the side honeycomb cells 11 a and 11 b , the junction walls 36 being able to cooperate to form a joint zone.
[0058] To that end, according to the embodiment shown in FIG. 3 , the edge honeycomb cells 33 a , 33 b are opened situated on the edges of a side part 9 a , 9 b of one or more blocks A, B intended to be joined and the adjacent honeycomb cells 34 a , 34 b to the edge honeycomb cells 33 a , 33 b so as to form the junction walls 36 . In this way, advantageously, junction walls 36 are formed on the side honeycomb cells 11 a and 11 b , the junction walls 36 being able to cooperate to form a joint zone.
[0059] In this embodiment, the edge 33 a and 33 b and adjacent 34 a and 34 b honeycomb cells are opened by section on a lateral side and/or a wall of a honeycomb cells using any means known by those skilled in the art. Thus, for example, it is possible to make a cutout using a cutting tool such as a pair of scissors.
[0060] According to another embodiment not shown, it is possible to use one or more cellular core blocks whereof the junction walls are formed during the production of said block(s). According to another embodiment, the junction walls can be attached using any means known by those skilled in the art on a cellular core block already formed.
[0061] In step B, the junction walls 36 thus formed are unfolded using any means known by those skilled in the art, in particular by using a clip. The deployment of the junction walls 36 thereby makes it possible to obtain a larger length of the joint zone.
[0062] As shown in FIG. 4 , in step C, the walls thus unfolded 46 belonging to two different side parts 9 a and 9 b are joined end-to-end so that said junction walls 46 fit together to form a joint zone 213 .
[0063] Advantageously, the cellular core structure obtained using the method according to the present invention has the advantage of not obstructing the honeycomb cells at the junction of the cellular core blocks. As a result, the inventive structure effectively absorbs the noise coming from the operation of the turbojet operation.
[0064] According to one alternative, the junction walls 46 are unfolded so as to arrange them substantially parallel to each other so that the junction walls 46 thus unfolded fit together like a comb.
[0065] The structure according to the invention 201 can be formed by a single block joined on itself or by joining a plurality of cellular blocks, in particular two blocks A, B or three cellular blocks.
[0066] The unfolded junction walls 46 can advantageously have a length e greater than or equal to the largest length l of a larger side or core honeycomb cell.
[0067] The largest length l is defined as the greatest distance between two edges of the honeycomb cell that are not immediately adjacent. In the case of regular honeycomb cells, this largest length l corresponds to the diameter of the circle inscribed or marked out of the largest honeycomb cell.
[0068] The fitting together in step C can be done in the “ribbon” direction 51 , corresponding to the orientation of the cellular core block A, B before expansion (see FIG. 5 ). The direction of “expansion” 53 corresponds to a direction perpendicular to the ribbon direction 51 (see FIG. 5 ). In one alternative, it is also possible to join one block in the “ribbon” direction and another block in the “expansion” direction.
[0069] The “expansion” direction designates the direction in which the core 7 a , 7 a ′, 7 b , 7 b ′ and side 11 a , 11 a ′, 11 b , 11 b ′ honeycomb cells are opened so as to form open cells able to trap sound and thereby form the honeycomb structure.
[0070] Thus in the case shown in FIG. 3 , the fitting together is done in the ribbon direction.
[0071] It is also possible for the opening of the honeycomb cells 11 a , 11 b to allow fitting together in the expansion direction, as shown in FIG. 6 .
[0072] According to one embodiment, in step C, at least two cellular core blocks whereof the side and core honeycomb cells are different sizes are joined end-to-end. According to one alternative, a same cellular core block can have side and core honeycomb cells of different sizes.
[0073] Thus, in the event at least two cellular core blocks of different sizes are joined, the largest length l is taken relative to the largest side and core honeycomb cells present in block A and/or block B.
[0074] In the event two blocks are joined including side and core honeycomb cells of substantially the same size, the largest length l can be taken relative to any side or core honeycomb cells.
[0075] According to one embodiment, the inventive method can comprise an additional step D in which the fitting together done in step C is maintained using fastening members.
[0076] The fastening members are for example clamps or staples, which makes it possible to ensure good maintenance.
[0077] The junction can be maintained by compacting in a bladder before curing prior to applying a usual glue between the cellular core blocks thus joined to fasten the outer skin.
[0078] The structure 2 , 102 , 202 obtained using the inventive method has one or more joint zones 13 , 113 and 213 , which are not stressed. Thus, the implementation of the method is simplified compared to the embodiments described in the prior art.
[0079] Furthermore, the majority of the junction walls 46 are not in contact, which makes it possible to ensure good bending strength. In fact, the junction walls 46 can each deform independently of the other junction walls. The interweaving of the cellular core blocks allows the passage of forces from one outer skin to the other so as to avoid a concentration of these forces in the axis of the junction. | The invention relates to a method for manufacturing a structure with cellular cores ( 202 ) that can be used in the structural panel of a turbojet nacelle, including at least one block of cellular cores (A, B) having a central portion ( 5 a, 5 b ) with core honeycomb cells ( 7 a, 7 b ) and at least two side portions ( 9 a, 9 a′, 9 b, 9 b ′) each including side honeycomb cells ( 11 a, 11 b ), wherein said method includes the following steps: A) forming junction walls on the side honeycomb cells ( 11 a, 11 b ), the junction walls being capable of interacting for forming a junction area ( 213 ); B) unfolding the junction walls thus formed; and C) joining the walls thus unfolded ( 46 ) and belonging to two different side portions ( 9 a, 9 b) end-to-end so that said junction walls ( 46 ) are fitted together so as to form a junction area ( 213 ). The invention also relates to a structural panel and to a nacelle including a structure with cellular cores obtained by said method. | 8 |
BACKGROUND OF THE INVENTION
The present invention relates to improved compositions and methods for enzymatic determination of components in biological fluids.
The invention is initially discussed in the context of a creatine phosphokinase assay.
Creatine phosphokinase (CPK) is found primarily in muscle, brain, and heart tissue. Determination of CPK, particularly in blood serum, is one of the most sensitive enzyme assays available for the detection of skeletal muscle disease and is also useful in the diagnosis of myocardial infarction and cerebrovascular incidents.
A basic method for assaying for CPK is the method of C. Oliver, J. Biochem, Volume 61, page 116 (1955). The method has been modified by several workers for use as a diagnostic reagent, see for example, S. B. Rosalki, J. Clin. Lab. Med., Vol. 69, p. 696 (1967). The assay is based on the following principals:
CPK catalyzes the transfer of the phosphate group from creatine phosphate to adenosine diphosphate (ADP) in the presence of magnesium ions and preferably also sulfhydryl groups as activators:
Creatine phosphate+ADP CPK Creatine+ATP
where ATP is adenosine phosphate. ATP is used to produce glucose --6-- phosphate from glucose. This reaction is catalyzed by hexokinase (HK):
ATP+glucose HK glucose-6-phosphate+ADP
Glucose-6-phosphate is then oxidized by a nicotinamide adenine dinucleotide coenzyme, namely nicotinamide adenine dinucleotide phosphate (NADP) or nicotinamide adenine dinucleotide (NAD) in the presence of glucose-6-phosphate dehydrogenase (G-6-PDH):
Glucose-6-phosphate+NAD(P) G-6-PDH 6-phosphogluconate+NAD(P)H
After an initial lag phase, the three reactions proceed stoichiometrically and quantitatively. The NAD(P)H, i.e. reduced NAD or reduced NADP, is determined spectrophotometrically at 340 nm. Alternatively, color coupling reagents may be added to enable spectrophotometric reading in the visible range, e.g. 500 nm.
In the above reaction, the enzymes HK and G-6-PDH may be referred to as indicator enzymes since they are used to convert reaction products into products which are spectrophotometrically measurable. The indicator enzymes in their purified form are used in a portion of about 30 micrograms per 40 milligrams of dry reagent, which is used to make one ml. of liquid reagent. Thus, two problems are presented. The first is that this extremely low percentage, i.e. 0.075% by weight of the dry mixture, is extremely difficult to mix. Therefore, a medium commonly referred to in the art as a bulking agent is needed in which the indicator enzymes may be mixed. Then the indicator enzymes may be uniformly dispersed within a dry mixture so that a conveniently measurable amount of the dry mixture may be used to provide a small amount of the indicator enzymes. This mixing in a medium of greater volume is commonly referred to as bulking. The second problem is that the bulking agent must be suitable for use in both a dry phase of the reagent for storage stability and in the aqueous reagent phase after it is mixed in an aqueous solution for use in assaying.
It is known in the art that it is desirable to provide a kit of several reagents to perform an assay and that providing reagents containing such components as enzymes, coenzymes and/or substrates a material in dry, solid form will be more stable and have a longer shelf-life than a liquid reagent. For example, such advantages are discussed in U.S. Pat. No. 3,540,984 to Alfred Deutsch, issued Nov. 17, 1970. A desired form of preparation of a dry powder enzyme reagent having a long shelf life comprises mixing reagent components in an aqueous solution and lyophilizing them to provide a stable, dry, enzyme-containing material. The enzyme-containing material is in turn mixed with other dry reagent components and with a further dry bulking agent in order to form an economical, conveniently manufactured form of a multicomponent reagent containing compounds which would not be stable over long periods of time in an aqueous phase.
A bulking agent must have the properties normally desirable, i.e. it must be millable, friable and mix well with reagent components. It is also highly desirable that the bulking agent have a salutory effect with respect to enzyme stability. Also, enzyme reactions are subject to interference from many different sources; enzyme activity may be inhibited by anyone of a number of substances. One material that has been used for bulking hexokinase and G-6-PDH is ammonium sulfate. In aqueous solution, this bulking agent ionizes into ammonium ions and sulfate ions. These ions have elevated ionic strength. It has been observed that the activity of CPK is inhibited by various ions such as ammonium and sulfate and by elevated ionic strength in solutions. The problem is therefore presented of stabilizing the CPK reagent in which indicator enzymes are stabilized in dry and in aqueous form without the use of bulking agents which form ions of elevated ionic strength, which may inhibit enzyme activity. In accordance with the present invention, improved bulking is provided for hexokinase and G-6-PDH as well as improved CPK and glucose determinations.
The determination of serum glucose is probably the most frequently performed test in the clinical laboratory, and often utilizes hexokinase and G-6-PDH. Many factors, both physiological and pathological, affect the circulating glucose level. Pathological states which tend to produce hyperglycemia include diabetes mellitus, uremia, hyperthyroidism, and hyperadrenalism. Hypoglycemia is found most commonly with excessive use of insulin and other antidiabetic drugs as well as in certain diseases of the pituitary and adrenals.
One significant commercial glucose determination is a modification of the method of Barthelmai and Czok, Klin. Wschr., Volume 40, page 585 (1962). Glucose is determined by the highly specific hexokinase and glucose-6-phosphate dehydrogenase enzyme system coupled in the final step to the reduction of nicotinamide adenine dinucleotide (NAD), the formation of reduced NAD (NADH) being monitored at 340 nm.
In this method, hexokinase (HK) with a magnesium activator catalyzes the phosphorylation of glucose in the sample by adenosine triphosphate (ATP): ##EQU1## where ADP is adenosine diphosphate.
Glucose-6-phosphate is then oxidized by a nicotinamide adenine dinucleotide coenzyme in the presence of glucose-6-phosphate dehydrogenase (G-6-PDH):
glucose-6-phosphate+NAD(P) G-6-PDH 6-phosphogluconate+NAD(P)H
Both reactions proceed stoichiometrically and quantitatively. The NADH produced is determined spectrophotometrically at 340 nm.
Again, it is necessary to bulk and stabilize hexokinase and G-6-PDH. It is also desirable to provide a reagent system or kit in a dry, solid form.
In the quantities of reactive compounds for the above method for 1 ml. of reagent weight about 15 mg. For example, the following components may be used:
0.03 mg. hexokinase
0.03 mg. glucose-6-PDH
0.4 mg. adenosine-triphosphate, sodium salt
0.6 mg. NAD
1.8 mg. magnesium maleate
12 mg. buffer material
These weights of materials cannot be dispensed by commercial equipment with sufficient accuracy. A preferred weight of such a mixture should exceed 70 mg. or preferably 100 mg. Therefore, a dry powder bulking agent to bulk dry reagent components as well as enzyme-containing components is desirable. One such prior bulking agent is mannitol. It is also desirable to provide such a bulking agent which has further useful properties compared to mannitol, such as providing buffering and further contributing to stability. A new such bulking agent, triethanolammonium terephthatale (TEA-TPA), is provided in accordance with the invention.
Another important function in a reagent system is activation or stabilization of enzymes other than the above-defined indicator enzymes. In the present context, activation refers to reversing of oxidation or other adverse effect, while stabilization refers to the prevention thereof. It is important that the enzyme CPK maintain its enzyme activity since its action on the substrate creatine phosphate is necessary for the measurement of CPK in the biological fluid being tested. However, it is known that CPK loses some activity in some sera as a result of reversible inactivation due to the oxidation of essential sulfhydryl groups. This inactivation of CPK may be reversed in part or totally by adding to a reagent composition, and hence reacting with CPK, sulfhydryl-containing compounds such as glutathione, mercaptoacetic acid, or dithiothereitol (DTT). This may be accomplished by adding the compound to the serum or by incorporating it in the enzyme assay mixture. The most commonly used sulfhydryl compounds for this application are glutathione (GSH) and DTT.
However, it has been noticed that in the embodiment in which iodonitrotetrazolium violet (INT) coupling is provided for spectrophotometric measurement in the visible range, sulfhydryl compounds slowly reduce the INT to form its colored formazan. This increases the amount of background color, or may be said to increase the blank reaction. The range of the useful curve of optical absorbance versus concentration of CPK which is useful is thereby reduced. It should be noted that GSH and DTT in particular are quite expensive. GSH has also been criticized somewhat in the literature. For example, see G. Anido, S. B. Rosalki, E. J. van Kampen and M. Ruben, Quality Control in Clinical Chemistry, pp. 180-183, (Walter de Gruyter, Berlin, 1975). It is stated that definitive recommendations on the appropriate thiol cannot be made.
It is therefore desirable to find an activator for CPK which is also compatible with the other components in the reagent system. It is also preferable if that reagent is of lower cost. Another consideration is that the activator be useful in a dry, solid reagent system having a long shelf-life. The material selected must be useful in the initial reagent preparation, the dry phase, and again in the aqueous state when the reconstituted reagent is used in the laboratory. It is also desirable to provide an improved stabilizer for enzymes used for the determination of glucose and serum urea nitrogen. Such an activator stabilizer is provided in accordance with the present invention.
The determination of serum urea nitrogen, also often referred to as BUN, is widely used for evaluation of the kidney function. One standard method is that of H. Talke and G. E. Schubert, Klin.-Wschr. Vol. 43,p. 174 (1965). This enzymatic method does not require the use of corrosive reagents or high reaction temperatures.
This determination is based on the following principles:
Urea is hydrolyzed by urease:
(NH.sub.2).sbsb.2CO+H.sub.2 O .sup.urease 2NH.sub.3 +CO.sub.2
Ammonia is produced which aminates α-ketoglutarate in the presence of glutamate dehydrogenase (GLDH) with concurrent oxidation of NADH:
NH.sub.3 +α-ketoglutarate+NADH→glutamate+H.sub.2 O+NAD
Both reactions proceed stoichiometrically and quantitatively. The disappearance of NADH is measured at 340 nm spectrophotometrically.
The novel activator and stabilizer of the present invention interacts in the CPK and glucose determinations described above and also interacts with the improved bulking agents referred to above to provide further improved CPK and glucose determinations. An improved serum urea nitrogen determination and improved stabilization of enzymes therein are also provided.
All of the elements described above cooperate to form an interactive reagent system. This concept is illustrated and defined by the example of the novel glucose reagent system. A novel bulking agent is provided for bulking indicator enzymes. This bulking agent improves stability in the dry phase. A further novel bulking agent is also provided for bulking other dry reagent components and also contributes to stability in the dry phase. The two bulking agents both contribute to stability while neither adversely affects the other. A novel enzymes stabilizer is also included in the dry reagent system. This stabilizer acts in the aqueous phase to improve reagent stability. The stabilizer does not adversely affect stability in the dry phase, and the bulking agents do not adversely affect stability in the aqueous phase. Also, the further bulking agent acts as a buffer in the aqueous phase. The bulking agents do not interfere with stability or with the chemical reactions in the aqueous phase. Compatability of reagent system components contributes to the desirable result of providing a reagent system which may be stored by a user on a shelf for prolonged periods of time before use and which is also stable for long periods of time in use. (The terms "prolonged" and "long" are used in their well-known sense in the context of clinical chemistry laboratory use.)
Stability is a significant aspect in the commercial use of reagents. A reagent with a long shelf life may remain in distribution channels such as in a manufacturer's and distributor's inventory before shipment to a laboratory, and the laboratory may order a sufficiently large inventory so that frequent reordering is not necessary. Increasingly critical cost factors are thus somewhat alleviated. In vitro diagnostic reagents must be discarded after expiration dates based on their stability, and it is important to provide a reagent which a laboratory will not need to return or discard before use.
SUMMARY OF THE INVENTION
It is therefor a general object of the present invention to provide improved reagent systems for CPK, glucose and urea nitrogen assays in which components thereof interact to improve reagent stability in the dry, storage stable phase and in the aqueous phase for performance of chemical determinations.
It is an object of the present invention to provide an improved bulking agent for the enzymes hexokinase or G-6-PDH.
It is a specific object of the present invention to provide a bulking agent for stabilizing hexokinase and G-6-PDH and which is of low ionic strength in aqueous solution.
It is a further object of the present invention to provide a bulking agent of the type described which also acts as a stabilizer.
It is another object of the present invention to provide a further bulking agent for bulking dry reagent system components, which components may include bulked enzymes.
It is a further object of the present invention to provide an improved CPK determination incorporating an improved bulking agent for indicator enzymes.
It is another object of the present invention to provide an improved glucose determination incorporating an improved bulking agent for indicator enzymes.
Additionally, it is another object of the present invention to provide a novel composition useful as an enzyme activator or stabilizer.
It is a more specific object of the present invention to provide a compound useful as an activator in CPK and as a stabilizer in glucose or urea nitrogen determinations.
It is also an object of the present invention to provide a novel CPK reagent system and determination incorporating an improved activator.
It is another object of the present invention to provide a novel glucose reagent system and determination incorporating an improved stabilizer.
It is still another object of the present invention to provide a novel urea nitrogen determination incorporating an improved stabilizer.
It is a further object of the present invention to provide a novel CPK reagent system and determination incorporating a novel bulking agent and novel activator which cooperate to provide improved reagent stability in both the dry and aqueous phases.
It is also an additional object of the present invention to provide a novel glucose reagent system and determination incorporating improved bulking agents and a stabilizer which cooperate in the reagent system for improved stability of reagent in both the dry and aqueous phases.
It is another object of the present invention to provide a novel serum reagent system and determination incorporating a novel bulking agent and a stabilizer which cooperate in the reagent system for improved stability of reagent in both the dry and aqueous phases.
Briefly stated, in accordance with the present invention, a bulking agent for the indicator enzymes hexokinase and G-6-PDH is provided. The bulking agent comprises bovine serum albumin and glycine and taurine. A novel compound is prepared consisting of the tris (hydroxymethyl) aminomethane salt of 2-mercaptosuccinic acid which is useful as an activator in CPK determinations and as a stabilizer in glucose and serum urea nitrogen determinations. A further bulking agent for dry reagents is provided, comprising triethanolammonium terephthalate (TEA-TPA). Stable reagent systems for the respective determination of CPK and glucose of the type in which hexokinase and glucose-6-phosphate dehydrogenase are indicator enzymes are provided. Further, the novel bulking agents and activator-stabilizer cooperate in reagent systems to provide improved reagent stability in both the dry phase in storage and the aqueous phase in use. An improved stable reagent system is also provided for urea nitrogen determinations.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The invention is initially discussed in the context of a CPK assay. All temperatures recited below are centigrade.
Materials
A CPK reagent system requires creatine phosphate substrate, ADP, magnesium activator, NAD, glucose, sulfhydryl activator compound such as glutathione or a different composition such as that provided in the present invention, hexokinase such as from a yeast source, and G-6-PDH from a leuconostoc source. Alternatively, NADP may be used in place of NAD, and the G-6-PDH utilized may be from a leuconostoc or yeast source. Additionally, buffer materials, AMP, filler, binder and stabilizers, particularly for the hexokinase and G-6-PDH, are required. In the preferred form, the stabilizer is also the filler.
EXAMPLE I
In the preferred form, it is desired to provide a dry powder CPK reagent system which is reconstituted for laboratory assay use. The following materials are dried in vacuo to constant weight. Each dry material is milled or ground to fine powder. The resulting dry powders are mixed such as by agitation in a ball mill, V-blender, or other mixer until samples withdrawn from the mix are found to be homogeneous. Operations and handling of materials should be performed under conditions in which atmospheric moisture will not be absorbed in or adsorbed to the materials so as to make the resulting reagent have a shorter life. The following components are utilized to make sufficient reagent to be reconstituted with 100 liters of water.
For 100 liters of CPK Reagent:
______________________________________Preferredamount______________________________________300,000 IU 100,000-600,000 IU at 37 degrees bulked, stabilized hexokinase300,000 IU 100,000-600,000 IU at 37 degrees bulked, stabilized glucose-6-phosphate dehydrogenase76 g 38-152 g. d-Glucose200 g 67-400 g nicotinamide-adenine dinucleotide free acid280 g 100-350 g magnesium maleate125 g 90-300 g adenosine diphosphate, trilithium salt1060 g 875-2430 g Disodium creatine phosphate dried to 1 mole or less of water of crystallization285 g 150-275 g adenosine monophsophoric disodium salt158 g 100-200 g tris (hydroxymethyl)aminomethane salt of 2-mercaptosuccinic acid (TMS)______________________________________ **tris (hydroxymethyl)aminoethane free base **Ntris-(hydroxymethyl) methyl2 amino ethanesulfonic acid **These are the buffering components added to produce the desired final p 6.9 (6.7- 7.2) *The 100 liters refers to the volume of water to be added to the dry reagent form to make the liquid form used for performing the test.
The components above are homogeneously mixed. The total weight is observed or calculated from the sum of the component weights. The total weight in grams divided by 100,000 is grams of dry reagent to be dissolved in 1 ml of water to form the aqueous reagent for laboratory use. In the preferred form, the powder mixture is packaged in butyl rubber stopper serum vials with powder sufficient for addition of 25 ml of water. The powder may be dispensed by utilizing known equipment, an example of which is the powder dispenser known by the trademark ACCO-FIL manufactured by Perry Industries.
It is noted that this reagent composition does not comprise a sulfhydryl compound such as glutathione (GSH) for activation of CPK. The reagent includes the tris (hydroxymethyl) aminomethane salt of 2-mercaptosuccinic acid. This salt is abbreviated herein as TMS.
TMS is a new substance prepared as described below in Example III. It has been discovered that TMS prevents or reverses the oxidation of CPK. Further, it aids in stabilizing the hexokinase and G-6-PDH components of the reagent system. TMS is also useful in an assay system because it is not a substrate for GSH dehydrogenase. GSH dehydrogenase is present in human cells and may be present in serum samples being assayed. The use of TMS in an activator system prevents the possibility of the activator reacting with the serum as may occur when GSH is used as the activator. Additionally, applicant has obtained glutathione at a cost of $353 per mole and DTT at $942 per mole (one mole of DTT being equivalent to two moles of GSH), while obtaining mercaptosuccinic acid at $21 per mole. There is approximately 0.01 mole of either substance used for 1 liter of reconstituted reagent.
CPK Determination
In the preferred utilization of the above reagent system, dry reagent powder is dissolved in deionized water.
The components above are homogeneously mixed. The total weight is observed or calculated from the sum of the component weights. The total weight in grams divided by 100,000 is grams of dry reagent to be dissolved in 1 ml of water to form the aqueous reagent for laboratory use. In the preferred form, the powder mixture is packaged in butyl rubber stopper serum vials with powder sufficient for addition of 25 ml of water. The powder may be dispensed by utilizing known equipment, an example of which is the powder dispenser known by the trademark ACCO-FIL manufactured by Perry Industries.
It is noted that this reagent composition does not comprise a sulfhydryl compound such as glutathione (GSH) for activation of CPK. The reagent includes the tris (hydroxymethyl) aminomethane salt of 2-mercaptosuccinic acid. This salt is abbreviated herein as TMS.
TMS is a new substance prepared as described below in Example III. It has been discovered that TMS prevents or reverses the oxidation of CPK. Further, it aids in stabilizing the hexokinase and G-6-PDH components of the reagent system. TMS is also useful in an assay system because it is not a substrate for GSH dehydrogenase. GSH dehydrogenase is present in human cells and may be present in serum samples being assayed. The use of TMS in an activator system prevents the possibility of the activator reacting with the serum as may occur when GSH is used as the activator. Additionally, applicant has obtained glutathione at a cost of $353 per mole and DTT at $942 per mole (one mole of DTT being equivalent to two moles of GSH), while obtaining mercaptosuccinic acid at $21 per mole. There is approximately 0.01 mole of either substance used for 1 liter of reconstituted reagent.
CPK Determination
In the preferred utilization of the above reagent system, dry reagent powder is dissolved in deionized water. The powder should not be exposed to air for prolonged periods of time before dissolution. A spectrophotometer is provided, set to 340 nm and allowed to stabilize. The spectrophotometer is "zeroed," i.e. set against an appropriate blank such as air or water.
The reagent is incubated in a cuvette at 37° C. for 10 minutes. A sample is added thereto, and mixed thoroughly with the reagent. The cuvette is incubated, preferably in a thermostated spectrophotometer compartment. Two minutes after addition of the sample, a first optical absorbance reading A1 of the reaction mixture is read. Five minutes thereafter, a second absorbance reading A2 is taken.
To calculate CPK activity in units per liter, U/L, Δ A is calculated.
ΔA=A1-A2
U/L=ΔA×F
when a 1 cm lightpath through the cuvette is provided: ##EQU2## where t is the time interval between the taking of readings A1 and A2,
TV is the total reaction volume in ml,
SV is the sample volume in ml, and
e is the molar extinction coefficient of NADH at 340 nm (6.22×10 6 )
where t=5 min, TV=2.15 ml, and SV=0.05 ml, then F=1382.
EXAMPLE II
A reagent system was prepared in accordance with Example I, but included further components for color coupling. A preferred color coupling component is iodonitrotetrazolium violet (INT), which is reduced by NAD to form its colored formazan whose optical absorbance is measured in the range of 505 nm. It is well known to perform this reaction in the presence of an electron asceptor such as diaphorase or phenazine methyl sulfate (PMS). Diaphorase may be stabilized in accordance with Example VI. From 50,000 to 300,000 international units, preferably 100,000 IU, may be added to the formulation of Example I.
Assays were performed utilizing the mixture. It is found that TMS provides the antioxidant properties, as does GSH or other sulfhydryl compounds. However, it is also noted that TMS does not react significantly with INT, while reaction of GSH with INT reduces INT to form a colored product. This reaction of GSH increases the blank reaction and thereby reduces the useful range of the CPK assay. The use of TMS thus permits for maintaining a full useful range of optical absorbance of reaction products versus concentration units of CPK therein.
In use of the reagent, the well-known factor accounting for the reduction of INT is utilized rather than the molar extinction coefficient of NADH at 340 nm.
EXAMPLE III
It has been found that the presence of TMS in a reagent prepared in accordance with Example I is at least as effective in activating CPK as GSH is in a similar reagent. In the absence of TMS, CPK activity was lost upon a sample's standing and was not initially recovered from the sample. TMS also prevents oxidation of enzymes in the above-described glucose and urea nitrogen determinations. It is for this reason TMS is referred to herein as an activator and stabilizer.
The preparation of TMS may be accomplished by the following method. To ten liters of water, 1.5 kg of mercaptosuccinic acid is added. Solid tris (hydroxymethyl)aminomethane (TRIS) is added with stirring until the resulting solution is at a pH of 6.8-7. This solution is frozen in a dry ice bath and lyophylized. The lyophylization results in a glassy material. This material is washed with acetone. The resulting mass is placed in ten liters of methanol, warmed and agitated. A white solid forms. When the white solid forms, ten liters of acetone are added. The product is collected by filtration, washed and dried to provide TMS. Alternatively for producing a CPK reagent in accordance with Example I, to the solution to be lyophilized may be added the requisite amount of AMP disodium salt. The lyophilization is carried out. In this case, the lyophilizate does not require the acetone treatment.
EXAMPLE IV
TMS is also useful in a glucose reagent. For 100 liters of reagent, the following components may be used.
______________________________________PreferredAmount______________________________________60 g 40-240 g NAD180 g 100-350 g Magnesium maleate40 g 20-120 g adenosine triphosphate disodium salt, preferably250 g 100-400 g TMS200,000 IU 100,000-600,000 IU at 37 degrees bulked stabilized hexokinase250,000 IU 100,000-600,000 IU at 37 degrees bulked stabilized G-6-PDH1000 g 500-2000 g Triethanol amine salt of terephthalic acid (TEA-TPA) (prepared in accordance with Example V) tris (hydroxymethyl)aminoethane sufficient to create a pH of 7.2-7.8 in reagent when dis- solved in water.______________________________________
It is useful to provide a magnesium salt as a source of magnesium ions. However, many magnesium salts are quite hygrosopic. Absorbance of water may adversely affect stability. Magnesium maleate is selected above since it is not hygroscopic. Other non-hydroscopic salts to provide activator ions may be used.
Glucose Determination
In the preferred utilization of the above reagent system, dry reagent powder is dissolved in deionized water. The powder should not be exposed to air for prolonged periods of time before dissolution. A spectrophotometer is provided, set to 340 nm, and allowed to stabilize. The spectrophotometer is "zeroed," i.e. set against an appropriate blank such as air or water.
The reagent is placed in a cuvette and a first absorbance reading A0 is taken. Sample is mixed in each cuvette and the resulting reaction mixture is incubated at room temperature for between 5 and 30 minutes. A second absorbance reading A is taken. A0 is subtracted from A to yield Δ A sample. A standard is similarly tested to obtain a value of Δ A standard. ##EQU3## where C is the glucose concentration in the standard. It should be noted that grossly icteric, hemolyzed or lipemic specimens may require a blank correction so that a term is provided for subtraction from A sample to compensate for optical absorbance not due to the presence of glucose.
EXAMPLE V
TEA-TPA is a novel bulking agent preferably used for bulking dry reagents, particularly for glucose and urea nitrogen reagents.
To prepare TEA-TPA, for example, 20 liters of water may be used to which are added 9.25 kg triethenolamine and 4.5 kg terephthalic acid. The solution is heated to 60 degrees centigrade and then allowed to cool to less than 40 degrees centigrade. Thereafter, 80 liters of acetone are added slowly. The solution is cooled. A fine white precipitate which forms is collected by filtration and washed and dried to provide TEA-TPA.
EXAMPLE VI
A similar preparation was also prepared to measure urea nitrogen in a determination in which urea is hydrolyzed by urease, ammonia is produced to aminate α-ketoglutarate in the presence of glutamate dehydrogenase with the concurrent oxidation of NADH which may be monitored spectrophotometrically. Again, the TMS was found to stabilize indicator enzymes.
A dry urea nitrogen reagent system which may be reconstituted to 100 liters of reagent is prepared from:
______________________________________PreferredAmount______________________________________128 g 60-360 g α-ketoglutarate (alpha)27.5 g 20-55 g NADH (yeast source)200 g 0-400 g ADP, trilithium salt800,000 IU 400,000-1,200,000 IU urease1,200,000 IU 600,000-2,400,000 IU glutamate dehydrogenase (beef liver source)1000 g 200-12,000 g TEA-TPA200 g 100-400 g TMS tris (hydroxymethyl)aminomethane sufficient to produce a pH of 7.6 ± 0.3______________________________________
Urea Nitrogen Determination
In the preferred utilization of the above reagent system, dry reagent powder is dissolved in deionized water. The powder should not be exposed to air for prolonged periods of time before dissolution. A spectrophotometer is provided, set to 340 nm, and allowed to stabilize. The spectrophotometer is "zeroed," i.e. set against an appropriate blank such as air or water.
The reagent is placed in a cuvette and a first absorbance reading A0 is taken. Sample is mixed in each cuvette and the resulting reaction mixture is incubated at room temperature for 15 minutes. A second absorbance reading A is taken. A is subtracted from A0 to yield Δ A sample. A standard is similarly tested to obtain a value of Δ A standard. ##EQU4## where C is the urea nitrogen concentration in the standard. It should be noted that grossly icteric, hemolyzed or lipemic specimens may require a blank correction so that a term is provided for addition to Δ A sample to compensate for the change in absorbance, or optical density, not due to the presence of urea nitrogen.
EXAMPLE VII
Preparation of bulked, stabilized hexokinase, glucose-6-phosphate dehydrogenase and/or diaphorase.
Each enzyme, HK, G-6-PDH or diaphorase, may be bulked together or separately, depending on the convenience of the manufacturing procedure. A stabilized solution is prepared and lyophilized to provide an enzyme-containing material. The material may be ground to provide a powder for combination with other reagent materials. To this solution is added 750,000 IU hexokinase, such as from a yeast source, and 750,000 IU G-6-PDH (leuconostoc).
Preparation of Stabilizer Solution for HK and G-6-PDH.
2-3 L 30% bovine serum albumin solution
60-120 g glycine
24-96 g taurine
Sufficient water to produce 12 liters of solution to which either dilute hydrochloric acid or tris (hydroxymethyl)aminomethane is added to give a pH of 6.8±0.1.
A preferred set of actual values is 2.4 liters bovine albumin solution, 96 grams glycine, 48 grams taurine and 9.6 liters of water.
EXAMPLE VIII
A reagent may be prepared in accordance with Example I utilizing bulked stabilized hexokinase and G-6-PDH in accordance with Example VII and including a sulfhydryl compound other than TMS. For example, GSH or DTT may be utilized.
EXAMPLE IX
A reagent is prepared in accordance with Examples II or VIII and a tetrazolium salt such as INT is used in the reagent for color coupling. The INT is reduced by the NADPH or NADH to form its colored formazan for spectrophotometric reading at 505 nm. For INT color coupling, it is necessary to use an electron acceptor such as phenazine methylsulfate, PMS, or preferably diaphorase in a strength of 50,000 to 300,000 IU in the bulk stabilized form. A strength of 100,000 IU is preferred in the above mixture. To prepare bulked, stabilized diaphorase, 50,000 to 300,000 units of diaphorase are added to the previously described stabilizer solution of Example VII. The diaphorase may be prepared together with the other two enzymes or separately.
EXAMPLE X
The stabilized indicator enzymes of Example VII are utilized in the reagent of Example I.
EXAMPLE XI
The stabilized indicator enzymes of Example VII are utilized in the reagent of Example II.
EXAMPLE XII
A glucose reagent is produced according to Example IV utilizing an activator other than TMS, e.g. GSH, and bulked stabilized indicator enzymes in accordance with Example VII.
EXAMPLE XIII
A glucose reagent is produced in accordance with Example IV utilizing bulked, stabilized indicator enzymes in accordance with Example VII.
EXAMPLE XIV
A glucose reagent is produced in accordance with Examples IV or XII utilizing mannitol as a bulking agent for dry reagent components in place of TEA-TPA.
EXAMPLE XV
A urea nitrogen reagent is produced in accordance with Example VI utilizing mannitol as a bulking agent for dry reagent components in place of TEA-TPA.
EXAMPLE XVI
A urea nitrogen reagent is produced in accordance with Example VI utilizing a sulfhydryl compound other than TMS, such as GSH or DTT.
It is seen that in the reagent systems and determinations above, stability in both the dry, storage stable state and in the aqueous state for use is provided. In addition, individual components of those which cooperate are unique. The specification will enable those skilled in the art to practice many specific forms of the invention in accordance with the above teachings. | An improved reagent system for chemical determinations and novel compositions therefor provide improved reagent stability, particularly in a dry, storage stable phase. For determinations in which hexokinase and glucose-6-phosphate dehydrogenase are indicator enzymes, glycine and taurine are combined with bovine serum albumin to provide a bulking agent for the indicator enzymes which also acts as a stabilizer. A novel salt, the tris (hydroxymethyl)aminomethane salt of 2 mercaptosuccinic acid, acts as an activator or stabilizer in chemistries utilizing the indicator enzymes, namely determinations of creatine phosphokinase or glucose. The novel salt also acts as a stabilizer in a urea nitrogen determination. Dry reagent components are bulked in triethanolammonium terephthalate. Novel CPK, glucose and serum urea nitrogen determinations are also provided. | 2 |
This application is a continuation of application Ser. No. 715,480, filed 3/25/85, abandoned.
BACKGROUND OF THE INVENTION
This invention relates to improvements in a wrapped bush, and more particularly, to a wrapped bush of which joint is extended slantwise or stepwise relative to a generatrix of the outer periphery of the wrapped bush.
A conventional wrapped bush is formed by rolling up a rectangular plate into a cylindrical configuration such that its joint corresponds with a generatrix of the outer peripheral surface. This kind of wrapped bush involves the following disadvantages. First, a large power is required for rolling up a rectangular plate into a cylindrical configuration, which results in the degree of adhesion being poor and it being difficult to maintain the out of roundness. Secondly, working becomes more difficult as the ratio of the wall thickness of the wrapped bush to the diameter thereof increases. Thirdly, working becomes more difficult as the width of the bush increases in relation to the diameter thereof. Fourthly, there is the possibility of portions on both sides of a joint of the wrapped bush shifting along the joint in the opposite directions to each other during services. Fifthly, there is the possibility of a lubrication film breaking to reduce the load bearing ability.
SUMMARY OF THE INVENTION
It is an object of the invention to eliminate the above-described disadvantages of the prior wrapped bush by forming an oil groove or a relief area particularly along a joint on the wrapped bush.
It is another object of the invention to provide a wrapped bush, of which joint is extended slantwise or stepwise relative to a generatrix of the cylindrical outer peripheral surface of the wrapped bush to facilitate working and to enable positively and closely putting the edges of the wrapped bush together, and which can eliminate breakage of an oil film produced due to discontinuity of the joint and is free from distortion in the radial and axial directions to ensure out of roundness.
It is a further object of the invention to provide a wrapped bush which comprises a joint extended slantwise or stepwise relative to a generatrix of its cylindrical outer peripheral surface and an oil groove or a relief area extended along the joint or the ridgeline of the joint, said oil groove or relief area being inclined relative to a generatrix of the cylindrical outer peripheral surface to enable avoiding any oil breakage due to discontinuity of the oil groove or relief area, and which is easy working to enable positively putting the edges of the wrapped bush together and is free from distortion in the radial and axial directions to ensure out of roundness.
The above and other objects, features and advantages of the present invention will become clear from the following description of the preferred embodiments thereof, taken in conjunction with the accompanying drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1A is a perspective view of a wrapped bush according to a first embodiment of the invention;
FIG. 1B is a plan view of a parallelogramatic plate serving as a material for the wrapped bush shown in FIG. 1A;
FIG. 1C is a plan view of a modified form of the first embodiment;
FIG. 2A is a perspective view of a wrapped bush according to a second embodiment of the invention;
FIG. 2B is a plan view of a parallelogramatic plate serving as a material for the wrapped bush shown in FIG. 2A; and
FIGS. 2C to 2H show in plan modified forms of the second embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIGS. 1A and 1B, there is shown a wrapped bush 1 according to a first embodiment of the invention. A parallelogramatic plate 5 has such a configuration as to have an angle of θ formed between a joint 2 of the wrapped bush 1 and a generatrix 2a on the outer peripheral surface 3, and may be a single material or a composite material. In the case of a single material, a casting or a sintered body made of a material such as a known bearing alloy, or a rolled body thereof is used. In the case of a composite material, a bimetal or trimetal is used which is formed by coating a base metal (rigid body) of a known steel, a cast iron or the like with non-ferrous bearing metals. When such composite material is used, the plate 5 is rolled up so that the bearing metal presents itself on the inner peripheral surface 4 or outer peripheral surface 5 depending upon the usage. In the first embodiment, the parallelogramatic plate 5 having an angle of θ=50° is rolled up to form the wrapped bush 1 with a diagonally disposed (straight type) butt-joint 2. As compared with the rolling up of a rectangular plate in the prior art, rolling up of a parallelogramatic plate in this way requires less power and enables positively and closely putting the edges of the bush together to be free from distortion in the radial and axial directions, thereby ensuring out roundness. Therefore, a predetermined clearance between the resulting wrapped bush 1 and an associated rotating shaft can be ensured and a good lubricating effect is attained without any breakage of a lubrication film.
Referring to FIGS. 2A and 2B, there is shown a wrapped bush 1' according to the second embodiment of the invention. This wrapped bush 1' is different from the first embodiment, that is, the wrapped bush 1, only in that an oil groove or relief area 6 is formed along the joint on the inner peripheral surface 4'. As this wrapped bush 1' has the oil groove or relief area 6 extending along the joint 2', the influence of the joint 2' on the lubrication film as well as the influence of breakage of an oil film can be reduced to improve the lubrication effect. The oil groove or relief area 6 shown in FIG. 2A has a U-shaped cross section, but the cross section of the oil groove or relief area may be arcuate, V-shaped, trapezoidal or square. The joint may be in the form of butt joint, clinch joint (single or combined) or weld joint.
The above described angle θ of the parallelogramatic plates 5, 5', which serve as the materials for the wrapped bushes in the first and second embodiments, is 50 degrees, but experiments have proved that the angle may be more than 0°, but less than 85°. If the angle θ were 85 degrees or more, the slantwise joint resulted from roll forming would be incomplete.
FIG. 1C is a plan view of a flat plate which is used for a modified form of the first embodiment shown in FIGS. 1A and 1B.
FIGS. 2C to 2H are plan views of flat plates which are used for modified forms of the second embodiment shown in FIGS. 2A and 2B. It has been confirmed that the modified forms shown in FIGS. 2C to 2H are substantially equivalent to the second embodiment of FIGS. 2A and 2B in effects.
In the above modified forms shown in FIGS. 1C and 2C to 2H, the angle θ is 20°, 30° and 40°, respectively, but may be within the range of 0° to 85°. Here, it is to be noted that the modified forms of FIGS. 2C and 2D in which any oil groove or relief area is not provided are included in the present invention.
As described above, according to the invention, there is provided a wrapped bush which is easy in working to enable positively and closely putting the edges of a joint together, and is free from distortion in the radial and axial directions to ensure out of roundness, and which can eliminate breakage of an oil film produced due to discontinuity of the joint.
Modifications, changes, and improvements to the preferred forms of the invention herein disclosed, described and illustrated may occur to those skilled in the art who come to understand the principles thereof. Accordingly, the scope of the invention should not be limited to the particular embodiments set forth herein, but rather should be limited by the appended claims. | A cylindrical wrapped bush has a joint extending over the entire width of the wrapped bush and serves to slidably or rotatably support a shaft on the inner peripheral surface of the wrapped bush. The joint is extended slantwise or stepwise relative to a generatrix on the outer peripheral surface of the wrapped bush at an angle which is more than 0 degree, but smaller than 85 degrees. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus for polishing objects such as semiconductor wafers, hard disks, glass substrates, liquid crystal display panels, and so on.
2. Description of the Related Art
A conventional chemical mechanical polishing (CMP) apparatus used in fabrication of, for example, semiconductor integrated circuit devices, is based on holding the semiconductor wafer in a rotating top ring and pressing the wafer against a polishing cloth mounted on a rotating turntable while supplying a polishing solution, including abrading particles to the polishing cloth. Hence, polishing is carried out mechanically by the abrading particles floating freely in the polishing solution, and chemically by a chemical solution at the pressing and sliding interface between the polishing cloth and the semiconductor wafer. However, such a CMP apparatus presents a problem in that, depending on the type of surface patterns and differences in the height of fine structures formed on the surface of the wafer, it was not possible to obtain a precisely polished flat and mirror surface on the wafer.
Therefore, in place of the CMP process, another polishing technology has been developed, based on a grinding member to produce a relative pressing and sliding motion against the wafer, in which abrading particles are bound in the grinding member and generated freely from the grinding member while water or a chemical solution is supplied at the sliding interface between the grinding member and the wafer. The polishing apparatus of the grinding member type includes variations using such as a ring-type grinding wheel attached on a supporting member or a cup-type grinding wheel having ring- shaped pellet attached on a supporting member. These grinding wheels include abrading particles bound therein.
FIG. 1 shows a cross sectional view of a conventional cup-type polishing apparatus using a grinding wheel. A wafer 100 is placed on the top surface of a disk-shaped wafer holder 80 . A cup-type grinding wheel 90 comprises of a grinding wheel holder 93 and a ring-shaped grinding wheel 91 , which is disposed above the wafer 100 . The grinding wheel 91 is pressed and slided against the wafer 100 . The wafer holder 80 and the wafer 100 are rotated in the direction of the arrow H while the grinding wheel 91 is rotated in the direction of the arrow J. Also, the grinding wheel 91 moves linearly in the radial direction of the wafer 100 (indicated by the arrows K). Thus, the entire surface of the wafer 100 is uniformly polished by the grinding wheel 91 .
In this apparatus, the wafer holder 80 is surrounded with a table surface 95 so that even if the rotational axis m of the grinding wheel 90 moves away from the outer periphery of the wafer 100 , tilting of the grinding wheel 90 is prevented by supporting the grinding wheel 91 on the table surface 95 .
This apparatus presents the following problems.
(1) In this design, it is difficult to adjust the surface levels between the wafer 100 and the table surface 95 so as to keep the same level therebetween, and basically, it is virtually impossible to attain a completely level surface.
(2) Polishing speed of the grinder 90 is rather slow, and the productivity is generally low.
(3) It is necessary to dress the grinding surface of the grinding wheel 91 after a given usage, to refurbish the polishing quality of the grinding wheel 91 , using a separate dressing tool. However, when a grinding wheel is being dressed, the wafer 100 cannot be polished. Thus, not only the productivity of polishing is lowered, but additionally, because a space must be allocated for the dressing tool, it becomes difficult to design a compact polishing apparatus using a cup-type grinding wheel.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a polishing apparatus having a grinding member of a compact design that can provide high efficiency for both polishing and dressing operations, and prevents tilting of the grinding member even if the rotation axis thereof is moved away from the outer periphery of the object being polished.
According to the present invention, there is provided a polishing apparatus for polishing an object using a grinding member, comprising an object holder for holding an object to be polished such that a surface to be polished is facing upward, and a dresser disk holder for holding a dresser disk for dressing the grinding member such that a dressing surface of the dresser disk is facing upward. The surface to be polished and the dressing surface are arranged so as to be coplanar. While the grinding member is polishing the object, the grinding member is being dressed by the dresser disk.
The grinding member has an abrasive surface which is facing downward, and the abrasive surface is disposed so as to straddle the surface of the object to be polished and the dressing surface of the dresser disk. The polishing and dressing occur as a result of the grinding member being pressed against and slid relative to the object and the dresser disk.
Accordingly, the polishing apparatus of the present invention provides the following advantages compared with conventional polishing apparatus having a grinding member.
Even when the center of rotation of the grinding member moves away from the outer periphery of the polishing object during a polishing operation, there is no danger of tilting the grinding member because the grinding member is supported also by the dresser disk. This arrangement eliminates the need for a separate table to prevent tilting, and provides an additional benefit in that dressing of the abrasive surface of the grinding member can be performed concurrently with polishing of the surface of the object. Therefore, there is no need to provide a separate dressing step to dress the abrasive surface of the grinding member, thereby increasing the polishing efficiency and providing a compact apparatus.
According to the present invention, a plural of object holders and a plural of dresser disk holders may be disposed for polishing a plurality of objects while the grinding member is being dressed by the plurality of dresser disks.
Accordingly, one grinding member can process a plurality of objects while being processed by a plurality of dresser disks, so that the polishing and dressing productivity is increased and the overall efficiency of the polishing operation is improved.
According to the present invention, a grinding member monitoring device may be provided to check conditions of a dressed abrasive surface of the grinding member, and a control device may be provided to control dressing conditions according to output signals from the grinding member monitoring device.
Accordingly, dressing conditions can be optimized by providing a grinding member monitoring device and a dressing control device.
According to the present invention, a weight limiting device may be provided so as to control a pressure exerted on the surface to be polished by the grinding member.
Accordingly, the polishing load can be decreased to a level, which is lower than the weight of the grinding member by providing a suspending device, which also facilitates vertical movements of a main pressing device to enable fine adjustment in pressure control.
The above and other objects, features, and advantages of the present invention will become apparent from the following description when taken in conjunction with the accompanying drawings, which illustrate a preferred embodiment of the present invention by way of example.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross sectional view of the fundamental portion of a conventional cup-type polishing apparatus having a grinding wheel.
FIG. 2 is a perspective view of a polishing apparatus having a grinding wheel in a first embodiment of the present invention.
FIGS. 3A and 3B are, respectively, a plan view and a cross sectional view of the fundamental portion of the polishing apparatus shown in FIG. 2 .
FIGS. 4A and 4B are, respectively, a side view and a plan view of the fundamental portion of the polishing apparatus in a second embodiment of the present invention.
FIGS. 5A and 5B are, respectively, a plan view and a cross sectional view of the fundamental portion of the polishing apparatus in a third embodiment of the present invention.
FIG. 6 is a block diagram of a regeneration device.
FIGS. 7A and 7B are, respectively, a side view and a plan view of the polishing apparatus in a fourth embodiment.
FIG. 8 is a partial cross sectional view of the polishing apparatus in a fifth embodiment of the present invention.
In the drawings of FIG. 1 through FIG. 8, same parts or same portions are given the same reference numerals, and their repeated explanations are omitted.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 2 shows a first embodiment of the polishing apparatus. The apparatus comprises an object holder 10 for holding a polishing object 100 , such as a semiconductor wafer, which is movably fixed on a base section 40 , and a dresser disk holder 30 for holding a dresser disk 200 , which is movably fixed on the base section 40 . A cup-type grinder 50 is attached to the bottom part of a drive shaft 45 extending from an end of an L-shaped arm section 43 , which is fixed on the base section 40 . Details of the components will be presented below.
Object holder 10 comprises a holder body 11 and a support rod 13 extending from the bottom center of the holder body 11 , which is rotated by an internal drive (not shown). Hence, object holder 10 holds and rotates a wafer 100 to be polished by the grinder 50 .
Dresser holder 30 comprises a disk body 31 which holds a disk-shaped dresser 200 , and a support rod 33 extending from the bottom center of the disk body 31 , which is rotated by an internal drive (not shown). The dresser 200 has a dressing surface, which is made of a metal disk having diamond particles of #400 particle size thereon by electroplating, or diamond particles of #400 particle size fixed on a abrading sheet attached thereon.
The surfaces of the wafer 100 and the dresser disk 200 are disposed so as to be coplanar.
The top surface of the base section 40 is provided with a guide groove 41 , and the support rods 13 , 33 for the object holder 10 and the dresser disk holder 30 , respectively, are engaged in the groove 41 . The support rods 13 , 33 are moved in a reciprocating linear pattern in the groove 41 in the direction shown by the arrow A, by virtue of a drive mechanism (not shown) while maintaining their separation distance constant.
The cup-type grinding wheel 50 comprises a ring-shaped grinder 51 (or small pieces of grinding pellets arranged in a ring shape). The grinder 50 is rotated by a drive shaft 45 of a drive device (not shown) inside the arm section 43 . The grinder 50 is disposed so that the abrasive surface of the grinding wheel 51 can straddle both the wafer 100 and the dresser disk 200 , and contact both the surface to be polished of the wafer 100 and the dressing surface of the dresser disk 200 .
Referring to FIGS. 3A and 3B, the wafer holder 10 , dresser holder 30 and the grinder 50 are independently driven. Polishing operation is carried out by rotating the holders 10 , 30 and the grinder 50 at the same time, while linearly reciprocating the wafer holder 10 and the dresser holder 30 relative to the grinder 50 in the direction of the arrow A, while maintaining the distance of separation between the holder 10 and the holder 30 constant. This arrangement enables the grinder 50 to polish the entire surface of the wafer 100 and, at the same time, to have the abrasive surface of the grinding wheel 51 be dressed by being in contact with the dresser disk 200 .
Even if the rotation center of the grinding wheel 51 moves away from the outer periphery of the surface to be polished of the wafer 100 , the grinding wheel 51 remains supported by the surface of the dresser disk 200 so that there is no danger of tilting the grinding wheel 51 .
FIGS. 4A and 4B show a second embodiment of the polishing apparatus having a grinding wheel, in which an arm section 62 is indicated by double-dot lines.
The polishing apparatus includes a pair of wafer holders 10 , 10 and dresser holders 30 , 30 disposed alternately in a square pattern. A grinding wheel 50 is disposed in the center of and above the square pattern.
Each of the wafer holders 10 , 10 and dresser holders 30 , 30 is driven by a respective drive motor 61 attached to a respective shaft 17 , 37 , and a dresser pushing cylinder 66 (dresser pushing device) for pushing the dresser disk 200 is attached to the underside of the drive motor 61 for the dresser holder 30 . Also, the left pair and the right pair of the wafer holder 10 and dresser holder 30 are each driven linearly in the direction of the arrows B by the rotation of ball screws 63 , 63 , which are disposed below the respective dresser pushing device 66 and the drive motor 61 , and which are driven by respective motors 65 , 65 . The drive motors 65 , 65 are variable speed motors so as to control the reciprocating motion of each pair the wafer holder 10 and the dresser holder 30 at any desired speed independently of the other pair in the direction of the arrows B. As in the first embodiment, the surfaces of the wafers to be polished and the dressing surfaces of the dresser disks 200 are disposed so as to be coplanar.
The grinder 50 is attached to a drive motor 71 installed on a press rod 69 of a pressing cylinder 67 (pressing mechanism), which is fixed to the center of the arm section 62 disposed above a base section 60 .
In this apparatus, two wafers 100 , 100 can be polished simultaneously by placing the wafers in respective wafer holders 10 , 10 and rotating the two pairs of wafer holder 10 and the dresser holder 30 by using the four respective drive motors 61 , while rotating the grinding wheel 50 by using the drive motor 71 . At the same time, the abrasive surface of the grinding wheel 51 is pressed against the surfaces to be polished of the wafers 100 , 100 and the dresser disks 200 , 200 by lowering the grinding wheel 51 via the pressing cylinder 67 , and the drive motors 65 are operated so that the wafer holders 10 , 10 and the dresser holders 30 , 30 are linearly moved in the direction of the arrows B. This procedure results in producing two uniformly polished wafers over their entire surfaces, as well as in performing a concurrent dressing operation on the grinding wheel 51 of the cup-type grinder 50 .
In the dressing operation, the pressing force of the dresser holder 30 can be adjusted by using the dresser pushing device 66 to press the dresser disk 200 against the abrasive surface of the grinding wheel 51 . The reason for providing the dresser pushing device 66 is explained in the following. If there is no pushing device for the dresser disk 200 , the surface to be polished of the wafer 100 and the dressing surface of the dresser disk 200 will be subjected to the same pressure exerted by the pressing cylinder 67 . However, this single-valued pressure is sometimes too high or too low for the dresser disk 200 . If the dressing pressure which is applied to the grinding wheel 51 is too high, service life of the grinding wheel 51 is significantly decreased. For this reason, a separate pushing device 66 is provided for the dresser holder 30 so that the load on the dresser disk 200 may be adjusted relative to the load applied on the surface to be polished of the wafer 100 . More specifically, for a dresser disk 200 having electroplated #100 diamond particles, for example, the stress on the dresser disk 200 should be less than 10 gf./cm 2 (981 Pa). This value should be changed depending on various conditions used in polishing the wafer 100 . Also, instead of using an air cylinder, a combination of motor and gears may be used for the dresser pushing device.
It is preferable that the dresser pushing device 66 is used, in the manner presented in this embodiment, in conjunction with two or more wafer holders 10 , each holding a wafer 100 , which are served by one grinding wheel 51 straddling the wafer holders. In such an arrangement, even if the grinding wheel moves anywhere, the design is such that the grinding wheel is always supported reliably by a plurality of wafers or polishing objects. The reason is that when the grinding wheel 51 is used in conjunction with a pair of one wafer 100 and one dresser disk 200 , if the pressure exerted by dresser disk 200 on the grinding wheel 51 is altered, there is a danger that the pressure exerted by the grinding wheel 51 on the wafer 100 may change or that the grinding wheel 51 may become tilted, causing deviation from the optimum polishing conditions. If there is no fear of such problems or the problems can be eliminated in some way it is quite acceptable to provide a dresser pushing device for the polishing apparatus in the first embodiment.
It is obvious that the number of wafer holders 10 and the dresser holders 30 can be changed to suit various applications.
FIGS. 5A and 5B show a third embodiment of a polishing apparatus having a grinding wheel.
The differences between the first and the third embodiments are that the condition of the abrasive surface of the grinding wheel 51 is monitored by a grinding wheel monitor 300 disposed in an appropriate location, and that the dressing parameters can be modified by a dressing control device 400 , according to the feedback signals from the grinding wheel or plate monitor 300 , as shown in FIG. 6 .
FIG. 6 shows a block diagram of the dressing control device 400 , which varies dressing conditions for the grinding wheel 51 by controlling the operations of the dresser-control section and the polisher-control section, according to output signals from the grinding wheel monitor 300 . For example, if it is determined that the grinding wheel 51 has not been dressed sufficiently, the pushing pressure on the dresser disk 200 may be increased or the rotational speed of the dresser disk 200 may be increased.
In short, a property of the dressed surface of the grinding wheel, is represented typically by a certain level of surface roughness value. It may be monitored by the grinding wheel monitor 300 , and output signals can be input into the dressing control device 400 through a feedback circuit to control the dressing parameters (for example, contact pressure between the dresser disk 200 and the grinding wheel 51 ) so that optimum dressing can be achieved at all times.
The grinding wheel monitor 300 may be a non-contact type transducer (optical, acoustic and the like), or contact type transducers (vibration or friction detection types or torque detection types). But it is obvious that any kind of monitor will be satisfactory if the monitor is sufficiently able to detect the dressed conditions of the abrasive surface of the grinding wheel 51 .
It would be evident that the third embodiment can be applied to the second embodiment or the following fourth and fifth embodiments.
FIGS. 7A and 7B show the polishing apparatus in a fourth embodiment, in which an arm section 62 is indicated by double-dot lines.
The difference between the fourth embodiment and the second embodiment shown in FIGS. 4A and 4B is that each wafer holder 10 , 10 and dresser holder 30 , 30 is independently movable in radial directions about the center of rotation of the grinder 50 . More specifically, respective drive motors 65 are used to rotate the ball screws 63 to drive the wafer holders 10 , 10 and the dresser holders 30 , 30 independently in the direction of the arrows C.
The reason for independent reciprocal movement for the wafer holders 10 , 10 and the dresser holders 30 , 30 is to enable fine adjustments of the polishing conditions for the wafer 100 and the dressing conditions for the grinding wheel 51 by the dresser disk 200 .
The reason for the reciprocal movement of the wafer holders 10 , 10 and the dresser holders 30 , 30 in radial directions about the center of rotation of the grinder 50 is to ensure that any wafer 100 or dresser disk 200 will be subjected to the grinding wheel 51 in relatively the same area at the same time (the same relative location and the same contact area). Therefore, all the wafers 100 and dresser disks 200 are respectively subjected to the same conditions of the grinding wheel 51 .
FIG. 8 shows a polishing apparatus in a fifth embodiment. This apparatus is different than the second embodiment apparatus shown in FIGS. 4A and 4B in that a weight limiting device is provided for the grinder 50 . More specifically, a weight 77 is attached by a rope 79 to the press rod 69 through a pulley 75 to reduce the load applied on the wafer by the grinder 50 .
This arrangement enables the reduction or elimination of the load exerted by the weight of the grinder 50 on the wafer 100 , thereby enabling polishing of the wafer 100 with a load that is less than the weight of the grinder 50 . Also, it is possible to reduce the load exerted by the pressing cylinder 67 that is necessary to lift the grinder 50 , so that the movement of the grinder 50 can be controlled precisely. This arrangement is also effective in reducing the load applied to the dresser disk 200 .
Other arrangements for limiting the weight of the grinder 50 may be applied. The weight limiting device can be attached to any location other than the press rod 69 so long as that location is on the grinder 50 . The weight limiting device can be applied to any of the foregoing embodiments but also to other types of polishing apparatus. The weight limiting device is applicable to any type of polishing apparatus in which polishing is performed by pressing an overhead grinding wheel on a polishing object while producing a relative sliding motion therebetween.
Although a certain preferred embodiment of the present invention has been shown and described in detail, it should be understood that various changes and modifications may be mad therein without departing from the scope of the appended claims.
For example, in the above examples, polishing apparatus having a cup-type grinding wheel were explained, however the present inventions is applicable not only to polishing apparatus having a grinding wheel as above mentioned, but also to polishing apparatus having a grinding member such as a disk shape and other shapes. The pressing cylinder 67 also may be replaced with other types of pushing devices, such as a motor driven pressing device.
Also, in some cases, the present polishing apparatus having a grinding wheel may be combined with a conventional CMP apparatus having a polishing cloth and polishing slurry so that the CMP process may be performed either before or after the polishing process performed by using a grinding member. | The object of the present invention is to provide a polishing apparatus having a grinding member in a compact design that can provide high efficiency for both polishing and dressing operations, and prevents tilting of the grinding member even if the rotation axis thereof is moved away from the outer periphery of the object. A polishing apparatus for an object, comprises: an object holder for holding an object to be polished, such that a surface of the object to be polished faces upward; a dresser disk holder for holding a dresser disk for dressing, such that a dressing surface thereof faces upward; and a grinding member for polishing the object, and for being dressed by the dresser disk, by pressing and sliding the grinding member relative to the object and the dresser disk. Thereby, the surface to be polished and the dressing surface are arranged so as to be coploanar, and the grinding member having an abrasive surface facing downward, is disposed so as to straddle the surface to be polished of the object and the dressing surface of the dresser disk to perform polishing of the surface to be polished and dressing of the abrasive surface of the grinding member. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a division of co-pending application Ser. No. 10/028,427, filed on Dec. 28, 2001, the entire contents of which are hereby incorporated by reference
BACKGROUND OF THE INVENTION
[0002] The invention relates to a composite driving belt provided with a carrier and a plurality of transverse elements assembled slidably thereon.
DESCRIPTION OF THE RELATED ART
[0003] Such Belt is generally known, e.g. described in U.S. Pat. Nos. 3,720,113 and 4,080,841. In the known belt, a carrier, alternatively denoted tensile element or tensile means, is composed as a package of a number of endless metal bands. The known belt may in particular be applied in a variable transmission, whereby the driving belt runs over pulleys, the substantial conical sheaves of which are adapted to be displaced axially relative to each other so that the running diameter of the driving belt over the pulley may vary. In turn, while the belt is in operation, the carrier or band package slides over a contact face, the so-called saddle part of the transverse elements. Also, the separate bands of the package slide relatively to each other during operation.
[0004] In practice the driving belt, in particular each of the bands, is under a very high tension, on the one hand to ensure a proper frictional contact between the pulleys and the transverse elements and on the other hand to properly conduct the transverse elements in the straight part of the driving belt, i.e. to prevent the belt, in particular the transverse elements in the straight trajectory part of the belt from splashing apart.
[0005] The efficiency of such Belt is rather high, but internal losses in the driving belt remain as result of frictional forces between the various parts, and as a result of such friction dissipated heat is to be removed. To meet these phenomena, the belt is in practice required to run in an oiled environment.
[0006] One manner of addressing these practical problems is addressed by European patent application 0014014, which shows a manner of draining oil to the locations where sliding contact may take place and where heat is to be removed. The main important contact areas dissipating heat are between pulley and transverse element, between saddle and tensile element and between the bands of the tensile element. According to the teaching of this publication, one flat side of each band should be profiled, such that when incorporated in a belt, this side abuts a band side without such profiling. In this manner an important oil drain is achieved by the profiling towards both sliding contacts in which a band is involved, viz. Mutually between the bands, and between the inner band of a carrier and the saddle of transverse elements.
[0007] The document thereby teaches that an improved mutual friction between the mutual bands disposed around each other leads to an efficiency increase.
[0008] From commercialised belts it is found that such profiling is applied on the inner side of such constituent metal rings of a band. This practice is also suggested by the figure of said EP publication and is confirmed by the recent patent publication EP-A-0909907.
[0009] A draw back of the known belts is that when the belt is operated in rotation transfer modes outside medium, i.e. outside ratio 1 , the efficiency decreases, in particular when the belt is operated close to so called low (LOW) or over drive (OD) mode. It is an object of the current invention to address this phenomenon, i.e. to improve the efficiency in these areas in a safe and reliable manner, i.e. without endangering the proper oiling of the various sliding contacts related to the functioning of the known belt.
SUMMARY OF THE INVENTION
[0010] According to the invention this may in particular be reached by a construction in accordance with the below features of the characterising portion of claim 1 . A construction having the feature of the invention surprisingly directs away from above said common practice of contacting, realises an improved overall efficiency through a decreased amount of friction in the above said ranges, already by the mere omission of the oiling profile. Moreover, the measure according to the invention enhances the belt's lifetime by virtue of the effect that the decreased amount friction also occurs in the much-used parts of a transmissions range of ratios. Thus according to an insight partly underlying the invention, a distinction should be made between the shape of contact faces required in a band-band contact and in a band-element contact. The radial inward directed carrier surface is relatively very smooth, at least diminished by a half compared to the roughness from known belts, while a predetermined profiling is omitted from this surface, i.e. no separate aimed treatment of the profiling can be recognised in the surface.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The invention will now be explained further by way of example along a drawing in which:
[0012] [0012]FIG. 1 represents a single ring of prior art belt;
[0013] [0013]FIG. 2, in a view according to FIG. 1 represents a belt in accordance with the invention;
[0014] [0014]FIG. 3 is a tribological graph realised by research underlying the invention, and providing the insight upon which the invention is based;
[0015] [0015]FIG. 4 represents a radial cross section of a belt, showing a transverse element and the tensile means cross section
[0016] [0016]FIG. 5 is a cross section of the transverse element along the line V-V in FIG. 4, while
[0017] [0017]FIG. 6 more in detail provides the cross section of the so-called saddle part in FIG. 5, alternatively denoted tensile means contacting face, in accordance with the invention.
[0018] [0018]FIG. 7, is a graph illustrating the efficiency characteristic of a belt in various drive ratios.
[0019] In the figures corresponding components are denoted by identical references.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0020] [0020]FIGS. 1 and 2 represent rings of a drive belt, in particular push belt as commonly known. The rings are in common applications like automotive personal vehicle and trucks, utilised in a nested arrangement of a plurality of circumscribing loops or rings, as may e.g. be taken from FIG. 4. Such a set of nested rings forms part or all of the belt's tensile means along which transverse elements are disposed freely moveable in the endless longitudinal direction of the belt. The elements are clamped between the sheaves of a set of pulleys and transmit rotation from one drive pulley to a driven pulley. The tensile means thereby serves to keep together the transverse elements pushing against each other.
[0021] When the driving belt runs over pulleys having different running diameters, the variable bands of the band package have a mutual speed difference, at least in situ of one of the pulleys. This speed difference may in practice be more than 1 meter per second between two successive bands disposed a round each other. Moreover, notably the inner bands of a carrier are pressed on to each other with substantial force, since the pressure force on a band is built up by all bands disposed outside i.e. there around.
[0022] By providing in particular the more inwardly disposed bands at least at one side with a surface profiling, through which an improved lubrication between the bands will be produced, an efficiency improvement occurs. Preferably, the surface profiling comprises grooves, which in practice provide good results. According to a further feature, the roughening value of the surface profiling lies between 0.30 and 0.75 μm Ra, here measured according to CLA method, and preferably between 0.46 end 0.55 μm Ra.
[0023] In a preferred embodiment provided in FIG. 2, the grooves are, like in the known belt, disposed in crossing sets, however at the radial outer side of the belt. A good result is achieved when the variable bands are provided with the surface profiling only at the outer one flat band side, while the radial inner side is provided relatively very smooth. The grooved profiling of the outer side of a metal band is achieved by rolling a band between rollers, one roller being fitted with a surface profiling on the circumferential surface.
[0024] The drawing in FIG. 1 diagrammatically shows an endless metal band. The width of such a hand may e.g. range between 5 and 20 mm and the thickness between 0.15 end 0.25 mm. The diameter of the band in circular condition may e.g. range between 150 and 400 mm. The endless band has an exterior side 1 and an interior side 2 . In the known embodiment of FIG. 1, the interior side 2 is provided with a surface profiling of cross wise disposed grooves, whereas in the embodiment according to the invention this profiling is made to the exterior side 1 of a ring of a belt. In this manner, a band-element contact is made by the flat side of the ring. According to a preferred embodiment of the invention a 11 rings of a belt's tensile means are incorporated in this manner.
[0025] It is further derived from the investigations underlying the current invention that contrary to the known manner of lubricating the contact between a carrier face and the saddles of the transverse elements a better performance is achieved alternatively at applying a combined set of measures. According to this set of measures, for lubrication of this contact should be relied on a natural flow of oil between element and carrier in combination with a very much smoothened surface area of both contacting faces, i.e. saddle face and the inner band facing of a carrier. However according to the invention, primarily, the smoothening, expressed in roughness index Ra, of both faces should be such that the so-called combined roughness Ra′, i.e.
Ra′=SQRT ( Ras 2 +Rar 2 ) (1)
[0026] where
[0027] Ra′=the reduced roughness index
[0028] Ras=the average roughness index of the saddle surface expressed in Ra.
[0029] Rar=the index for the average roughness of the inner ring face contacting the saddle.
[0030] SQRT=square root of ( . . . )
[0031] meets the requirement to remain smaller than 0.5 μm, preferably to remain within the area smaller than 0.25 μm.
[0032] [0032]FIG. 3 diagrammatically reflects a curved typical relation according to the invention between a friction coefficient or index, linearly indexed along the Y-axis of the figure, and a “belt and oil features” index L, alternatively Lubrication number L, logarithmically indexed along the X-axis. The index L is calculated utilising the formula:
L = η 0 V r p av R a ( 2 )
[0033] in which:
[0034] L=a lubrication number or index in accordance with an insight underlying the invention;
[0035] Vr=the relative speed between the two contacting surfaces, here of the inner belt ring and a transverse element's saddle;
[0036] η 0 =the dynamic viscosity index of the lubricating medium;
[0037] Pav=the average Hertzian stress within the band/saddle contact;
[0038] Ra=the combined surface roughness Ra′ of both saddle and ring surface.
[0039] The combined surface roughness' is alternatively denoted reduced roughness is calculated in the ordinary manner in the art provided above, expressed in roughness coefficient Ra′.
[0040] The principal characteristic of the curved relation given by formula 1 and FIG. 3 is according to the invention determined by dominant parameters Vr, and Ra, whereas the viscosity and the average Hertzian pressure parameters are in accordance with the insight according to the invention not, at least not directly related to design parameters of the belt. The formula (2) according to the invention more in particular reveals that relative speed Vr is the most dominant factor for influencing the friction coefficient since also Ra is given once the belt is set into operation.
[0041] [0041]FIG. 3 shows in accordance with experimental results of research underlying the invention and matching the index line of formula 1, that the relation between an actual friction coefficient and the lubrication index appears to typically follow a curve with three main sections. In the first section BL, suggestedly where so called boundary lubrication, i.e. shearing contact exists between the two contacting surfaces, the friction coefficient is virtually constant with increasing index L. In a second section ML, suggestedly where mixed lubrication and friction occurs, the friction coefficient drops with increasing L number, typically from somewhere like 0.18 to somewhere like 0.01. In the third section HL, where suggestedly hydrodynamic lubrication exists, i.e. with shear occurring within the lubricant and not between the contacting surfaces, the actual friction index has it's lowest value and again is virtually constant or may slightly increase again with increasing value of L.
[0042] [0042]FIG. 7 diagrammatically shows the efficiency curve of a known belt. It reveals that efficiency is lowest towards the extreme ends of a typical ratio range, i.e. between overdrive ratio area OD to the left of the graph and low drive ratios area LOW to the right of the graph. In the exemplary graph typical values for ratio i at LOW are around i=2.4 while at OD area ratio i is around i=0.5. Highest efficiency occurs in Medium ratio with i=1. With the measure in accordance with the invention, i.e. with fully smooth contacting faces of preferably low roughness contacting each other, the efficiency of the belt is increased by an amount within the higher part within the range between 0.25 and 1% of efficiency increase, whereas the extreme ends of the ratio range show an increase of values within the lower part of the range. The overall increase in efficiency is of considerable significance at long life operation of the belt.
[0043] The efficiency increase achieved by the primary, above-mentioned measure is in accordance with a further, separate though here combined measure according to the invention achieved by a specific shaping of the transverse elements saddle. This measure in particular, i.e. mostly effects the belt efficiency towards the LOW and OD sides of the ratio range. The measure is illustrated by the drawing in FIG. 7, described in the following.
[0044] [0044]FIG. 4 provides a cross section of a belt and a view of a transverse element known per se, depicted according to a view in the longitudinal direction of the belt. FIG. 5 is a transverse cross section thereof over the line B-B, with the tensile means being omitted from the drawing, providing a view in a belt's axial direction. FIG. 6 in an enlarged scale depicts the in FIG. 5 encircled part of the element, in fact the part which contacts the inner face of a belts tensile means, the so called saddle of an element, here shaped in accordance with the invention.
[0045] In the saddle according to the invention the contacting face is shaped so as to realise both a line shaped contact between tensile means and saddle and a wedge shaped space between the relevant contacting element and the portion of the tensile means extending over the relevant element. According to the invention, in this manner lubricating medium, at normal operation applied constantly to the belt, may be collected in a manner so as to have a concentration at a point, i.e. an axial line of contact between the tensile means and the saddle. With this concentration of lubricating medium, sufficient amount of medium is ensured for realising the conditions to achieve a so-called Hydrodynamic Lubrication in the contact between saddle and tensile means. The saddle is also shaped such so as to achieve the same condition also in cases where the relative movement between saddle and tensile means in the longitudinal direction, depending on the operating conditions of the belt, may temporarily be reversed. At achieving the said lubricated condition in the said mutual contact, use is made of the insight that the element and the tensile means each have a different effective radius of rotation within a pulley, so that relative difference Vr in velocity of each belt component occurs, thereby creating the possibility of having a lubricated contact. To achieve such condition, the saddle is in accordance with the invention, as taken in cross section, provided with an elliptical shape. In this manner, with respect to a lubricated contact, even at the circular trajectory with smallest radius of a belt within a transmission, a sufficient amount of wedge shaped spacing, the so called entry space, between the tensile means and the saddle is guaranteed before the mutual contact takes place.
[0046] It will be evident from the preceding description that it is a further prerequisite in accordance with the invention that for achieving the desired condition in the mutual contact, the local bending radius Rb of the band, i.e. tensile means, and of the saddle Rs may not be equal, thus:
Rb< >Rs ( 4 a )
[0047] while also
Rs<Rb ( 4 b )
[0048] In accordance with a further aspect underlying the invention, the combined local radius, i.e. the reduced radius of both the saddle and the tensile means is taken into consideration by the requirement:
1 /Rr= 1 /Rs+ 1 /Rb (5)
[0049] Where
[0050] Rr=the reduced radius of a Carrier and Saddle face contact
[0051] Rs=the local radius of the saddle measured in mm
[0052] Rb=the instantaneous radius of the band measured in mm
[0053] It is in accordance with the invention considered that for most applications of a belt, generally Rs should range up to 25 mm, whereas Rr for commonly applied transmissions typically ranges between 25 and 80 mm during operation of the Belt. Both the radii are taken in accordance with the radial and longitudinal direction of a belt, considering the normal operation and configuration thereof in a pulley. More in particular it is considered that for realising the said wedge shaped entry space at the largest amount of possible contacting locations on a saddle, as taken in longitudinal direction of the belt over the saddle surface, without the radii of saddle and band becoming equal, the saddle should according to the preferred embodiment be shaped elliptical, with the ellipse extending over virtually the entire thickness of an element, thereby obviating non-continuous transitions in a possible contacting surface since from experience underlying the invention it is known that these will break, i.e. remove the lubricated condition in the mutual contact. Thus, in dependence of an elements thickness, the saddle is shaped so as to at least largely, e.g. within 90% reliability, correspond to the shape of a half ellipse, the corresponding ellipse being defined by the mathematical formula for an ellipse and departing from the prerequisites in accordance with the insights underlying the invention according to which, the ellipse largest width corresponds to the elements width, while the derived local radius of curvature at the ellipse largest height should be smaller than the smallest possible radius of curvature of the belt. In this manner, also a continuous transition from the elements principal face to the saddle is achieved, i.e. by an infinitely small radius of curvature.
[0054] The invention particularly aims at realising a generally applicable design rule. Thus it is taken that for most applications a minimum element thickness will be 1.5 mm, while a smallest radius of curvature, either defined by the physical features of the belt or by the smallest diameter of transmission shafts over which the belt will run, will be about 25 mm. It is to be understood that in the latter respect the specification of the belt, i.e. the prescribed boundaries of use take precedence over the radius that a belt may actually presume due to it's physical characteristics. Thus in accordance with a preferred embodiment and design rule of the invention, a generally applicable shape is attained of which the largest diameter through the elliptical centre is 1.5 mm, the shortest diameter about 0.046 mm or smaller, while the local radius of curvature concurring with the line of the said shortest diameter is 25 mm or smaller, while the radius of curvature over the line concurring with the line of the said largest diameter, is 6.75 E-4 mm, i.e. infinitely small, thus obviating a non-continuous transition from an element principle plane to the saddle surface.
[0055] For even better performance of a belt and transmission in accordance with the invention the invention provides to apply an lubricating medium in the form of an oil type having a dynamic viscosity η larger or equal to 9 MPa*s at a nominal temperature of 100 degrees Celsius, preferably also having a kinematic viscosity v larger than or equal to 10 E-6 m 2 /s. In this manner all factors influencing the quality and efficiency of operation of a belt are optimised, more importantly, are brought into a functionally safe area.
[0056] In the latter respect, according to a further aspect of the invention, the so-called rocking edge of the belt is provided below 1 mm from the saddle surface, more in particular in a range between 1.25 and 2 mm below the saddle surface. In this manner it is achieved to increase the relative velocity Vr between saddle and tensile means, alternatively denoted carrier, in particular at the extreme OD and LOW ends of the range of ratios in which the belt will operate. In combination with any, preferably all of the previous measures this measure appears to increase the belts efficiency, in particular in these LOW and OD areas in which the belt may operate most of its operating time.
[0057] The invention further relates to all details of the figures pertaining to the description and all features defined in the following claims. | A composite driving belt provided with a carrier and a plurality of transverse elements assembled slidably thereon, the carrier including one or more bands, preferably composed of a plurality of endless metal bands disposed radially around each other, each element being provided with a radially outward directed carrier contact plane for contacting a radial inner contact plane of the carrier while in operation, wherein the contact plane of both the carrier and the element have a non profiled surface. In particular the roughness and shape of the relevant contacting faces of a belt are adapted to achieve a hydrodynamic lubricating condition, while the lubricating oil is defined to meet the requirements of an improved efficiency push belt. | 5 |
This application is a Rule 60 Divisional of U.S. Ser. No. 826,229 filed on Feb. 5, 1986, now U.S. Pat. No. 4,710,555, which is a continuation-in-part of U.S. Ser. No. 688,238, filed on Jan. 2, 1985 now abandoned, which is a continuation-in-part of U.S. Ser. No. 560,543, filed on Dec. 12, 1983, now abandoned.
FIELD OF THE INVENTION
The present invention relates to improved viscosification agents for a variety of aqueous solution which comprises a family of intramolecular polymeric complexes (i.e., polyampholytes) which are terpolymers of acrylamide/metal styrene sulfonate/methacrylamidopropyltrimethylammonium chloride (MAPTAC). These polymeric materials have viscosity-polymer concentration relationships that are invarient with the addition of high levels of acid, base and salt to the fresh water system.
The metal styrene sulfonate is an anionic monomer, while MAPTAC is cationically charged. These acrylamide-based polyampholytes have approximately 1 to about 50 mole % of the anionic monomer and approximately 1 to about 50 mole % of the cationic moiety present within the macromolecular structure. These groups are not necessarily present in an equimolar charge ratio. The excess undissociated charge allows for facile dispersability of solubility of the polyampholytes to fresh water.
BACKGROUND OF THE INVENTION
In recent years, there has been a renewed interest in the behavior of ion-containing polymers in fresh and high ionic strength aqueous media. These materials have a variety of useful properties, including the ability to expand its hydrodynamic volume in fresh water as the polymer concentration is diluted resulting in an increase in the solution viscosity. It is generally accepted that this expansion is due to the repulsion between like charges chemically bonded to the chain backbone (i.e., polyelectrolyte effect). However, if the influence that each charge has on each other is screened, than the chain will contract and the viscosity will correspondingly decrease. A very effective screening mode becomes operative through the addition of a soluble salt, such as sodium chloride. Therefore, these homogeneously charged polymers are not generally useful viscosifiers in high ionic strength medium.
Recently we have developed a novel class of ionomeric polymers in which cationic and anionic groups are chemically attached to the backbone chain. The hydrodynamic volume of these intramolecular complexes, i.e., polyampholytes, expand with the addition of soluble acids, bases, or salts. This is due primarily to the inability of the ionomeric monomer units to move freely into the bulk solution as found in classical polyelectrolytes. Thus, these complexes are more soluble in high ionic strength solutions than in fresh water and have a higher viscosity in the former than the latter solution. Moreover, an equimolar ratio of anionic and cationic groups are not required for these materials to function effectively.
We report the finding that specific intramolecular polymeric complexes, composed of neutral (acrylamide), cationic (methacrylamidopropyltrimethylammonium chloride), and anionic (sodium salt of styrene sulfonate) monomer units are capable of retaining its fresh water viscosification characteristics with the addition of a soluble salt. That is, the viscosity of these polymer solutions remains essentially unchanged with the addition of acid, base or salt. In qualitative terms, these polymers are polyampholytes with a relatively minor amount of dissociable and mobile charge which counterbalance (via charge screening mechanism) the previously detailed chain expansion. These viscosity characteristics are novel, since the general tendency of homogeneously charged macromolecules in these types of aqueous solutions shows a marked decrease in thickening efficiency.
These novel polymers can be useful in a variety of technologically interesting fluids as required in well control and workover fluids and in other systems where viscosity concentration relationships are required to be invarient with the addition of high levels of salt to the fresh water system.
Typical water soluble monomers incorporated into the terpolymers that are envisioned in the present invention are listed as follows:
Anionic: 2-acrylamido-2 methylpropane sulfonic acid, sodium styrene sulfonate, (meth) acrylic acid, 2-sulfoethylmethacrylate, and the like.
Cationic: methacrylamidopropyltrimethylammonium chloride, dimethyldiallylammonium chloride, diethyldiallylammonium chloride, 2-methacryloxy-2-ethyltrimethylammonium chloride, trimethylmethacryloxyethylammonium methosulfate, 2-acrylamido-2-methylpropyltrimethylammonium chloride, vinylbenzyltrimethylammonium chloride, and the like.
Nonionic: (N,N-dimethyl) acrylamide, hydroxyethyl (meth) acrylate, alkyl substituted acrylamides, (meth) acrylates, N-vinyllactanes (e.g., n-vinyl-2-pyrrolidone), and the like.
These monomers possess the appropriate water solubility for polymerization to take place.
Salamone et al., of the University of Lowell (Massachusetts), have investigated ampholytic polymers. They have studied the solution properties of divinylic cationic-anionic monomer pairs and also cationic-anionic monomer pairs with a neutral comonomer. This latter group of materials contains styrene as the neutral comonomer (J. Polym. Sci. Al, 18, 2983 [1980]), which can be incorporated into the ampholytic macromolecular structure through both solution or emulsion polymerization schemes. Apparently, other neutral vinylic monomers (i.e., acrylamide) were also polymerized (Gordon Research Conference--1981); but as of the present time, reports of this work have not been published in the scientific literature. However, in all of Salmone's work, detailed descriptions of his synthesis is reported. In all instances, the polymerization of the anionic-cationic monomeric species occurred via an "ion-pair comonomers that have no nonpolymerizable counterions present" (J. Polym. Sci. Letters, 15, 487 [1977]). The physical and chemical properties of these ion-pair comonomers are quite different than the individual ions (J. Polym. Sci. Letters 15, 487 [1977]).
Excess dissociable charges are not present within these polymeric materials.
SUMMARY OF THE INVENTION
The present invention relates to a novel family of intramolecular polymer complexes synthesized from acrylamide, sodium styrene sulfonate, and methacrylamidopropyltrimethylammonium chloride, having viscosity-polymer concentration relationships that are invariant with the addition of high levels of acid, base, or salt to the fresh water system. These complexes possess a "balance" between conventional polyelectrolyte and polyampholyte behavior.
The polymers of the instant invention have solution properties that remain approximately constant as high levels of acid, base or salt are added to the solution. There is no rise in the solution properties as acid, base or salt is added.
The present invention relates to improved viscosification agents for an aqueous solution which can contain high concentrations of acids, bases, or salts. Typically, the viscosification agents are intramolecular polymeric complexes (i.e., polyampholytes) which are formed by a free radical terpolymerization of acrylamide monomer, sodium styrene sulfonate monomer and methacrylamidopropyltrimethylammonium chloride (MAPTAC) monomer, wherein the formed water soluble terpolymers have the formula: ##STR1## wherein x is about 0.1 to about 50 mole %, more preferably about 1 to about 48 mole %, and most preferably about 3 to about 45 mole %, y is about 1 to about 50 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to about 10 mole %, and z is about 1 to about 50 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to about 10 mole %, A is about 1 to about 25 mole%, wherein y is equal to z and y, z and A are les than 50 mole % and M is selected from the group consisting of amines and a metallic cation being selected from the group consisting of lead, iron, aluminum, Groups IA, IIA, I Bond IIB of the Periodic Table of Elements. These ionic groups are not present in an equimolar charge ratio, since the excess undissociated charge allows for facile dispersibility of the polyampholytic into fresh water. In addition, this excess charge prevents the hydrodynamic volume of the polyampholyte from expanding or contracting in the previously described acid, base, and salt solutions, thus preventing a viscosity increase upon the addition of acid, base or salt to the aqueous solution containing the terpolymer.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates viscosity concentration of the polyampholyte in fresh water.
FIG. 2 illustrates viscosity concentration of the polyampholyte in a 1 molar sodium chloride solution.
GENERAL DESCRIPTION
The instant invention describes a new class of terpolymers which are improved viscosification agents for aqueous solutions containing acid, base, or salt. Typically, these terpolymers are formed by a free radical terpolymerization process in an aqueous medium of an acrylamide monomer, a sodium styrene sulfonate monomer and a methacrylamidopropyltrimethylammonium chloride monomer. The resultant water soluble terpolymer has the formula which possess an excess of sodium styrene sulfonate monomer--the anionic monomer. ##STR2## wherein x is about 0.1 to about 50 mole %, more preferably about 1 to about 48 mole %, and most preferably about 3 to about 45 mole %, y is about 1 to about
50 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to about 10 mole %; and z is about 1 to about 50 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to about 10 mole %, A is about 1 to about 25 mole%, wherein y is equal to z and y, z and A are less than 50 mole % and M is selected from the group consisting of amines and a metallic cation being selected from the group consisting of lead, iron, aluminum, Groups IA, IIA, I Bond IIB of the Periodic Table of Elements, the ratio of A/y+z should be about 0.1 to about 15 and the ionic content is about 50 to about 99 mole percent.
Several other polymer compositions were synthesized along the identical synthetic route. The composition of these polymers are shown in the following formulae: ##STR3## wherein x is about 0.1 to about 50 mol %, more preferably about 1 to about 48 mole %, and most preferably about 3 to about 45, y is about 1 to about 50 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to about 10 mole %, and z is about 1 to about 50 mole %, more preferably about 2 to about 20, and most preferably about 5 to about 10, y is equal to z, B is about 1 to 25 mole %, more preferably about 2 to about 20 mole %, and most preferably about 5 to 10 mole %, wherein B, y and z are less than 50 mole % and the ratio of B/y+z is about 0.01 to about 15.
The molecular weight, as derived from intrinsic viscosities, for the terpolymers of acrylamide/sodium styrene sulfonate/methacrylamidopropyltrimethylammonium chloride is about 10 3 to about 5×10 6 , more preferably about 10 4 to about 2×10 6 and most preferably about 10 5 to about 10 6 . The means for determining the molecular weights of the water soluble terpolymers from the viscosity of solutions of the terpolymers comprises the initial isolation of the water soluble terpolymers, purification and redissolving the terpolymers in water to give solutions with known concentrations. The flow times of the solutions and the pure solvent were measured in a standard Ubbelholde viscometer. Subsequently, the reduced viscosity is calculated through standard methods utilizing these values. Extrapolation to zero polymer concentration leads to the intrinsic viscosity of the polymer solution. The intrinsic viscosity is directly related to the molecular weight through the well-known Mark-Houwink relationship.
The water soluble terpolymers of acrylamide/sodium styrene sulfonate/methacrylamidopropyltrimethylammonium chloride are formed by a conventional free radical terpolymerization in an aqueous medium which comprises the steps of forming a reaction solution of acrylamide monomer, sodium styrene sulfonate monomer and methacrylamidopropyltrimethylammonium chloride monomer typically (50 wt. % solution in water) in distilled water, wherein the total monomer concentration is about 1 to about 40 grams of total monomer per 100 grams of water, more preferably about 5 to about 30, and most preferably about 10 to about 20; purging the reaction solution with nitrogen; adding sufficient acid to the reaction solution to adjust the pH of the reaction solution to about 4.5 to about 5.0; heating the reaction solution to at least 55° C. while maintaining the nitrogen purge; adding sufficient free radical initiator to the reaction solution at 55° C. to initiate terpolymerization of the acrylamide monomer, the sodium styrene sulfonate monomer, and the methacrylamidopropyltrimethylammonium chloride monomer; terpolymerizing said monomers of acrylamide, sodium styrene sulfonate and methacrylamidopropyltrimethylammonium chloride at a sufficient temperature and for a sufficient period of time to form said water soluble terpolymer; and recovering said water soluble terpolymer from said reaction solution.
The total concentration of monomers in the polymerization solvent (e.g. water) is about 1 to about 40 grams of total monomer per 100 grams of water, more preferably about 5 to about 30 and most preferably about 10 to about 20. Terpolymerization of the acrylamide monomer, sodium styrene sulfonate monomer, and methacrylamidopropyltrimethylammonium chloride monomer is effected at a temperature of about 30 to about 90, more preferably at about 40 to about 70, and most preferably at about 50 to about 60 for a period of time of about 1 to about 24 hours, more preferably about 3 to about 10, most preferably about 4 to 8.
As is well known to those versed in the art, the level of ionic monomers incorporated in the growing polymer chain is directly related to the initial concentration of the reacting species. Therefore, modulation of the ionic charge within the polymer structure is accomplished through changes in the initial anionic and/or cationic vinylic monomer concentrations.
A suitable method of recovery of the formed water soluble terpolymer from the aqueous reaction solution comprises precipitation in acetone, methanol, ethanol and the like.
Suitable free radical initiators for the free radical terpolymerization of the acrylamide monomers, the sodium styrene sulfonate monomer, and the methacrylamidopropyltrimethyl ammonium chloride monomer are selected from the group consisting of potassium persulfate, ammonium persulfate, benzoyl peroxide, hydrogen peroxide, azobisisobutyronitrile, and the like. The concentration of the free radical initiator is about 0.001 to about 2.0 grams of free radical initiator per 100 grams of total monomer, more preferably about 0.01 to about 1.0 and most preferably about 0.05 to about 0.1.
It should be pointed out that neither the mode of polymerization (solution, suspension, or emulsion polymerization technique and the like), nor the initiator is critical, provided that the method or the products of the initiation step does not inhibit production of the polyampholyte or chemically modify the initial molecular structure of reacting monomers.
Typicaly water soluble monomers incorporated into the terpolymers that are envisioned in the present invention are listed as follows:
Anionic: 2-acrylamido-2-methylpropane sulfonic acid, sodium styrene sulfonate, (meth) acrylic acid, 2-sulfoethylmethacrylate, and the like.
Cationic: methacrylamidopropyltrimethylammonium chloride, dimethyldiallylammonium chloride diethyldiallylammonium chloride, 2-methacryloxy-2ethyltrimethylammonium chloride, trimethylmethacryloxyethylammonium methosulfate, 2-acrylamido-2-methylpropyltrimethylammonium chloride, vinylbenzyltrimethylammonium chloride, and the like.
Nonionic: (N,N-dimethyl)acrylamide, hydroxyethyl (meth)acrylate, alkyl substituted acrylamides, (meth)acrylates, N-vinyllactanes (e.g., n-vinyl-2-pyrrolidone), and the like.
These monomers possess the appropriate water solubility for polymerization to take place.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following examples illustrate the present invention, without; however, limiting the same hereto.
EXAMPLE 1
Synthesis
A representative example for the synthesis of the intramolecular polymer complexes (designated 136A) is outlined below.
Into a 1-liter, 4-necked flask add:
12.08 g methacrylamidopropyltrimethylammonium chloride (MAPTAC), 50% aqueous solution
5.64 g sodium styrene sulfonate (SSS)
35.0 g acrylamide (AM)
300 ml. distilled water
or on a molar basis
5.0 moles MAPTAC
5.0 moles SSS
90.0 moles AM
We should emphasize that the anionic and cationic monomers were added to the aqueous phase without attempting to form ion-pair comonomers that do not possess nonpolymerizable counterions.
The solution was purged with nitrogen gas for approximately one hour to remove dissolved oxygen. As the nitrogen gas purging began, the solution is heated to 50° C. At this point, 0.1 g potassium persulfate (i.e., initiator) was added to the solution. After 8 hours, the polymer was precipitated from solution with acetone. Subsequently, the resulting polymer was washed several times with a large excess of acetone and dried in a vacuum oven at 60° C. for 24 hours.
The composition of 136A is as follows:
x=0.90 Y+Z=0.082 A=0.018
Note that the polymer structure has 1.8 mole % "excess" nonpolymerizable free charge attached to some of the styrene sulfonate units.
EXAMPLE 2
A further representative example for the synthesis of an intramolecular polymr complex (designated 136B) is similar to Example 1, except for the initial monomer feed composition. This is outlined below.
34.6 g methacrylamidopropyltrimethylammonium chloride, 50% aqueous solution
5.76 g sodium styrene sulfonate
35.0 g acrylamide
or on a molar basis
5.0 moles MAPTAC
7.0 moles SSS
88.0 moles AM
The composition of 136B is as follows:
x=0.887
Y+Z=0.087
B=0.026
Note that the polymer structure has 2.6 mole % "excess" nonpolymerizable free charge attached to some of the MAPTAC units.
EXAMPLE 3
A further representative example for the synthesis of an intramolecular polymer complex (designated 136C) is similar to Example 1, except for the initial monomer feed composition. This is outlined below.
45.5 g methacrylamidopropyltrimethylammonium chloride, 50% aqueous solution
5.9 g sodium styrene sulfonate
35.0 g acrylamide
or on a molar basis
5.0 moles MAPTAC
9.0 moles SSS
86.0 moles AM
The composition of 136C is as follows:
x=0.871
Y+Z=0.091 B=0.038
Again, it should be noted that the polymer structure has 3.8 mole % "excess" nonpolymerizable free charge attached to some of the MAPTAC units.
136A is best described as an intrapolymer complex with a modest amount of anionic charge, while 136B and 136C terpolymers contain increasing amounts of cationic charge.
As is well known to those versed in the art, the level of ionic monomers incorporated in the growing polymer chain is directly related to the initial concentration of the reacting species. Therefore, modulation of the ionic charge within the polymer structure is accomplished through changes in the initial anionic and/or cationic vinylic monomer concentrations.
We would also recognize that the above described polymers are only one example of a whole family of water-soluble polymers capable of possessing high degrees of acid, base, or salt tolerance in solution. The major requirement is the availability of water-soluble (and polymerizable) anionic, cationic, and neutral vinylic monomers.
EXAMPLE 4
In FIGS. 1 and 2 are typical data of the viscosity-polymer concentration behavior of fresh water (FIG. 1) and 1 molar sodium chloride solutions (FIG. 2) containing the above described polymers, i.e., 136A, 136B and 136C.
The 136B data show a decrease in viscosity occurs at all polymer levels due to the dominant influence of the dissociabled charge over the intrapolymer complex i.e., y+z. <B. The ratio
B/(y+Z)=0.3
in this instance.
The 136C data show the effect of significantly increasing the level of dissociable charge over the complex concentration, i.e.,
B/(y+Z)=0.42
As the salt level is increased, the viscosity values deteriorate rapidly at all polymer concentrations. That is, this polymer is behaving as a classical polyelectrolyte than an intrapolymer complex. More specially, the dissociable charges are largely dominating the solution behavior of this polymeric material.
The 136A data show the effect of lowering the
A/(y+Z)
ratio, (=0.25), to a modest degree. The viscosity concentration profiles show that little change occurs with the addition of sodium chloride. Therefore, it is readily observed that this material possesses a very high degree of salt tolerance. Apparently, a balance is achieved between the influence of the dissociable charge and the intrapolymer complex structure on the hydrodynamic volume of the polymer chain.
In summary, what we claim is the synthesis of a water-soluble copolymer material possessing a high degree of salt tolerance, such as in 136A. This material contains a balance between the influence of the highly mobile dissociable charges and the anionic-cationic monomer complex structure. The latter structures allow the hydrodynamic volume of the polymer to increase with addition of a soluble, low molecular weight additive. The former charges cause the chain to shrink upon acid, base, or salt addition. If an "imbalance" between these two factors exist, then the viscosity will increase or decrease accordingly (136B and 136C). In addition, although the molecular weight, complex composition, dissociable charge structure, and charge density can be varied over a relatively wide range, substantially different and improved salt tolerance results as compared to conventional homogeneously-charged polyelectrolytes and previously described intrapolymer complexes. | Intramolecular polymer complexes synthesized from acrylamide, sodium styrene sulfonate, and methacrylamidopropyltrimethylammonium chloride, having viscosity-polymer concentration relationships that are invarient with the addition of high levels of acid, base, or salt to the fresh water system. These complexes possess a "balance" between conventional polyelectrolyte and polyampholyte behavior. | 2 |
[0001] This application is a continuation application claiming priority to Ser. No. 15/070,127, filed. Mar. 15, 2016, which is a continuation of Ser. No. 14/455,974, filed Aug. 11, 2014, U.S. Pat. No. 9,327,198, issued May 3, 2016, which is a continuation of 13/013,478, filed on Jan. 25, 2011, U.S. Pat. No. 9,199,172, issued Dec. 1, 2015.
BACKGROUND
[0002] The present application relates to the field of computers, and specifically to the use of computers in management of software design, coding and other work events, normally used in building software applications. Even more particularly, the present invention relates to the use of computers in creating events, scoring submitted designs and code, and rewarding event participants for submissions that meet an acceptance criteria.
BRIEF SUMMARY
[0003] A computer implemented apparatus and computer program product provides design, coding, and other work challenge events and competition events associated with building a software application. The apparatus includes a portal for communicating the events to potential participants and receives computer software designs and code submissions from selected participants. An event manager server creates the events. The apparatus includes a catalog of reusable code assets and a pricing calculator on the event manager server for pricing the event based on use of the catalog and based on results of previous events as determined by an analytics engine. Participants are selected using a selector subsystem. Computer code submitted by the selected participants is executed in a challenge server layer and also evaluated and scored. A design event may require creation of a formal document or use of a design tool such a Rational Software Architect available from International Business Machines Corporation of Armonk, N.Y. A payment application rewards participants according to the event specifications and the scoring results or other outcome meets the event specifications and a minimum threshold scoring result.
[0004] A major benefit of the present invention is that challenge and competition events are completed in short cycles. Research has shown that work that is properly broken down to a consumable level can be completed with the highest chance of success. Although, any cycle time may be used with the present invention, typically events are conducted in short cycles, usually of three to seven days duration using work specifications that have been broken down to a consumable level.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0005] FIG. 1 depicts an exemplary computer in which the present invention may be implemented;
[0006] FIGS. 2 a and 2 b are block diagrams showing the progression of a challenge event and a competition event respectively; and
[0007] FIG. 3 is a block diagram of one embodiment of the present invention.
DETAILED DESCRIPTION
[0008] As will be appreciated by one skilled in the art, aspects of the present invention may be embodied as a system or computer program product. Accordingly, aspects of the present invention may take the form of an entirely hardware embodiment, and entirely software embodiment (including firmware, resident software, micro-code, etc.) or an embodiment combining software and hardware aspects that may all generally be referred to herein as an “apparatus” “module” or “system.” Furthermore aspects of the present invention may take the form of a computer program product embodied in one or more computer readable storage mediums(s) having computer readable program code embodied thereon.
[0009] A computer readable storage medium may be, for example, but not limited to, an electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system, apparatus, or device, or any suitable combination of the foregoing. More specific examples (a non-exhaustive list) of the computer readable storage medium would include the following: an electrical connection having one or more wires, a portable computer diskette, a hard disk, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only (EPROM or Flash memory), a portable compact disc read-only memory (CD-ROM), an optical storage device, a magnetic storage device, or any suitable combination of the foregoing. In the context of this document, a computer readable storage medium may be any tangible medium that can contain, or store a program for use by or in connection with an instruction execution system, apparatus, or device.
[0010] Computer program code for carrying out operations for aspects of the present invention may be written in any combination of one or more programming languages, including an object oriented programming language such as Java, Smalltalk, C++ or the like and conventional procedural programming languages, such as the “C” programming language or similar programming languages. The program code may execute entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the latter scenario, the remote computer may be connected to the user's computer through any type of network, including a local area network (LAN) or a wide area network (WAN), or the connection may be made to an external computer (for example, through the Internet using an Internet Service Provider).
[0011] Aspects of the present invention are described below with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems) and computer program products according to embodiments of the invention. It will be understood that each block of the flowchart illustrations and/or block diagrams, and combinations of blocks in the flowchart illustrations and/or block diagrams, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the flowchart and/or block diagram block or blocks.
[0012] These computer program instructions may also be stored in a computer readable medium that can direct a computer, other programmable data processing apparatus, or other devices to function in a particular manner, such that the instructions stored in the computer readable medium produce an article of manufacture including instructions which implement the function/act specified in the flowchart and/or block diagram block or blocks.
[0013] The computer program instructions may also be loaded onto a computer, other programmable data processing apparatus, or other devices to cause a series of operational steps to be performed on the computer, other programmable apparatus or other devices to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide processes for implementing the functions/acts specified in the flowchart and/or block diagram block or blocks.
[0014] With reference now to the figures, and in particular to FIG. 1 , there is depicted a block diagram of an exemplary computer 102 , which may be utilized by the present invention. Note that some or all of the exemplary architecture, including both depicted hardware and software, shown for and within computer 102 may be utilized by software deploying server 150 .
[0015] Computer 102 includes a processor 104 that is coupled to a system bus 106 . Processor 104 may utilize one or more processors, each of which has one or more processor cores. A video adapter 108 , which drives/supports a display 110 , is also coupled to system bus 106 . System bus 106 is coupled via a bus bridge 112 to an input/output (I/O) bus 114 . An I/O interface 116 is coupled to I/O bus 114 . I/O interface 116 affords communication with various I/O devices, including a keyboard 118 , a mouse 120 , a media tray 122 (which may include storage devices such as CD-ROM drives, multi-media interfaces, etc.), a printer 124 , and external USB port(s) 126 . While the format of the ports connected to I/O interface 116 may be any known to those skilled in the art of computer architecture, in one embodiment some or all of these ports are universal serial bus (USB) ports.
[0016] As depicted, computer 102 is able to communicate with a software deploying server 150 using a network interface 130 . Network 128 may be an external network such as the Internet, or an internal network such as an Ethernet or a virtual private network (VPN).
[0017] A hard drive interface 132 is also coupled to system bus 106 . Hard drive interface 132 interfaces with a hard drive 134 . In one embodiment, hard drive 134 populates a system memory 136 , which is also coupled to system bus 106 . System memory is defined as a lowest level of volatile memory in computer 102 . This volatile memory includes additional higher levels of volatile memory (not shown), including, but not limited to, cache memory, registers and buffers. Data that populates system memory 136 includes computer 102 's operating system (OS) 138 and application programs 144 .
[0018] OS 138 includes a shell 140 , for providing transparent user access to resources such as application programs 144 . Generally, shell 140 is a program that provides an interpreter and an interface between the user and the operating system. More specifically, shell 140 executes commands that are entered into a command line user interface or from a file. Thus, shell 140 , also called a command processor, is generally the highest level of the operating system software hierarchy and serves as a command interpreter. The shell provides a system prompt, interprets commands entered by keyboard, mouse, or other user input media, and sends the interpreted command(s) to the appropriate lower levels of the operating system (e.g., a kernel 142 ) for processing. Note that while shell 140 is a text-based, line-oriented user interface, the present invention will equally well support other user interface modes, such as graphical, voice, gestural, etc.
[0019] As depicted, OS 138 also includes kernel 142 , which includes lower levels of functionality for OS 138 , including providing essential services required by other parts of OS 138 and application programs 144 , including memory management, process and task management, disk management, and mouse and keyboard management.
[0020] Application programs 144 include a renderer, shown in exemplary manner as a browser 146 . Browser 146 includes program modules and instructions enabling a world wide web (WWW) client (i.e., computer 102 ) to send and receive network messages to the Internet using hypertext transfer protocol (HTTP) messaging, thus enabling communication with software deploying server 150 and other computer systems.
[0021] Application programs 144 in computer 102 's system memory (as well as software deploying server 150 's system memory) also include a portal 148 . Portal 148 includes code for implementing the processes described below, including those described in FIGS. 2-3 . In one embodiment, computer 102 is able to download portal 148 from software deploying server 150 , including in an on-demand basis, wherein the code in portal 148 is not downloaded until needed for execution to define and/or implement the invention described herein. In other embodiments, the portal is a web based application that is accessed from a client computer over a network using a web browser. Note further that, in one embodiment of the present invention, software deploying server 150 performs all of the functions associated with the present invention, thus freeing computer 102 from having to use its own internal computing resources to execute portal 148 .
[0022] The hardware elements depicted in computer 102 are not intended to be exhaustive, but rather are representative to highlight essential components required by the present invention. For instance, computer 102 may include alternate memory storage devices such as magnetic cassettes, digital versatile disks (DVDs), Bernoulli cartridges, and the like. These and other variations are intended to be within the spirit and scope of the present invention.
[0023] In FIG. 2 a , there is shown a block diagram depicting the progression of steps 210 - 222 performed during a challenge event.
[0024] In step 210 a detailed description of a challenge event is posted on a portal. A challenge event is also referred to as a component herein, and the detailed description is also referred to as a specification herein. The specification may include use of certain reusable code assets from a catalog posted on the portal. The specification also includes the results of a pricing calculator described below from an event manager server.
[0025] In step 212 , participants (also referred to herein as vendor players) propose their respective solutions and terms such as cost, schedule, or approaches to provide a design or code their solution or provide another outcome based on the selected event. Participants may accept the price in the specification or propose a higher or lower price. Other terms from the specification may also be changed in their proposal. A single participant is then chosen for each challenge event using a selector subsystem (not shown). An important consideration in making the selection is each potential participant's digital reputation. In every previous event, participants are evaluated on reliability, i.e., did they submit and submit on time? They are scored on adherence to specifications using a standard scorecard with a 0-100 rating scale. Additional elements are also scored, including frequency of reuse from the catalog, the type of events the participant is working on, and how recent their event history is. All of these elements become part of the participant's digital reputation which is continuously maintained, updated, and available for use by the selector subsystem. Reliability of both submissions and wins may be displayed by month as a time line graph in a digital reputation display. The digital reputation of participants may be stored in a database accessible by the challenge server layer. After producing the work, the chosen single participant then delivers his solution in step 214 .
[0026] In step 216 , a challenge server layer in communication with the portal, evaluates submitted computer code. For example, a static analysis of submitted computer code may be performed. The code is validated for quality and evaluated using objective criteria, such as a published scorecard. If fixes are required, the participant applies the fixes in step 218 . This process can iterate. Once the outcome (the submitted design or code) meets the specification and is validated for quality, it is accepted and is delivered to the client who originally requested the coding event.
[0027] In step 220 , compensation is distributed to the participant. The submitted code is added to the catalog of reusable assets. Compensation may be a payment in actual dollars (green dollars), a credit of billable hour, digital reputation credit, or any other type of compensation known in the art and agreed to by the participant at the time the participant is chosen for the challenge coding. The client is then billed for the challenge event in step 222 .
[0028] In FIG. 2 b , the steps of a competition event are shown. In step 250 , a detailed description (specification) of a competition event (component) is posted to the same portal used for challenge events as described above. The results from the same pricing calculator described above are included in the competition event specification.
[0029] In step 252 , approved participants (company staff) register to provide their solutions to the specification. Some or all of the approved participants may be the same individuals who participant in challenge event as described above. Other limitations may be placed on who may be participants, for example, participant may be limited to employees of a particular company or employees who are temporarily unassigned to other projects. The approved participants deliver their solutions according to a time schedule in the specification, in step 254 .
[0030] In step 256 , each of the submitted code solutions for a competition is evaluated by performing a static analysis of the submitted computer code. The quality is validated and each solution is scored using a published scorecard. A single best solution is selected as the winner of the competition. A second place winner may also be selected. Other winners may also be selected according to the competition event description.
[0031] If fixes are needed they are applied in step 258 and the winning software design or computer code is delivered to the client who requested the competition be held.
[0032] Compensation is distributed in step 260 . If more than one winner is selected, then more than one participant my receive compensation. As above, the compensation may be in the form of green dollars, billable hours credit, or any other form of compensation. The first place wining solution is added to the catalog of reusable assets.
[0033] In step 262 , the client is billed for the outcome (first place winning software design or computer code).
[0034] In FIG. 3 , there is shown a system block diagram of the present invention. An engagement team 301 operates the system on behalf of one or more clients. The system includes an event manager server for creating the events. The engagement team uses block 303 to forecast demand for events and manage capacity by sourcing and supplying staff 304 for managing events. This may include procuring channel partners, as well as registering participants from suppliers 302 , for both challenge events and competition events in block 324 . Outcomes are delivered to clients by engagement team 301 from block 318 .
[0035] Rules for event specifications are developed and event staff trained using blocks 305 and 306 respectively.
[0036] A catalog of reusable assets is structured in block 307 . After each event, the delivered solution is added to the catalog in block 308 . Other code assets may be added in block 309 .
[0037] A project comprising one or more events is registered by block 310 . The event includes the results of pricing calculator 311 described below. The requirements in the specification of an event are validated in block 312 . However, block 312 may be bypassed by an event leader who is certified to operate events without assistance.
[0038] An event proceeds by dispatching a work request in block 313 and is executed in block 314 by event manager 323 . In block 315 , solutions are executed, evaluated for quality, and scored.
[0039] Selector subsystem 316 selects a winner for competition events. Final accounting, including compensating the participants(s) and billing the client, is preformed in block 317 . The solution is delivered to the client using block 318 by engagement team 301 .
[0040] The performance of the entire system is continually improved by gathering market intelligence in block 319 and by monitoring event performance in block 320 . Additional event types may be developed in block 321 . The event platforms, including the portal, the pricing calculator, and catalog, are managed in block 322 . In block 324 , overall performance of the system is analyzed and optimized.
[0041] In block 325 , the community of participants is promoted. In block 326 , the reputation of the participants is managed and its various compensation methods reviewed for improvement.
[0042] Pricing calculator 311 is an integrated capability of the event manager server that allows the client or event sponsor to enter characteristics about the event, such as the number of components, use case scenarios, or screens, and receive recommendations for sizing the event based on analytics captured from previous events. Pricing calculator 311 provides a total price for running the event based on size and components from reusable asset catalog 309 . Correctly sizing an event is very important to getting participants to register to work on the event.
[0043] As noted above, blocks 303 and 304 are important elements and are important features in managing events. A recommendation engine in the portal uses business analytics techniques to manage supply and demand, and to make recommendations for current and future events. Some of the data elements which may be captured by the recommendation engine include:
event type and technology platform event duration event value in points, hours, and dollars assets specified number of business rules, use cases, classes, or objects in event specification event registrants and digital reputations submission scores assets reused by participants scores of delivered solutions
The recommendation engine uses this prehensive outcome level data with business analytics techniques to provide:
recommendations of participants who would be expected to perform well in an event recommendations for participants of events that they should consider registering for recommendations for participants of assets that may help them deliver an outcome more efficiently success prediction of likelihood of a successful outcome based on event parameters identifying changes to skills or resources 304 needed to meet forecasted demand for outcomes alerts for troubled events
Various business analytics techniques known in the art may be used such as, but not limited to, computer algorithms in which the parameters are continuously adjusted based on current outcomes, or static models developed from historical data.
[0059] The present invention is also used to produce other types of outcomes to support the software development and support lifecycle. These other outcomes are required elements on projects where software code and design is being produced, and therefore, the computer system (portal application) supports the delivery of these additional accessory outcome types in order to assemble a working software system. The portal application allows for a selection on event type, with multiple choices for the different types of software project outcomes represented. The portal allows for outcomes to be requested in the areas of test case creation, test case execution, system architecture deliverables, graphic designs, software component assembly, and idea generation. The scoring method for these types of outcomes is consistent with coding and design events, but the scorecard used and the evaluation criteria are specific to the type of outcome.
[0060] While there have been shown and described what are at present considered the preferred embodiments of the invention, it will be obvious to those skilled in the art that various changes and modifications may be made therein without departing from the scope of the invention as defined by the appended claims. For example, it will be obvious that some steps shown sequentially may be performed in parallel. | A method and system for managing a challenge event from which a computer code that supports software development for a client computer is obtained. At least two participants are selected to participate in the challenge. Assets of software code are provided to the participants for assisting the participants to deliver respective submissions as outcomes of participation by the participants in the challenge event. A solution to the challenge event in a form of a computer code is received from only one participant previously chosen from the selected at least two participants as the only participant to submit the solution. The received solution is validated for quality and is accepted. In response to the validating and accepting of the received solution, the received solution is delivered to the client computer. The received solution is configured to be used by the client computer to support software development for the client computer. | 0 |
BACKGROUND OF THE INVENTION
The present invention pertains to periodic pulse generation and more particularly to the generation of frequency stable, low noise periodic pulse generation.
Deriving very accurate timing signals (clock signals) is important to many electronic systems. It is becoming common to utilize the highly accurate timing data from Global Positioning System Satellites as a source of accurate time and frequency. Other highly accurate clocks have been designed using Rubidium or Cesium clocks as the reference clock. Such designs are highly accurate, but are also very expensive and have complex designs.
Typical pulse generation apparatus provide a local oscillator and count-down circuit. The accuracy of such generation apparatus is generally a function of the stability of the reference clock frequency. This means that the timing output pulse of such systems displays jitter due to the inability of the count-down circuit to resolve the output frequency to less than one integer clock cycle.
Accordingly, it would be desirable to have a periodic pulse generation apparatus for providing a low-cost, highly accurate clock output signal which is frequency stable and has little jitter or no added noise due to the implementation.
BRIEF DESCRIPTION OF THE DRAWINGS
The single sheet of drawings presented herewith dipicts a pulse generation apparatus in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The single sheet of drawings depicts an accurate pulse producing circuit, which is based on controlling the local oscillator frequency of a Global Positioning System (GPS) receiver as a fine adjustment control, and steering of a pulse to the resolution of the main system clock as a coarse pulse control. Control processor 10 is coupled to programmable counter 15. Programmable counter 15 produces the desired one pulse per second output. A one kilohertz signal derived by integer division of the local oscillator 25 is transmitted from receiver time base 30 to programmable counter 15 and to control processor 10. Control processor 10 is also coupled to RF down converter and digital GPS correlator 35. Control processor 10 is coupled to digital-to-analog converter 20. Control processor 10 provides a Local Oscillator (LO) fine frequency control word to digital-to-analog converter 20. Digital-to-analog converter 20 is coupled to voltage controlled crystal oscillator 25. Voltage controlled crystal oscillator 25 provides the function of a local oscillator, required for any receiver. The output of voltage controlled crystal oscillator 25 is the "flo" lead which couples programmable counter 15, receiver time base 30 and RF down converter 35 to the voltage controlled crystal oscillator 25.
It is desired that an accurate signal on the one pulse per second lead be provided which is a useful output of a low cost global positioning system receiver.
An approximate one pulse per second signal is generated by programmable counter 15 as a result of dividing the flo output of vcxo 25. The error in the one pulse per second output randomly falls in time within -1/flo and +1/flo, provided that the control processor 10 provides programmable counter 15 with the correct count each second so as to place the resulting output pulse on or near the UTC second tic. Control processor 10 measures the error and computes the count for the programmable counter 15. The control processor uses the clock bias and clock bias rate outputs of the GPS receiver navigation solution 35 to compute corrections which are input to digital-to-analog converter 20 and programmable counter 15. As a result of the continual adjusting of the D/A converter 20 and programmable counter 15 by the control processor 10, digital-to-analog converter 20 steers the output flo of vcxo 25 to an integer frequency. Programmable counter 15 then outputs a one pulse per second signal at the same time every second, which is consistent with the UTC one second tic. The programmable counter 15 acts as a course time adjustment of the output pulse and the voltage controlled oscillator & D/A converter acts as a fine adjustment on the output pulse. The coarse adjustment process allows for simplification of the D/A converter as the dynamic tuning range required is greatly reduced since the oscillator only needs to be adjusted in frequency to the next closest integer frequency. Once that is accomplished, the integer programmable counter can then subsequently divide the local oscillator frequency by an integer and place the output pulse at the same point in time each second, which results in an output pulse in which the short term frequency stability is that of the local oscillator itself with little added noise and time jitter.
Low cost GPS receivers of today generate 1 PPS pulses by integer division via a programmable counter only of the receiver local oscillator. In the Motorola Oncore case, the oscillator frequency is flo=19.096 MHz. The uncertainty of the local oscillator is about ±2PPM, thus it will vary over temperature between 19.096 MHz-38 Hz and 19.096 MHz+38 Hz. The oscillator in prior implementations is free running, thus after integer division by a programmable counter, there is a residual time error in the resulting 1 PPS output that is at most 1/2 of 1 clock cycle of the local oscillator frequency, that is; the time error falls between -1/2 flo seconds to +1/2 flo seconds in time and the error waveform is a function of the local oscillator frequency. In this new embodiment, the local oscillator frequency is steered to an integer frequency such that when divided by the programmable counter (which by nature is an integer process), the resulting 1 PPS output pulse falls precisely on top of the UTC second tic with no residual time error.
It is well known that in addition to position coordinates of latitude, longitude, height, every GPS receiver has the ability to compute its internal measurement epoch time (i.e., the precise time of the range measurements within the receiver), and the frequency of the internal local oscillator. The time and frequency outputs are a direct result of the navigation solution of 4 (or more) equations and 4 unknowns for each of the processes of computing position and velocity. The GPS receiver solves for these quantities as a direct result of computing the clock bias and clock bias rates from the standard GPS navigation solution.
Each second, the GPS receiver computes in processor 10 the measurement epoch time and the local oscillator frequency. Call these:
Tme -- gps: The computed measurement epoch time.
Fos -- gps: The computed local oscillator frequency.
After computation of these quantities, the new embodiment uses processor 10 to make appropriate control adjustments via the D/A (digital-to-analog) converter 20 so that the frequency of the local oscillator is an integer. The three step algorithm to do so is as follows:
STEP 1: LO FREQUENCY ADJUSTMENT TO INTEGER FREQUENCY
a) Compute Fos -- gps using the traditional GPS navigation algorithms.
b) Compute frequency error fe as follows:
fe=INT(Fos.sub.-- gps+0.5)-Fos.sub.-- gps;
c) Filter the parameter fe via a 1st or 2nd order low pass loop filter, call this process LPF1(fe);
d) Integrate the output of the low pass filter to be used as an input to the D/A converter as follows:
DA.sub.-- word=DA.sub.-- word+K1* LPF1(fe);
where DA -- word is initially set to mid-range of the D/A converter input and K1 is the appropriate scale factor so that the resulting sum integrated into DA -- word is in units of LO -- Hz per fe -- Hz after the D/A converter transfer function. Step 1 forms an automatic frequency control loop which drives the LO frequency to the closest integer frequency.
e) Send the current value of DA -- word to the D/A converter, which will adjust the frequency of the local oscillator up or down slightly depending on the correction this second.
In a preferred embodiment, this processing may be accomplished in software via control processor 10.
STEP 2: COMPUTATION OF PROGRAMMABLE COUNTER CONTROL
Next, begins the process of computing the controls for the programmable counter 15. The steps accomplished by control processor 10 are:
a) Compute the time difference dt between the measurement epoch time and the next 1 PPS UTC second, as follows:
dt=INT(Tme.sub.-- gps+1)-Tme.sub.-- gps;
b) Compute the number of LO clock cycles in this dt time measurement as:
clks=Flo.sub.-- gps* dt;
c) Compute the number of integer counts to be applied by the programmable integer counter so as to place the 1 PPS output pulse to within ±1/2 of 1 LO clock as:
int.sub.-- clks=INT(clks+0.5);
Apply a correction to the programmable counter so that it will put out its pulse after counting "int -- clks" counts of the receiver local oscillator.
STEP 3: ELLIMINATION OF RESIDUAL TIME ERROR (if any)
The last step requires the computation of the residual time error in the 1 PPS output pulse, and mild control on the local oscillator frequency in order to elliminate it. The steps required are:
a) From step 2 part b, compute the fractional part of the number of clocks that are required to place the pulse closest to the 1 second tic as follows:
frac.sub.-- clks=clks-int.sub.--count;
b) Low pass filter the quantity "frac -- clks" with a 1st order low pass filter that has a time constant that is greater than that used in STEP 1, call this LPF2(frac -- clks);
c) Add a correction term to the D/A converter that is proportional to the output of the LPF2 filter, as follows:
DA.sub.-- word=DA.sub.-- word+K2* LPF2(frac.sub.-- clks);
d) Send the current value of DA -- word to the D/A converter, which will adjust the frequency of the local oscillator up or down slightly depending on the correction this second.
Step 3 acts as a phase locked loop which automatically adjusts the LO frequency so as to elliminate any phase error in the resulting 1 PPS output signal.
Since the bandwidths of the two processes in STEP 1 and STEP 3 are different, they will work together to set the LO on an integer frequency AND elliminate any subsequent time residual in the output 1 PPS signal.
This invention produces a 1 PPS signal whose phase and frequency error performance is superior to that mechanized by other low cost GPS receivers. The combination of mild local oscillator frequency steering (to the nearest integer frequency) and appropriate control loop software to control the phase and frequency of the resulting signal provide a highly stable output signal and low cost system implementation.
This invention recognizes that by steering the local oscillator to one of many possible integer frequencies by addition of a D to A converter, changing the design of the crystal oscillator to a VCXO, and adding sufficient control software to steer the LO frequency to one of many integer frequencies, the system can be controlled so that the 1 PPS pulse does not have added sawtooth noise. It also recognizes that there are many integer LO frequencies that are appropriate and voltage steering need only be such that it be able to steer to the closest integer frequency.
It is also recognized that steerage of the LO to the closest integer frequency greatly simplifies the D/A control circuit since the dynamic range of this element need only be such that it has the ability to move the LO ±0.5 Hz maximum instead of over the entire range of unknown frequency range, say ±2 PPM or more on a typical local oscillator used in GPS receivers today.
Until now, to achieve an accurate 1 PPS pulse, a system needed to have a high clock frequency as a basis for division into fine resolution time slices. With this system, high accuracy can be achieved using a low system clock frequency, allowing for lower component and overall system cost and lower power consumption.
Although the preferred embodiment of the invention has been illustrated, and that form described in detail, it will be readily apparent to those skilled in the art that various modifications may be made therein without departing from the spirit of the invention or from the scope of the appended claims. | A periodic pulse generator has a programmable counter (15) and processor (10) coupled to a GPS receiver for generating a periodic clock signal. The processor (10) transmits a control word to a digital to analog converter (20) which steers a voltage controlled crystal oscillator (25), processor 10 also controls the programmable counter (15) to produce a stable output pulse, if the voltage controlled crystal osciallator (25) output is an integer frequency. | 6 |
TECHNICAL FIELD
The present invention relates to systems and methods for controlling the operation of automotive air conditioning compressors, especially variable displacement compressors which may be regulated for optimal operation for a particular engine operating state and environmental condition.
BACKGROUND
Electronically controlled automotive air conditioning compressors are well known in the prior art. Typically, prior art electronically controlled compressor systems include an electronic control module in communication with various sensors for measuring vehicle interior and exterior environmental conditions, switches for actuating various air conditioning system modes, output ports for relaying output signals to actuate various system components, such as vent doors, blower motor, fans, and valves.
These electronically controlled compressors require a control strategy to optimize system operation. Without a control strategy capable of optimizing the performance of the air conditioning system, there is little justification for electronically controlling the compressor as compared to mechanically controlling the compressor. Generally, electronically controlled compressor systems weigh more, are more expensive, and require more sensors than their mechanical counterpart.
However, with optimum control of the electronically controlled compressor systems, the inefficiencies of mechanically controlled compressors, that are operated at lower evaporator temperatures than otherwise required (typically around 35 F) may be avoided. Such air conditioning systems having mechanically controlled compressors, thus do more work than is required in the vast majority of operating conditions.
Therefore, what is needed is a new and improved method for controlling electronically controlled automotive air conditioning compressors. The new and improved method must not run the compressor unnecessarily. Moreover, it must not create a passenger compartment environment that is prone to fogging or is too humid.
SUMMARY
A method for controlling a vehicle air-conditioning system for cooling an interior of a vehicle is provided. In an aspect of the present invention the vehicle air conditioning system has a compressor coupled to an electronic control valve. In another aspect of the present invention, the method includes reading a user manipulatable switch, determining a desired vehicle interior temperature based on the read user manipulatable switch, reading a plurality of sensors indicative of an interior and an exterior climate of the vehicle, determining a heat load on the vehicle air conditioning system, determining a desired evaporator discharge temperature, evaluating a humidity level inside the vehicle by determining a humidity ratio, filtering the updated electronic control valve duty cycle to obtain a new electronic control valve duty cycle based on the desired evaporator discharge temperature, and sending the new electronic control valve duty cycle to a compressor controller, wherein the controller is in communication with the electronic control valve and commands the valve to operate at the new duty cycle.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a schematic diagram of an air conditioning system for an automobile having a variable displacement compressor, in accordance with the present invention;
FIG. 2 is a schematic diagram of a variable displacement compressor that is selectively driven by the engine, in accordance with the present invention; and
FIGS. 3-5 are a flowcharts illustrating a method for controlling the variable displacement compressor, in accordance with the present invention.
DETAILED DESCRIPTION
Referring now to FIG. 1 an automotive air conditioning or climate control system 10 is schematically represented, in accordance with the present invention. System 10 includes an air conditioning duct which defines an air passage 14 for directing conditioned air into a passenger compartment.
Air conditioning duct 12 includes a plurality of inlets and outlets for drawing in outside air and for directing conditioned air into the passenger compartment. For example, the inlets include an outdoor air inlet 16 for drawing in outside air, and an inside air recirculation inlet 18 for recirculating air contained within the passenger compartment. A mode selector door 20 driven by a small motor 22 is provided to allow a passenger to select between an outside intake mode and an inside air recirculation mode.
Further, a blower 24 such as a centrifugal blower is provided within air conditioning duct 12 for producing air flow from the air inlets to the air outlets. Blower 24 further includes a centrifugal fan 26 and a motor 28 . Motor 28 is controlled by a motor driver circuit 30 .
Air conditioning duct 12 further includes a plurality of air outlets for directing air conditioned air to various parts of the passenger compartment. More specifically, a defroster outlet 32 is provided for directing conditioned air to a vehicle windshield 34 . A defroster mode is selected by actuating a defroster door 36 . Further, an upper body air outlet 40 is provided for directing conditioned air toward a vehicle occupant's upper body. An upper body selection mode is selected by actuating an upper body air mode door 42 . Similarly, a foot air outlet 44 is provided for directing conditioned air towards the feet of vehicle occupants. Preferably, a foot air mode door 46 is provided for selecting a foot air mode.
With continuing reference to FIG. 1, a heater unit 50 having a heater core is provided for heating cold air passing by an evaporator unit 52 . Typically, the heater core is supplied with heated cooling water from the engine 11 . During the heating cycle of the air conditioning system, the heater unit 50 acts as a heat exchanger using the heater cooling water to heat the cold air passing through the evaporator 52 . An air regulator door 54 is provided for regulating the amount of air heated by the heater unit 50 .
Evaporator 52 is in fluid communication with a compressor 60 . Compressor 60 is preferably a variable displacement compressor, or a fixed displacement compressor or a mechanically controlled compressor, that draws in refrigerant, compresses the refrigerant and discharges the refrigerant. Evaporator 52 is also in communication with an expansion valve 62 . Expansion valve 62 expands the liquid refrigerant fed from a receiver 64 . Receiver 64 performs vapor liquid separation of the refrigerant fed from a condenser 66 . Condenser 66 condenses and liquefies the refrigerant fed from compressor 60 through heat exchange with outdoor air. Condenser 66 is cooled by a cooling fan 68 which is driven by a driver motor 70 .
Compressor 60 further includes an electromagnetic clutch 72 that is in communication with a compressor drive pulley 76 for engaging and disengaging a drive belt 78 driven by engine 11 . However, in alternative embodiments of the present invention compressor 60 does not include an electromagnetic clutch and thus is in continuous engagement with engine 11 .
An air-conditioning system control unit 82 (ACU) is further provided for controlling the operation of the air conditioning system in accordance with the present invention. Air-conditioning control unit 82 includes a microprocessor 84 , read only memory (ROM) 86 , and random access memory (RAM) 88 and other conventional computer components. The ACU is supplied power by the vehicle battery 90 when the ignition switch 92 is switched on. A plurality of switches and sensors are in communication with ACU 82 for sending to the ACU electrical signals indicative of air conditioning environmental factors necessary for determining how to optimally air condition the passenger compartment. The sensors include, for example, an indoor air temperature sensor 94 for determining the temperature of the air inside the passenger compartment, an outdoor air temperature sensor 96 for determining the temperature of the outside air, a solar radiation sensor 98 for determining the intensity of the solar radiation incident on the passenger compartment, a post evaporator temperature sensor 100 detects the actual air cooling by the evaporator, a humidity sensor 102 for detecting a relative humidity of air inside the passenger compartment and a rotational speed sensor 104 for detecting rotational speed of engine 11 .
The switches for manual control of the air conditioning system 10 include, for example, a temperature setting switch 106 for setting a desired indoor air temperature to a desired temperature level, an indoor/outdoor air selector switch 108 for selecting outdoor air intake mode or indoor air recirculation mode, an air conditioning on/off switch 110 for turning on and off the air conditioning system, and an automatic mode switch 112 for selecting automatic air conditioning operation. Further, control unit 82 has a plurality of output ports 114 for sending control signals to the various air conditioning system components. For example, control signals are sent to the various vent doors, fan motors, and the variable displacement compressor 60 .
Referring now to FIG. 2, a schematic diagram of variable displacement compressor 60 is shown in greater detail, in accordance with the present invention. Compressor 60 includes a driveshaft 140 that is operatively coupled to an external drive source such as vehicle engine 18 by electromagnetic clutch 72 and to electric motor 20 . A swashplate 142 is rotatably secured to shaft 140 and is pivotable about the driveshaft. A pair of guide arms 161 and 162 are attached to swashplate 142 at a first end and to pistons 150 and 151 at a second end. The engagement between guide arms 161 , 162 and the associated pistons guides the inclination of the swashplate 142 and rotates the swashplate with respect to the driveshaft 140 . Driveshaft 140 and swashplate 142 are positioned within a crankcase chamber 147 . The pressure in crankcase chamber 147 controls the angle of inclination of the swashplate.
Generally, compressor 60 further includes a cylinder housing 148 having cylindrical bores 144 and 145 extending therethrough. Each bore 144 and 145 accommodates one piston 150 , 151 . Each piston and bore define compression chambers 153 , 155 . Alternatively, each piston may be coupled to the swashplate by a pair of shoes (not shown). Rotation of the swashplate is converted into reciprocation of pistons 150 , 151 in bores 144 , 145 by means of the shoes, as well known in the art.
Further, compressor 60 includes a rear housing 170 having a suction chamber 172 and 173 and a discharge chamber 174 . Suction ports 176 and 177 and discharge ports 178 and 179 are also provided at each chamber. A suction valve (not shown) is provided at each suction port for opening and closing the suction port. A discharge valve (not shown) is provided at each discharge port for opening and closing the discharge port. Further, a bypass port or orifice 175 is provided between crankcase chamber 147 and suction chamber 172 .
As each piston 150 , 151 moves from a fully extended position to a fully retracted position refrigerant is drawn into the corresponding suction port from the suction chamber to enter the associated compression chamber. Conversely, when each piston moves from a fully retracted position to a fully extended position, the refrigerant is compressed in compression chambers 153 , 155 and the discharge valve opens allowing refrigerant to flow into discharge chamber 174 through associated discharge ports 178 , 179 . The inclination of swashplate 148 varies in accordance with the difference between the pressure in crankcase chamber 147 and the pressure in compression chambers 153 , 155 . More specifically, the difference between the pressure in crankcase chamber 147 (PC) and the pressure in the suction chambers 172 , 173 (PS) or the pressure difference “PC−PS” determines the inclination of the swashplate. PC is maintained at a pressure value that is higher than the suction pressure PS (PC>PS). An increase in the pressure difference PC−PS decreases the inclination of the swashplate. This shortens the stroke of each piston 150 , 151 and decreases the displacement of compressor 60 . On the other hand, a decrease in pressure difference PC−PS increases the inclination of swashplate 142 . This lengthens the stroke of each piston 150 , 151 and increases the displacement of compressor 60 .
In FIG. 2 swashplate 142 is indicated by solid-lines (a) in a first position (position a). When the swashplate is in position (a) the pistons 150 , 151 do not reciprocate within chambers 153 , 155 . Compressor 60 is at its minimum displacement. As indicated by dashed-lines (b) the swashplate may be disposed in a second position (position b). Position (b) illustrates the maximum angle of inclination the swashplate can achieve. This is also the position in which compressor 60 achieves its maximum displacement. Depending on the pressures in crankcase chamber 147 , suction chamber 172 and discharge chamber 174 the swashplate may be inclined at any angle between position (a) and (b) achieving variable displacement.
An electronic control valve 200 is in communication with the discharge chamber 174 , through a refrigerant/oil separator 202 , and with the crankcase chamber. Electronic control valve 200 regulates the pressure in crankcase chamber 147 , suction chamber 172 and discharge chamber 174 , by selectively opening and closing communication ports connecting the crankcase chamber to the discharge chamber. A control strategy for actuating valve 200 will be described hereinafter.
The electromagnetic control valve 200 serves to regulate the discharge capacity of compressor 60 by changing a set level of suction pressure of the compressor according to a control current supplied by the air conditioning electronic control unit 82 .
In a preferred embodiment of the present invention a control strategy for controlling the operation of electromagnetic control valve 200 is implemented in software, or in hardware or in both software and hardware. For example, control logic for controlling the operation of control valve 200 in one embodiment is stored in the ACU's read only memory 86 .
Referring now to FIG. 3, a variable compressor and valve control strategy 201 is illustrated in flow chart form, in accordance with the present invention. The initial step of the control strategy is to determine the load acting on the AC system. The thermal load is determined by analyzing four elements (1) the fresh air and body leakage air intake load, (2) the convection and conduction losses through the body of the car, (3) the solar gain load through the car, and (4) the thermal inertia which must be overcome to bring the interior temperature of the car down to a desired level. The fresh air and body leakage load is calculated as a function of blower speed, the blend door position, the recirculation door position, and the interior and exterior temperatures. The blower speed and flow rate determines how much of the fresh air is being injected into the vehicle. This control strategy is based on the assumption that if the blower is in recirculation mode, then 20% of the flow is outside air and 80% of the flow is inside air. If the mode doors are set for floor/defrost or defrost, then this strategy assumes that the AC system is set in fresh air mode. The fresh air and body leakage load may be described by the following equation:
{dot over (Q)} fresh ={dot over (m)} blower ·K door ·C air ·( T amb −T set )
where:
K door =0.8 fresh
{dot over (m)}=mass flow rate of blower
T amb =ambient air temperature
T set =set temperature
The body conductivity losses should be based on actual or simulated test data recorded at 110 F. Body leakage is a function of the inside and outside air temperature difference and the thermal insulation characteristics of the vehicle.
The convection losses through the body of the vehicle are determined first by conducting thermal testing of the vehicle in question to determine the heat absorption rate at a given temperature. Using this data a convection constant (K con ) is determined, and the following equation describes the convection load:
{dot over (Q)} con =K con ·( T amb −T set )
where: K con = 0.012 + S veh · 1.0 110 - 70 - 0.75 110 - 70 96 - 48
S veh =Speed of Vehicle (km/hr)
The sun load is a function of the measurements from a sun load sensor and also particular characteristics of a given vehicle. Again, vehicle testing would be required to determine the amount of energy a vehicle absorbs under full sun load. The sun load may be described by the following equation:
{dot over (Q)}
sun
=K
sun
·T
sun
where:
K sun =0.67 m 2
1 kWm −2 ≧T sun ≧0 kWm −2
The remaining load determines the thermal inertia load. This load is a function of the interior temperature and the vehicle occupant's desired interior temperature. Desired interior temperature is determined by reading control switches and buttons, as represented by block 202 . In an embodiment of the present invention, the compressor is operated at a maximum capacity until the desired temperature is reached. Preferably, the load is based on the difference between the current interior temperature and the desired temperature. This allows the two temperatures to converge asymptotically and thus avoid overshoot. An acceleration timer can be used to increase the speed of convergence. The thermal inertia load may be described by the following equation:
{dot over (Q)} inertia =K acc ·{dot over (m)} blower ·C air ·( T int −T set )
Thus, the total load is calculated by summing the above loads as described by the following equation:
{dot over (Q)}
tol
={dot over (Q)}
fresh
+{dot over (Q)}
con
+{dot over (Q)}
sun
+{dot over (Q)}
inertia
At block 204 , the various system sensors described above are read. Three conditions are checked at blocks 206 , 208 and 210 . All of these conditions must be met to continue strategy 201 . The first condition, represented by block 206 is to determine whether the ambient outside air temperature is greater than a predefined minimum temperature, and whether the vehicle ignition is “on”. If the ambient air temperature is greater than the predefined temperature and the ignition is “on”, the next condition is checked, at block 208 . However, if the ambient temperature is not greater than the predefined minimum temperature and/or the ignition is “off”, then control valve 200 is not activated, as represented by block 212 . The next condition checked is whether climate control system 10 has been activated, as represented by block 208 . If the system is “on”, then the third condition is checked, as represented by block 210 . If system 10 is not “on”, then control valve 200 is not activated, as represented by block 212 . At block 210 , the strategy determines whether the electromagnetic clutch 72 is engaged. If the clutch is not engaged, then valve 200 is not activated, as represented by block 212 . However, if the clutch is engaged then the desired evaporator discharge air temperature is determined, as represented by block 214 and further in FIG. 4 .
In FIG. 4, a method 280 for determining the desired evaporator discharge air temperature (T et ) is illustrated, in accordance with the present invention. If climate control system 10 has been requested, the system sets the T et to the lower of the driver (T des1 ) or passenger (T des2 ) desired temperatures in a dual zone system, at block 290 . At block 300 , the system determines whether defrost or floor/defrost modes are selected. If defrost or floor/defrost modes are activated, then T et is set for maximum dehumidification. However, if defrost or floor/defrost modes are not activated, then the system determines if the temperature is set to maximum cooling mode, as represented by block 304 .
If the temperature is set to maximum cooling, then T et is set for maximum cooling, as represented by block 306 . However, if temperature is not set to maximum cooling, the system determines whether the temperature is set for maximum heating, as represented by block 308 . If the system determines that the temperature is set to maximum heating, then valve 200 is not activated and T et is set equal to T desired , where T desired is equal to the maximum system temperature (T max ), as represented by block 310 . However, if the temperature is not set to maximum heating, then the system sets T et to the greater of T et and the minimum temperature (T min ), as represented by block 316 .
The next step, as indicated by block 216 , is to evaluate the humidity level in the vehicle and determine what steps are necessary to prevent fogging. With reference to FIG. 5, a method 318 for evaluating the humidity level in the passenger compartment to prevent fogging is illustrated. This is accomplished by setting a target temperature for air passing through the evaporator and modulating the compressor accordingly to achieve the target temperature. Having calculated the load and knowing the air mass flow rate ({dot over (m)}) from previous calculations shown above, T desired and T et may be described by the following equation: T desired = T ei - Q . tot m . blower · C air
T et =T desired
T et =evaporator inlet temperature
As illustrated in this equation, the evaporator capacity is modulated based on the thermal loading on the system.
At block 320 the humidity level within the passenger compartment is measured by a humidity sensor. If the humidity level is too high, irrespective of the interior or exterior conditions, the air within the passenger compartment must be cooled to remove the humidity from the air. A target evaporator discharge temperature of approximately 55° F. is selected, which falls within the normal comfort level, as defined by ASHRAE. When the air is reheated, the air will fall into a comfortable region. In order to determine if the humidity is too high, a humidity ratio must be evaluated. The humidity ratio is evaluated by referring to table 1 below and by measuring the humidity, using the humidity sensor, and the temperature using the temperature sensor, as represented by blocks 320 and 322 . The humidity ratio is then evaluated, as represented by block 324 . Preferably, table 1 is stored in system memory. The humidity ratio is compared to a target humidity ratio such as approximately 0.009, as reprsented by block 326 . If at a given temperature the relative humidity is greater than the relative humidity shown in the table 1, then the humidity ration is determined to be greater than the target humidity ratio. The air must then be dehumidified, as represented by block 328 . Table 1 below shows the temperature versus humidity values for a humidity ratio of 0.009 kg water/kg air.
TABLE 1
Temperature Vs. Relative Humidity at 0.009 Humidity Ratio
Temperature
Relative Humidity
54
100
57
90
60
80
64
70
69
60
74
50
81
40
90
30
103
20
If the measured interior air has a humidity ratio above 0.009 kg water/kg air, then the air must be cooled to 55° F. This is due to the fact that the humidity ratio at 55° F. and 100% relative humidity is 0.009 kg water/kg air. The following control logic statement may be used in the control strategy to accomplish this objective:
IF((T et )55 F) and (HR)0.009))T et =55° F.
Finally, the control strategy determines if fogging is probable, as represented by 332 . If fogging is likely, the compressor will be operated to produce the lowest evaporator discharge temperature possible to remove or dilute the moisture in the air, as represented by blocks 332 and 334 . The following control logic statement may be used to accomplish this objective:
IF(Fogging Probability=High)T et =35° F.
Fogging occurs when the humidity in the vehicle is high enough that water condenses on the interior of the car. The strategy returns to the main program at block 336 .
Having decided upon the target evaporator outlet temperature, the strategy returns to FIG. 3 . The next step is to determine the output current for the compressor, as represented by block 218 . The control current/depends on current control setting for the compressor and the difference between the actual evaporator outlet temperature (T et ) and the real evaporator temperature (T evapout ). The following closed loop control logic may be used:
ΔT=T et −T evapout I l + 1 = I t + I max · K · Δ T 10
where.
I l+1 ≦I max
ΔT≦10
As any person skilled in the art of electronic control automotive air conditioning compressors will recognize from the previous detailed description and from the figures and claims, modifications and changes can be made to the preferred embodiments of the invention without departing from the scope of this invention defined in the following claims. | A method for controlling a vehicle air-conditioning system for cooling an interior of a vehicle is disclosed. The vehicle air conditioning system has a compressor coupled to an electronic control valve. The method includes reading a user manipulatable switch, determining a desired vehicle interior temperature based on the read user manipulatable switch, reading a plurality of sensors indicative of an interior and an exterior climate of the vehicle, determining a heat load on the vehicle air conditioning system, determining a desired evaporator discharge temperature, evaluating a humidity level inside the vehicle by determining a humidity ratio, filtering the updated electronic control valve duty cycle to obtain a new electronic control valve duty cycle based on the desired evaporator discharge temperature, and sending the new electronic control valve duty cycle to a compressor controller, wherein the controller is in communication with the electronic control valve and commands the valve to operate at the new duty cycle. | 5 |
BACKGROUND OF THE INVENTION
The field of the present invention is apparatus and technique for installing casing in a well.
In oil well drilling operations, a plurality of tasks must be performed in completing a well beyond drilling the well bore. Well casing extending upwardly from the production zone is to be positioned and cemented. Where multiple production zones overlay one another, scab casings between each production zone are frequently cemented into place. Once the casing has been installed, slotted liners may be positioned in the production zones, frequently with gravel packing, cementing and sealing of such liners to the casing. Underreaming of the production zone areas may precede placement of the liners. Finally, appropriate mechanisms are placed in the hole for production.
Economical completion of a well is of great interest. One means to reduce the cost of well completion is to limit the number of trips required down the well. Each trip involves the placement and/or removal of tools and equipment. A pipe string thousands of feet long must be assembled and disassembled in the process of inserting tools and equipment. Consequently, it is advantageous to complete as many functions as possible with a single trip into the well bore.
Duplex cementing systems have been available for cementing sections of a well. Such systems are available for either liners or casings. The duplex tool is associated with either a guide shoe or a cementing basket depending on the position in the well. Duplex tools are most appropriately of aluminum to allow the blockage created by the tool to be drilled out for later placement of liners or equipment. The tool includes a port or ports for delivering a charge of cement to outwardly of a casing or liner to which the tool is fixed. These cementing ports can then be closed or blocked and other ports opened to establish circulation down the drill pipe, out the duplex tool and up the interior of the liner or casing. The valve portion of the equipment is then unthreaded from the aluminum shoe or collar and removed. The system has required one trip down the well for each section placed.
In the installation of liners in a well, multiple functions with a single trip into the well are known. Schemes for gravel packing wells and the like with a single placement of drilling tools has been used. Reference is made to U.S. Pat. Nos. 5,253,708 for PROCESS AND APPARATUS FOR PERFORMING GRAVEL-PACKED LINER COMPLETIONS IN UNCONSOLIDATED FORMATIONS; 5,255,741 for PROCESS AND APPARATUS FOR COMPLETING A WELL IN AN UNCONSOLIDATED FORMATION; 5,425,423 for WELL COMPLETION TOOL AND PROCESS; and 5,497,840 for WELL TOOL AND PROCESS OF COMPLETING A WELL, the disclosures of which are incorporated herein by reference.
SUMMARY OF THE INVENTION
The present invention is directed to the placement and cementing of casings accomplished with a single placement of equipment in the well.
In a first, separate aspect of the present invention, a valve assembly is configured to extend into the cavity of a duplex tool. An engagement pipe includes a threaded pin for association with one end of the valve assembly. A ratchet assembly is associated with the engagement pipe and the valve assembly to control the engagement between the two. In further association with this aspect, the ratchet may be spring biased from a position on the engagement pipe with stops provided on the valve assembly. The ratchet may also be cylindrical in configuration. The duplex tool may include a duplex shoe or a cementing basket.
In a second, separate aspect of the present invention, a duplex assembly includes a duplex tool with a valve assembly extendable into the cavity of the duplex tool. A lock assembly on the valve assembly provides selective engagement with the duplex tool for extraction without unthreading components. This aspect may further include association of a scab casing with the duplex tool. The duplex tool may again include a shoe or a cementing basket.
In a third, separate aspect of the present invention, a duplex assembly includes a duplex tool and a valve assembly extending into the cavity of the duplex tool. The duplex assembly provides a through passage. Valving systems provide for closure of the passage and direction of the flow outwardly of the associated casing for cementing and inwardly of the casing for flushing of the annulus.
The foregoing aspects may also be considered in combination with one another to form yet further, separate aspects of the invention. Additionally, multiples of the features of the foregoing aspects may be associated. Such association provides for the placement of multiple separate sections of casing in a well with a single insertion of equipment.
In a further, separate aspect of the present invention, the steps of positioning multiple liner segments in a well with subsequent cementing of the segments and flushing of the interiors are accomplished in sequential order. Release of the casing segments may be further applied to this aspect of the present invention.
Accordingly, it is an object of the present invention to provide improved systems for the placement of casing segments within a well. Other and further objects and advantages will appear hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a string assembly employing multiple duplex assemblies.
FIG. 2 is the string assembly of FIG. 1 with the bottom scab casing cemented.
FIG. 3 is the string assembly of FIG. 1 with the bottom scab casing and an upper scab casing cemented.
FIG. 4 is another string assembly similar to FIG. 1 but including a duplex system for cementing the surface casing with all casings cemented.
FIG. 5 is a compound assembly of duplex tools shown in partial cross section.
FIG. 6a is a cross section of a duplex assembly.
FIG. 6b is a cross section of the duplex assembly of FIG. 6a with a valve sleeve in the open position.
FIG. 6c is a cross section of the duplex assembly of FIGS. 6a and 6b with the locking sleeve in an unlocking position.
FIG. 7a is a cross section of a duplex assembly.
FIG. 7b is a cross section of the duplex assembly of FIG. 7a with a valve sleeve in the actuated position.
FIG. 7c is a cross section of the duplex assembly of FIG. 7a with a second valve sleeve in the actuated position.
FIG. 7d is a cross section of the duplex assembly of FIG. 7a with a locking sleeve in an unlocking position.
FIG. 8 is a partial cross-sectional view of an engagement pipe with a ratchet.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning in detail to the drawings, FIG. 1 illustrates a compound duplex assembly generally presenting the layout of one of the preferred embodiments. Drill pipe 10 is shown extending into a well bore 12. A lower duplex assembly, generally designated 14, is shown with attachment to the end of the pipe string. The assembly 14 includes a scab liner 16. This lower duplex assembly 14 is fitted with a duplex shoe 18. An upper duplex assembly, generally designated 20, includes attachments to drill pipe 10 both top and bottom. The upper duplex assembly 20 is fitted with a cementing basket 22. Multiple upper duplex assemblies 20 may be included within the duplex assembly. Each upper duplex assembly 20 is also fitted with a scab liner 24. FIG. 1 illustrates the compound duplex assembly as it is positioned within the hole. FIGS. 2, 3 and 4 illustrate progressive cementing steps as the cementing operation moves upwardly in the well bore 12. FIG. 4 additionally illustrates an upper duplex assembly 20 used with a surface casing 25. The system may be employed for all casings within a well as may be required.
Looking to the details of the lower duplex assembly 14 seen in FIG. 5, a cylindrical housing 26 provides a central core of the lower duplex tool, generally designated 27, and defines a central cavity 28 extending axially of the lower duplex assembly The housing 26 is externally threaded and locked with an annular ring 29. A threaded collar 30 is in turn positioned about the outside of the annular ring 29. The duplex shoe 18 is associated with the lower side of the threaded collar 30 while the scab casing 16 extends upwardly as seen in FIGS. 1 through 4, also from the threaded collar 30.
The duplex shoe 18 has a passage centrally therethrough aligned with the central cavity 28 and defined in part by an upper port 32 and a lower port 34. A ball check valve is within the passage. The ball check valve includes a ball 36 and a spring 38 biasing the ball 36 against a seat 40 at the upper port 32. Thus, the check valve only allows passage of fluid through the duplex shoe 18 in a downward direction against the operation of the spring 38. The duplex tool 27 is preferably made of a material which can be easily drilled out during subsequent operations. Aluminum is commonly employed for the several components with the exception of the threaded collar 30 and the scab casing 16 which are not to be drilled out.
A valve assembly, generally designated 42, extends into the central cavity 28 of the lower duplex tool 27. The valve assembly 42 includes a substantially cylindrical body 44 having a passage 46 therethrough. The passage 46 of the cylindrical body 44 is threaded through a portion of its upper length, defining an internally threaded end 48. This end 48 faces upwardly away from the duplex tool 27. Below the threads in the internally threaded end 48 is an annular cavity 50, best seen in FIGS. 6a through 6c. The cavity receives a seal 52, shown in FIG. 5 to be a lip seal. Stops 54 are defined by recesses cut partially into the body 44 about the outside of the upper rim of the internally threaded end 48, as best illustrated in FIG. 5.
Below the internally threaded end 48, the cylindrical body 44 includes radial ports 56 extending through the wall and spaced about the periphery. The radial ports 56 are shown to be above the cylindrical housing 26 as seen in the preferred embodiment. Below the radial ports 56, a shoulder 58 is found on the outside of the body 44. The shoulder 58 extends to a seat 60 on the upper end of the cylindrical housing 26. The shoulder 58 and seat 60 may each lie in a plane or may include interlocking tab portions so as to axially align the body 44 with the housing 26.
Tapered slots 62 extend radially through the wall of the body 44 at four equiangular positions below the shoulder 58. The cylindrical housing 26 includes corresponding recesses 64 in the wall of the housing 26 from the cylindrical cavity 28. Floating dogs 66 are arranged in the tapered slots 62 and corresponding recesses 64. The dogs 66 are also tapered so as to fit closely within the cavities thus formed.
A further set of radial ports 68 is arranged below the tapered slots 62 in the body 44 and also extends through the housing 26. These radial ports 68 and the radial ports 56 are spaced about and through the wall of the body 44 so that fluid flow may easily exit through these ports when open.
Internally of the body 44, a uniform bore is provided between an upper shoulder 70 and a lower shoulder 72. The lower shoulder 72 is defined by an inwardly extending flange 74 on an end piece 76 which is threaded to the main body portion of the cylindrical body 44. A set screw 78 retains the end piece 76 on the lower end of the cylindrical body 44. The uniform bore between the shoulders 70 and 72 on the inner surface of the body 44 provides for the placement and sliding of sleeve elements therein. On the outer surface of the cylindrical body 44 fitting within the cavity 27 of the cylindrical housing 26, a lip seal 80 and an O-ring 82 prevent flow between the components.
The duplex assembly 14 further includes a valve sleeve 84 as part of the valve assembly 42. The valve sleeve 84 closely slides within the uniform bore of the cylindrical body 44. O-rings 86 prevent flow between the valve sleeve 84 and the uniform bore of the cylindrical body 44. The valve sleeve 84 is originally positioned to cover the radial port 68. In that position, shear pins are placed to extend from the body 44 to the valve sleeve 84. A tapered shoulder 88 on the inner surface of the valve sleeve 84 provides a seat for a ball 90. When the ball 90 is positioned in the valve sleeve 84, the shear pins fail and the valve sleeve 84 assumes a second position displaced from the radial ports 68 and against the lower shoulder 72. The two positions of the valve sleeve 84 are illustrated in FIGS. 6a and 6b. Circulation is terminated through the end of the duplex tool 27 with the ball 90 in place. Access from the central passage to outwardly of the scab casing 16 is, therefore, cut off. Instead, the central passage is in communication through the ports 68 with the annulus, inwardly of the casing.
Positioned within the uniform bore of the body 44 is a locking sleeve 92. The locking sleeve 92 in cooperation with the dogs 66 define a lock assembly. The locking sleeve 92 includes O-rings 94 to prevent fluid flow between the sleeve 92 and the body 44. The sleeve 92 has an annular recess 96 through a portion of its axial length. Shear pins retain the locking sleeve 92 in its upper, initial position which is seen in FIGS. 6a and 6b. In this position, the radial ports 56 are covered and the floating dogs 66 are forced outwardly to extend through the tapered slots 62 into the corresponding recesses 64 in the cylindrical housing 26. Thus, the upper position of the locking sleeve 92 provides a locking between the duplex tool 27 and the valve assembly 42. The locking sleeve 92 is illustrated in the lower position in FIG. 6c. In that position, the recess 96 extends over the floating dogs 66, releasing them from the recesses 64 in the cylindrical housing 26. Additionally, the radial ports 56 are open. A second ball 98 cooperating with a tapered shoulder 100 on the inside of the locking sleeve 92 shears the locating pins and drives the locking sleeve 92 to its lower, final position as seen in FIG. 6c.
An engagement pipe 102 includes a threaded pin 104 at one end thereof as seen in FIG. 8. The threaded pin threadably engages the internally threaded end 48 of the cylindrical body 44 of the valve assembly. FIG. 8 illustrates the engagement pipe 102 while FIG. 5 shows the association between the engagement pipe 102 and the cylindrical body 44. A cylindrical ratchet 106 is arranged about the engagement pipe 102 adjacent to the threaded pin 104. The ratchet 106 is maintained in place by a pin 108 riding within a slot 110 on the cylindrical ratchet 106. The ratchet 106 includes teeth 112 at one end thereof. A spring 114 biases the cylindrical ratchet 106 toward the threaded pin 104.
With the engagement pipe 102 threaded into the internally threaded end 48, the teeth 112 of the ratchet 106 engage the stops 54 on the cylindrical body 44. Once engaged, the engagement pipe 102 cannot be disengaged from the cylindrical body 44 without axially displacing the ratchet 106 against the force of the spring 114. The engagement pipe 102 may be fixed to the valve assembly 42 without necessarily requiring the application of high torque to the connection to insure retention. The valve assembly is in turn locked to the duplex tool 27 by the lock assembly in order that the entire lower duplex assembly 14 may be suspended by the engagement pipe 102. Drill pipe 10 is in turn coupled with the engagement pipe 102 to support the lower duplex assembly 14.
The upper duplex assembly 20 is illustrated in association with the lower duplex assembly 14 in FIG. 5. Additionally, details of this device are presented in FIGS. 7a through 7d. The upper duplex assembly 20 has similar mechanisms to that of the lower duplex assembly 14. A cavity extends through a duplex housing, generally designated 116. In this case, the housing 116 is made of a first substantially cylindrical element 118 having a threaded pin 120 at one end and an integral internally threaded collar 122 at the other. The threaded pin 120 receives a collar 124 having a beveled lower entry 126 into the interior of the housing 116. The integral collar 122 receives the end of a scab casing 24 as seen in FIG. 1 which extends upwardly beyond this upper duplex assembly 20.
Associated with the outer element 118 is a cementing basket 22 only illustrated in FIGS. 7a and 7b. The cementing basket 22 includes a collar 128 held between a shoulder 130 and the lower collar 124. The cementing basket 22 further includes overlapping leaves 132 extending outwardly and upwardly from the collar as seen in FIG. 5. The leaves are able to open outwardly against the well bore and yet provide a solid barrier against cement flowing downwardly through the basket.
The housing 116 also includes an inner, annular element 134. This element includes an annular boss 136 having threads thereabout to engage mating threads on the inner side of the element 118. A gap is found between the elements 118 and 134 adjacent to the annular boss 136. This gap is .filled with cement 138. The annular element 134 extends upwardly from the annular boss 136 to form the substantially cylindrical body.
A valve assembly, generally designated 139, is positioned in the cavity of the inner, annular element 134. This valve assembly 139 includes a substantially cylindrical body 140. The body extends from a threaded pin 142 to an internally threaded end 144. An adapter element 146 includes a pin 148 to threadably attach to the end 144. It also includes an internally threaded upper end 150 having stops 152 about the outer periphery in the same configuration as the stops 54 associated with the cylindrical body 44. An annular cavity 154 is arranged to receive a lip seal 155 for sealing between the components.
The body 140 includes a first substantially uniform bore extending between the bottom of the pin 148 and an inwardly extending shoulder 156. Within that uniform bore, radial ports 158 extend through the wall of the body 140.
As provided in the lower duplex assembly 14, a lock assembly is associated with the valve assembly and extends to engage the housing 116. Tapered slots 160 extend through the wall of the body 140 into corresponding recesses 162. Floating dogs 164 are arranged in the tapered slots 160, extending outwardly into the corresponding recesses 162. Also, as with the lower duplex assembly 14, an annular shoulder 166 in the body 140 rests within a seat 168 in the housing 116.
Below the upper uniform bore extending down to the shoulder 156, a second uniform bore is provided to an inwardly extending annular shoulder 170 cut within the inside of the body 140. Two further sets of radial ports 172 and 173 extend through the wall of the body 140 in the lower uniform bore. Aligned ports 174 and 175 extend through the inner element 134 and the outer element 118, respectively, of the housing 116. Passage is also provided through the cement 138, all aligned with the ports 172. Ports 176 aligned with the ports 173 extend through the inner element 134.
A valve sleeve 178 is arranged within the lower uniform bore within the body 140. This valve sleeve 178 includes O-rings 180 and an inner tapered seat 182 to receive a ball 184. The valve sleeve 178 is originally placed in a first position as seen in FIG. 7a with the wall of the sleeve 178 extending over the radial ports 172. FIGS. 7b through 7d illustrate the valve sleeve 178 in its actuated position with the radial ports 172 uncovered. The initial position of the valve sleeve 178 is maintained until driven by the ball 184 to the lower position by shear pins. The placement of the ball 184 terminates flow from the lower end of the upper duplex assembly 20 through the body 140. With movement of the valve sleeve 178, access from the central passage in the duplex assembly 20 to outwardly of the scab casing 127 is achieved through the ports 172.
A second valve sleeve 186 is arranged above the lowermost valve sleeve 178. This second valve sleeve 186 also includes O-rings 188 to prevent flow around the sleeve 186. An inner tapered seat 190 is arranged to receive a ball 192. Each succeeding ball which is placed in the entire string must be incrementally larger in order that preceding balls can fit through the succeeding inner tapered seats. The second valve sleeve 186 also includes one or more pins 194 extending radially outwardly from the body of the sleeve 186 into and through the ports 173 formed in the body 140. The ports 173 are elongate to form slots. The valve sleeve 186 initially is positioned and held in place by shear pins with the pins 194 at the upper ends of the slots 173 as seen in FIGS. 7a and 7b. The sleeve 186 ends up in its lowered position with the pins 194 at the bottom ends of the slot 173 as seen in FIGS. 7c and 7d. In the upper position, the second valve sleeve 186 covers radial ports or slots 173 extending through the wall of the body 140. With the restraining shear pins broken by the pressure behind the ball 192, the valve sleeve 186 moves to the lower position and uncovers the ports or slots 173.
The second valve sleeve 186 is coupled via the pins 194 through the slots 173 to a sleeve assembly 195. The sleeve assembly is driven downwardly with the valve sleeve 186. The sleeve assembly 195 includes a cylindrical valve 196 which moves downwardly with the valve sleeve 186 to cover over the radial ports 174 exposed by the movement of the valve sleeve 178. The sleeve assembly 195 also closes the radial ports 172 in the body 140. This cylindrical valve 196 remains with the duplex tool when the valve assemblies are withdrawn. A lip seal 197 prevents flow upwardly around the sleeve assembly 195. With placement of the ball 192, communication with the well bore outwardly of the scab casing 127 from the central passage is terminated. At the same time, communication is established between the central passage and the annulus inwardly of the scab casing 127 through the ports or slots 173.
A locking sleeve 198 is positioned in the upper uniform bore. This sleeve also includes O-rings 200 to prevent leakage around the sleeve. An annular recess 202 is arranged about the locking sleeve 198 and an inner tapered seat 204 is arranged to receive a ball 206. With the locking seat 198 in the upper position, held by shear pins, the radial ports 158 are covered as seen in FIGS. 7a. The floating dogs 164 are pressed outwardly so as to engage the duplex housing 116. With the introduction of the ball 206, the shear pins are broken and the locking sleeve 198 drops to the lower position exposing the radial ports 158 and relieving the floating dogs 164 from engagement with the housing 116 as seen in FIGS. 7a-7c.
As seen in FIG. 5, an engagement pipe 208 is arranged above the adapter element 146. The engagement pipe includes a pin 210 for coupling with the internally threaded end of the adapter element 146. The engagement pipe 208 includes a mechanism as shown in FIG. 8. Further drilling pipe 10 can be tightly associated with the engagement pipe 208 which in turn can be less forcefully engaged with the valve assembly 139 of the duplex assembly 20. In this way, the pipe string engages the valve assembly and the valve assembly engages the duplex housing 116 through the lock assembly.
FIG. 4 illustrates yet another duplex assembly associated with the surface casing 25. This further assembly and any more which may be employed would be configured as the upper duplex assembly 20 and associated components. However, care must be taken that each succeeding assembly be sufficiently larger so that the components intended to be removed prior to further drilling have clearance.
Looking to the operation of the overall system, the lower duplex assembly 14 is assembled before entry into the well. This includes assembly of the lower duplex tool 27 including the duplex shoe 18 and the cylindrical housing 26. The valve assembly 42 is positioned with the body 44 extending into the cylindrical housing 26. The scab casing 16 is then assembled with the duplex tool 27. Drilling rod 10 assembled with the engagement pipe 102 is then inserted into the drill pipe 10 and threaded into the internally threaded end 48. The ratchet 106 insures locking between the engagement pipe 102 and the valve assembly 42 without requiring large torque forces on the assembly. The length of the scab casing 16 is substantially the length of the well between the lowest production zone and the adjacent production zone above it. Consequently, the height of this first assembly can be substantial and can require a significant number of drill pipe sections. The upper end of each scab liner may be castellated as shown to provide guides.
The drill pipe 10 extending above the top of the scab casing 16 is intended to traverse the second production zone from the bottom when positioned in the well.
The upper duplex assembly 20, including the cementing basket 22, the valve assembly 139 and the scab casing 127 is assembled. The scab casing 16 is fabricated to extend the length of a nonproduction zone between the second and third production zones from the bottom. This assembly is then coupled with the preceding drill pipe 10 by means of the pin 142. Additional drill pipe 10 is fed into the scab casing 127 from the other end. The engagement pipe 208 is initially coupled with the drill pipe 10 which is inserted into the scab casing 127 to couple with the adapter element 146, the ratchet assembly once again locking the string with the duplex assembly.
Successive upper duplex assemblies 20 may be assembled. Care must be taken that each succeeding system includes sizes which allow the lower systems to be removed as will be discussed below. One last upper duplex assembly 20 may be associated with the bottom of the surface casing 25 as seen in FIG. 4. Drill pipe 10 and casing 25 would then be added as the entire assembly is lowered to the appropriate position indexed with the production zones.
Once the entire assembly is in position, fluid may be introduced if desired to clean out the well. The fluid would proceed down the drill pipe 10 and through the center passage of each valve assembly, finally exiting through the lower port 34 in the duplex shoe 18. Next, a charge of cement is introduced through the drill pipe so that it also flows from the lower port 34 at the bottom of the string. As drilling fluid is present below the duplex shoe 18, the cement is caused to rise around the duplex shoe 18 and upwardly around the scab casing 16. The amount of cement is calculated to substantially fill the annular space between the scab casing 16 associated with the lower duplex assembly 14 and the well bore. As the last of the cement is fed into the well, the ball 90 is added to the circulation and the material being fed down the drill pipe is changed to drilling fluid.
As the charge of cement leaves the lower duplex assembly 14, the ball 90 seats in the valve sleeve 84. The pressure of the flow then shears the pins holding the valve sleeve 84 in the upper position and causes it to drop downwardly to the lower position. This exposes the radial ports 68 as illustrated in FIG. 6b. The flow is then prevented from passing through the length of the duplex assembly 14 by the ball 90. Rather, flow is through the radial port 68. The radial ports 68 are shown to open above the attachment point for the scab casing 16. Consequently, flow down the drill pipe 10 exits through the radial port 68 into the annular space between the cylindrical housing 26 and the scab casing 16. In this way, the entire string is flushed of excess cement.
Once clear of cement, circulation may be discontinued. A period may be required for the cement to set around the lowermost scab casing 16 so as to support its weight.
Once a set is accomplished, circulation is again established and the ball 98 is dropped into the drill pipe 10. The ball 98 seats in the locking sleeve 92, driving the locking sleeve 92 to the lower position. This movement of the locking sleeve 92 opens the radial ports 56 so that circulation may continue. Circulation is cut off through the lower radial port 68.
Additionally, the annular recess 96 moves to a position adjacent the floating dogs 66, allowing the floating dogs 66 to release from the corresponding recesses 64 in the cylindrical housing 26. The valve assembly and the entire string attached above the valve assembly is then released. Circulation may be stopped and the valve assembly pulled upwardly to separate it from the duplex tool 27. The distance the string is lifted is only intended to be sufficient to insure that the lowermost duplex tool 27 is released.
A ball 184 is next positioned in the drill pipe and circulation resumed. The ball 184 seats in the valve sleeve 178 of the next upper duplex assembly 20. This shears the pins and causes the valve sleeve 178 to move to the lower position, opening radial ports 172. The ball 184 also terminates flow through the drill pipe 10 below this upper duplex assembly 20.
A second charge of cement is then introduced into the drill pipe. The charge is sufficient to cement the scab casing 127 into position. At the end of the charge of cement, the ball 192 is dropped into the drill pipe 10 to seat in the valve sleeve 186. As before, this valve sleeve 186 is driven downwardly to its lower position where the cylindrical valve 196 is positioned over the ports 174. At the same time, the radial ports 173 are uncovered to divert flow inwardly of the scab casing 127. Circulation continues through the radial ports 173 until the system is appropriately flushed. Once again time may then be required to allow setting of the cement to a degree sufficient to support the scab casing 127.
Ball 206 is dropped with circulation down the drill string. The ball 206 seats in the locking sleeve 198 and drives it downwardly to the lower position. This opens the radial ports 158 and releases the floating dogs 164. Again, the drill string may be lifted to insure separation.
If additional duplex systems are employed, the process is repeated through completion. Once fully completed, the assembly unlocked from the duplex tools is withdrawn from the well.
Subsequent operation typically requires a drilling out of the aluminum equipment extending inwardly of the casing bore along with residual cement. This drilling may be in concert with underreaming, the placement of liners, gravel packing and the like. Once completed, a production zone exists below what remains of the lower duplex tool 27. Another production zone is above the top of the scab casing 16 associated with that lowermost duplex tool 27 and below what remains of the upper duplex assembly 20. This pattern continues upwardly depending upon the number of scab casings placed.
Accordingly, a system for placing and cementing a plurality of casing segments in a well with one entry is disclosed. While embodiments and applications of this invention have been shown and described, it would be apparent to those skilled in the art that many more modifications are possible without departing from the inventive concepts herein. The invention, therefore is not to be restricted except in the spirit of the appended claims. | A system including method and apparatus for placing and cementing a plurality of scab liners as well as a surface liner in a well with one placement. A duplex assembly is created using a lower duplex tool having a duplex shoe with a valve assembly positioned in the duplex tool. A scab casing is fixed to the duplex tool and drill pipe extends into the scab casing to mate with the valve assembly. A ratchet insures locking of the drill string. The valve assembly includes elements to control flow of cement to outwardly of the scab casing and the flow of flushing fluid inwardly of the scab casing. A locking mechanism using floating dogs controlled by a locking sleeve allows unlocking of the valve assembly from the duplex tool upon completion of the cementing and flushing operation. Similar operations are conducted in succeeding duplex assemblies upwardly along the string, each succeeding scab casing being cemented in turn. Once the cementing is complete, the string and valve assemblies are withdrawn from the well leaving liner segments cemented in place with drill-out duplex elements remaining. | 4 |
CROSS REFERENCE TO PRIOR APPLICATIONS
This application is a National Stage Patent Application of PCT International Patent Application No. PCT/KR2011/001928 (filed on Mar. 21, 2011) under 35 U.S.C. §371, which claims priority to Korean Patent Application No. 10-2010-0059265 (filed on Jun. 22, 2010) which are all hereby incorporated by reference in their entirety.
TECHNICAL FIELD
The present invention relates to a louver module and a louver system employing the same, and more particularly, to a louver module which has an improved ventilation control structure, operating method, material, and shape for imparting heat-resistance and water-tight properties and prevents a louver from deviating through mutual fixation and reinforcement among a plurality of materials, and a louver system having the louver module coupled to a window chassis or door chassis.
BACKGROUND ART
A louver module is devised to screen the sun while reducing visual exposure to the exterior in a place where ventilation is frequently required, to prevent rainwater from flowing into the place in case of rain, and to ensure the ventilation.
In a case where the louver module is of a fixed type, the louver module of the fixed type is configured to be inclined at an angle of 40 to 50 degrees. The inclined angle of the louver is changed depending on an installation purpose or situation of the louver module. The louver module is generally installed in a place where ventilation is required, such as a machine room, parking lot or factory wall.
There has been developed an openable/closable louver module by improving a conventional louver module to be of a rotary type. The openable/closable louver module of the rotary type has excellent sealing performance and ventilation characteristics as compared with the conventional louver module of the fixed type.
The louver module of the rotary type is frequently installed in a place where a boiler in an apartment building, studio apartment or complex building are mounted or in a place where an outdoor unit of an air conditioner is mounted.
However, in the louver module of the rotary type, a louver and a frame are generally made of an aluminum material, and therefore, its heat-resistance effect is lowered. In a case where the temperature difference between the interior and exterior of a room is large, a dew condensation phenomenon occurs, and therefore, walls of the room are contaminated due to the formation of mold in the room.
Further, the conventional louver module of the rotary type has a problem in that sufficient water-tight properties between louvers are not ensured, and therefore, rainwater flows into the room.
Further, in the conventional louver module of the rotary type, a driving mechanism for rotating the louvers is structurally weak, and therefore, the locking state of the louvers is released or some of the louvers are deviated by a malfunction or external impact.
DETAILED DESCRIPTION
Technical Problems
It is thus an object of the present invention to provide a louver module having a rotatably openable/closable louver, in which a louver is configured to be made of a material having heat resistance, such as synthetic resin, and to include compartments in which several air layers are formed, so that it is possible to ensure the heat resistance and to prevent the occurrence of a dew condensation phenomenon even when the temperature difference between the interior and exterior of a room is large.
It is another object of the present invention to provide a louver module which can perform smooth ventilation when louvers are opened, ensure sealing performance between the louvers when the louvers are closed, and prevent rainwater from flowing into the interior of a room between the louvers and frames.
It is still another object of the present invention to provide a louver module in which a driving force is transmitted to a louver using a manual or electric worm gear, so that it is possible to perform a fine manipulation of the louver and to prevent an opening/closing of the louver from being changed by an external impact.
It is still another object of the present invention to provide a louver module in which louvers are firmly coupled to a frame by improving the structure of the louvers, so that it is possible to prevent a phenomenon that the louver is deviated or bent.
It is still another object of the present invention to provide a louver system in which the louver module is coupled to a window chassis or door chassis for ventilation, lighting and entrance.
Technical Solutions
To solve the objective, the present invention provides a louver module, including: a frame having horizontal and vertical frames assembled in a rectangular shape; an opening/closing mechanism assembled with any one of the vertical frames so as to provide torque using worm gears; a louver unit made of a synthetic resin material and including a plurality of louvers each having a compartment forming an air layer for heat resistance therein, wherein symmetrically-shaped brackets are respectively coupled to both ends in the length direction of the respective louvers, a reinforcing beam extended in the length direction is assembled inside each louver, at least one surface of outer surfaces of each louver has a streamline shape, and the plurality of louvers are rotatably mounted between the vertical frames constituting left and right sides of the frame while being horizontally spaced apart in vertical direction from one another; and a power transmission mechanism including a plurality of holders respectively disposed at positions corresponding to end portions of the louvers inside the vertical frames constituting the frame and a pair of shafts disposed inside each vertical frame, wherein each holder has one surface on which a fixing projection is formed and the other surface on which a pair of link projections are formed, the fixing projection of the holder is coupled to the end portion in the length of the reinforcing beam by passing through the vertical frame and the bracket, corresponding to the position of the fixing projection, the link projections of each holder are linked with the respective shafts, and the end portions of the pair of link projections of a specific holder corresponding to the mounting position of the opening/closing mechanism are mounted to the opening/closing mechanism by passing through the linked shafts, wherein the torque is transmitted to the specific holder from the opening/closing mechanism, the pair of shafts are driven in opposite directions to each other by rotation of the specific holder so that the torque is transmitted to other holders, as the holders inside the vertical frame forming one side of the frame are rotated, the torque is transmitted to the louver to be rotated, the holders inside the vertical frame forming the other side of the frame are rotated in connection with the rotation of the louvers coupled to the respective holders, and the pair of shafts inside the vertical frame forming the other side of the frame, which are linked with the holders, are driven in opposite directions to each other.
The opening/closing mechanism may include a driving mechanism providing an original driving force; a worm gear including a worm rotated by the original driving force transmitted from the driving mechanism and a first wheel tooth-combined with the worm 204 so as to generate the torque in a direction vertical to the original driving force; and a second wheel shaft-coupled to the first wheel of the worm gear so as to be rotated by receiving the torque transmitted from the first wheel, and coupled to the pair of link projections of the holder at a position corresponding to the second wheel.
The driving mechanism may include a knob shaft-coupled to the worm and rotated by a user's hand.
The driving mechanism may include an electric motor rotated by a user's manipulation and shaft-coupled to the worm.
The louver unit may further include.
The bracket of the louver unit may further include fixed louvers respectively coupled to uppermost and lowermost portions of the frame in a state corresponding to the state in which the louver is closed.
The bracket of the louver unit may further include at least one of a wedge and a fixing screw, which are coupled to an end portion in the length direction of the louver by passing through the bracket.
The louver may be coupled to the frame so that the streamline-shaped surface of the louver becomes an outer surface, each of the brackets respectively coupled to both ends in the length direction of the louver may further include a beak that comes in contact with a short edge formed on the vertical frame contacting the bracket in the state in which the louver is closed while being extended downward along the streamline-shape surface of the louver, and rainwater may be guided to the streamline-shaped surface of another louver positioned beneath the louver by the beak in the state which the louver is closed so as to prevent the rainwater from flowing in the interior.
A gasket may be further inserted into the louver so as to be parallel with the other surface of the louver, which contacts the streamline-shaped surface of another louver disposed beneath the louver in the state in which the louver is closed.
To solve the objective, the present invention provides a louver system, including: the louver module; and a chassis supporting the louver module to be rotatably opened/closed.
The chassis may support the louver module to be rotatably opened/closed using the horizontal or vertical direction as an axis.
The chassis may be assembled with the louver module to be rotatably opened/closed using the horizontal or vertical as the axis, and the chassis may be coupled to a window or door having a sliding opening/closing function or a hinged opening/closing function.
The chassis may be fixed and coupled to an external chassis.
Advantageous Effects
Based on the above structure, in the louver module having louvers of a rotary type, a louver is configured to be made of a material having heat resistance, such as synthetic resin, and to include compartments in which several air layers are formed, so that it is possible to ensure the heat resistance and to prevent the occurrence of a dew condensation phenomenon even when the temperature difference between the interior and exterior of a room is large.
Further, at least one surface of the louver is formed in a streamline shape, so that it is possible to perform smooth ventilation when the louvers are opened, ensure sealing performance between the louvers when the louvers are closed, and prevent rainwater from flowing into the interior of a room between the louvers and frames.
Further, a driving force is transmitted to the louver using a manual or electric worm gear, so that it is possible to perform a fine manipulation of the louver and to prevent an opening/closing of the louver from being changed by an external impact.
Further, the louvers are firmly coupled to a frame by improving the structure of the louvers, so that it is possible to prevent a phenomenon that the louver is deviated or bent.
Further, the louver system for various windows and doors can be implemented by coupling the louver module to various kinds of chassis such as window and door chassis for ventilation, lighting and entrance.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a perspective view illustrating an embodiment of a louver module according to the present invention;
FIG. 2 is a front view of FIG. 1 ;
FIG. 3 is a left side view of FIG. 1 ;
FIG. 4 is a right side view of FIG. 1 ;
FIG. 5 is a rear view of FIG. 1 ;
FIG. 6 is a perspective view of a louver unit;
FIG. 7 is a side view illustrating the structure of an embodiment of a louver;
FIG. 8 is a side view illustrating the structure of another embodiment of the louver;
FIG. 9 is an enlarged perspective view of portion A of FIG. 6 ;
FIG. 10 is an enlarged perspective view of portion B of FIG. 6 ;
FIG. 11 is a perspective view of a reinforcing beam;
FIG. 12 is an enlarged perspective view of portion C of FIG. 11 ;
FIG. 13 is a perspective view of a gasket;
FIG. 14 is an enlarged view of portion D of FIG. 11 ;
FIG. 15 is a perspective view of a bracket;
FIG. 16 is a left side view of the bracket;
FIG. 17 is a right side view of the bracket;
FIG. 18 is a side view illustrating a state in which an upper fixing louver of the louver unit and an upper horizontal frame are coupled to each other;
FIG. 19 is a side view illustrating a state in which a lower fixing louver of the louver unit and a lower horizontal frame are coupled to each other;
FIG. 20 is an exploded perspective view of a vertical frame;
FIG. 21 is an exploded perspective view illustrating a configuration a power transmission mechanism inside the vertical frame;
FIG. 22 is a perspective view illustrating the vertical frame and an opening/closing mechanism coupled to the vertical frame;
FIG. 23 is an enlarged view of portion E;
FIG. 24 is an enlarged perspective view illustrating a state in which a main vertical frame is removed from the portion E;
FIG. 25 is an enlarged perspective view of the opening/closing mechanism in a state in which a side vertical frame is removed and a case is opened;
FIG. 26 is a schematic view illustrating a link state between the louver and a shaft in a state in which the louver is closed;
FIG. 27 is a schematic view illustrating a link state between the louver and the shaft in a state in which the louver is semi-opened;
FIG. 28 is a schematic view illustrating a link state between the louver and the shaft in a state in which the louver is completely opened;
FIG. 29 is a perspective view illustrating an embodiment of a louver system, which illustrates a state in which the louver system is coupled to a chassis in a state in which the louver module is closed; and
FIG. 30 is a perspective view illustrating an embodiment of the louver system, which illustrates a state in which the louver system is coupled to the chassis in a state in which the louver module is opened.
MODES FOR PRACTICING INVENTION
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the invention are shown. This invention should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, like numbers refer to like elements throughout.
FIG. 1 is a perspective view illustrating an embodiment of a louver module according to the present invention. FIGS. 2 to 5 are front, left side, right side and rear views of the embodiment, respectively.
In the louver module according to the embodiment of the present invention, a louver unit 12 is assembled in a rectangular frame 10 .
Here, the frame 10 includes horizontal frames 14 and 15 and vertical frames 16 and 17 , which are made of a synthetic resin material. The horizontal frames 14 and 15 and the vertical frames 16 and 17 are assembled into a rectangular shape. The assembled horizontal and vertical frames 14 , 15 , 16 and 17 are inserted into a window chassis or door chassis and are screened from the exterior, thereby ensuring heat resistance. The horizontal and vertical frames 14 , 15 , 16 and 17 are preferably made of a material having heat resistance, such as a synthetic resin material.
An opening/closing mechanism 18 is mounted to the vertical frame 16 . The opening/closing mechanism 18 is used to drive the louver unit 12 by providing torque using worm gears described later.
Louvers 20 that occupy most of the area of the louver module according to the embodiment of the present invention are made of a synthetic resin material, and have a structure including a compartment for forming an air layer that acts as a buffer for heat resistance. Therefore, the louver module according to the embodiment of the present invention has heat resistance according to the material and structure of the louvers 20 . That is, since the heat resistance of the synthetic resin material is generally superior to that of the aluminum material, the louvers 20 do not conduct external cool or warm air to the interior. The structure of the louvers 20 will be described later with reference to FIGS. 7 to 10 .
When considering that the louver module according to the embodiment of the present invention is installed in a place where a boiler in an apartment building, studio apartment or complex building are mounted or in a place where an outdoor unit of an air conditioner is mounted, cooling and heating efficiency can be enhanced by the heat resistance of the frame 10 , the louvers 20 and components constituting the louver module and a louver system employing the same. The components constituting the louver module and the louver system are preferably made of a heat-resistance material such as a synthetic resin material, in consideration of the heat resistance.
As described above, the frame 10 and the louver unit 12 has high heat resistance because of their material characteristics, so that it is possible to prevent a dew condensation phenomenon when the temperature difference between the interior and exterior of a room is large.
As configured in FIGS. 1 to 5 , the louver unit 12 includes the louvers 20 and symmetrically-shaped brackets 22 coupled to both ends in the length direction of the respective louvers 20 .
The louver unit 12 receives torque transmitted from the opening/closing mechanism 18 described later, and the louvers 20 are opened/closed by being rotated by the torque. Thus, louver unit 12 performs operations of opening the louvers 20 for the purpose of ventilation and closing the louvers 20 so as to prevent the ventilation from the exterior. The opening/closing of the louvers 20 is performed by being rotated by the torque transmitted from the opening/closing mechanism 18 .
As shown in FIGS. 6 to 10 , the louver 20 of the louver unit 12 has a streamline-shaped surface, and the louver unit 12 includes fixed louvers 20 a and 20 b respectively formed at upper and lower portion thereof. The louvers 20 are horizontally spaced apart in vertical direction from one another between the fixed louvers 20 a and 20 b.
The louver 20 has a streamline-shaped surface disposed toward the exterior when being mounted, and has a structure in which a bottom end in the width direction of one louver 20 is engaged with a top end in the width direction of another louver 20 in a state in which the one louver 20 is closed. A surface opposite to the streamline-shaped surface of the louver 20 may has a flat structure so as to form a flat vertical surface with respect to surfaces of other louvers disposed adjacent to the louver 20 .
A compartment 20 d for buffering both surfaces of the louver 20 using an air layer in the interior thereof is formed inside the louver 20 . Wedge grooves 20 h and fixing screw grooves 20 c are formed at upper and lower portions of the compartment 20 d , respectively. The interior of the compartment 20 d is preferably formed to have a space into which a reinforcing beam 24 having a shape shown in FIGS. 11 and 12 is inserted and to have projections 20 e for supporting the reinforcing beam 24 , protruded from the interior of the compartment 20 d . A recessed portion into which a projection 26 a of a gasket 26 , which has a shape shown in FIGS. 13 and 14 , is formed at one end of the louver 20 .
A reinforcing compartment 20 for forming an air layer may be configured in various shapes at each portion of the louver 20 . As shown in FIG. 7 or 8 , various reinforcing compartments may be formed in the louver 20 , in consideration of the heat-resistance effect, etc. Meanwhile, in FIG. 8 , reference numeral 185 denotes a fixing screw for illustrating a state in which the fixing screw 185 is coupled to the fixing screw groove 20 c.
Hereinafter, the louver 20 configured according to the embodiment of the present invention is illustrated as one configured in an embodiment of FIG. 7 . However, the louver 20 configured in an embodiment of FIG. 8 may be applied according to a manufacturer's intention. FIGS. 7 and 8 illustrate louvers in which the structure of the reinforcing compartment 20 f , etc. is modified in consideration of the heat-resistance effect as described above.
The reinforcing beam 24 having the shape shown in FIGS. 11 and 12 is assembled to the interior of the louver 20 . The reinforcing beam 24 is provided with a fixing port 24 a that has a shape extended in the length direction thereof and is inserted into the louver 20 so as to receive torque while being rotated together with the louver 20 . A fixing projection of a holder, which will be described with reference to FIGS. 20 to 22 , is inserted into the fixing port 24 a.
The reinforcing beam 24 is inserted into the louver 20 , so that it is possible to prevent a phenomenon that the louver 20 is bent due to strong wind pressure or physical environment applied from the exterior. The reinforcing beam 24 may be configured as a beam made of high-strength synthetic resin or metal such as aluminum.
The gasket 26 is inserted into the louver 20 so as to be parallel with the other surface of the louver 20 , which contacts the streamline-shaped surface of another louver 20 disposed beneath the louver 20 in a state in which the louver 20 is closed. As shown in FIGS. 13 and 14 , the gasket 26 has a shape extended in the length direction thereof, and is provided with an arrowhead-shaped projection 26 a inserted into the recessed groove formed in the surface of the louver 20 . The projection 26 a is extended in the length direction of the gasket 26 .
The gasket 26 is mounted at an end portion in the width direction of the louver 20 , so that the sealing performance of the louver 20 can be ensured by the gasket 26 in a state in which the louver 20 is closed to be engaged with another louver 20 . That is, inflow/outflow of a fine draft of air, inflow/outflow of cool or warm air, inflow of moisture, etc. can be blocked by the gasket 26 . To this end, the gasket 26 may be formed of a synthetic rubber material such as an ethylene propylene dienimethylene linkage (EPDM), which has no change in temperature and no deformation caused by ultraviolet light.
The symmetrically-shaped brackets 22 are coupled to both the ends in the length direction of the respective louvers 20 . The bracket 22 can be described with reference to the perspective view, the perspective, left side and right side views of FIGS. 15 to 17 . The bracket 22 may be made of a synthetic resin material.
The bracket 22 is provided with holding portions 22 a and 22 b protruded on one surface so as to hold an end portion in the length direction of the louver 20 .
The bracket 22 has a beak 22 c that comes in contact with a short edge ( 160 of FIG. 20 ) formed at a side of each vertical frame 16 or 17 contacting the louver 20 in the state in which the louver 20 is closed while being extended downward along the streamline-shaped surface of the louver 20 . As the beak 22 c comes in contact with the short edge 160 of each vertical frame 16 or 17 , the flow of rainwater is induced to the streamline-shaped surface of another louver 20 disposed beneath the louver 20 in the state in which the louver 20 is closed. That is, the beak 22 c can prevent exterior rainwater from flowing between the louver 20 and each vertical frame 16 or 17 .
A holder hole 22 d which a fixing projection 182 b of a holder 180 , which will be described later with reference to FIGS. 20 to 22 , passes through is formed at the center of the bracket 22 . Wedge holes 22 e and 22 f which will be described later with reference to FIGS. 20 to 22 are formed in a region adjacent to the holder hole 22 d . Fixing screw holes 22 g and 22 h are formed adjacent to the wedge holes 22 e and 22 f , respectively.
Meanwhile, as shown in FIG. 18 , the horizontal frame 14 is assembled at an upper portion of the fixed louver 20 a disposed at the upper portion of the louver unit 12 , and the horizontal frame 15 is assembled at a lower portion of the fixed louver 20 b disposed at the lower portion of the louver unit 12 .
Referring to FIG. 18 , the upper portion of the fixed louver 20 a is inserted into a clipping horizontal frame 146 . Projections may be formed on an inner wall of the clipping horizontal frame 146 so as to support the coupling state with the fixed louver 20 a inserted into the clipping horizontal frame 146 , and a support 146 b for maintaining the coupling state with a main horizontal frame 144 may be formed on an outer wall of the clipping horizontal frame 146 .
The main horizontal frame 144 has an upwardly opened channel and a downwardly opened channel. The clipping horizontal frame 146 is inserted into the downwardly opened channel of the main horizontal frame 144 , and the upwardly opened channel of the main horizontal frame 144 is closed by being coupled to a cover horizontal frame 142 .
Here, a short edge formed at an end portion of the upwardly opened channel of the main horizontal frame 144 is fastened with a short edge formed on a bottom surface of the cover horizontal frame 142 , so that the assembling state between the main horizontal frame 144 and the cover horizontal frame 142 can be supported. In addition, a short edge formed at an end portion of the downwardly opened channel of the main horizontal frame 142 is fastened with the support 146 b formed on the outer wall of the clipping horizontal frame 146 , so that the assembling state between the main horizontal frame 144 and the clipping horizontal frame 146 can be supported.
Referring to FIG. 19 , the lower portion of the fixed louver 20 b is also coupled to a clipping horizontal frame 156 of the horizontal frame 15 , and the horizontal frame 15 having the same structure as the horizontal frame 14 as described in FIG. 18 is coupled to the fixed louver 20 b . Thus, the coupling structure of the clipping horizontal frame 156 , the main horizontal frame 154 and the cover horizontal frame 152 can be described with reference to FIG. 19 , and its detailed description will be omitted to avoid redundancy.
The fixed louvers 20 a and 20 b of FIGS. 18 and 19 are illustrated as ones applied by partially cutting away the upper and lower ends of the louvers 20 shown in FIGS. 7 and 8 . Any one of the louver 20 according to the embodiment of FIG. 7 and the louver 20 according to the embodiment of FIG. 8 may be selected as the fixed louvers 20 a and 20 b.
The configuration of the vertical frames 16 and 17 will be described with reference to FIGS. 20 and 21 .
The vertical frames 16 and 17 are coupled to the bracket 22 coupled to the louvers 20 . Each vertical frame 16 or 17 includes a cover vertical frame 172 , a main vertical frame 174 and a side vertical frame 176 . A pair of shafts 180 a and 180 b and holders 182 corresponding to the respective brackets 22 are included between the main vertical frame 174 and the cover vertical frame 172 . Here, the holder 182 and the pair of shafts 180 a and 180 b are included in a power transmitting mechanism.
First, a pair of wedges 184 passing through the bracket 22 are inserted into the wedge grooves 20 h of the louver 20 through the wedge holes 22 e and 22 f , respectively. A pair of fixing screws 185 passing through the fixing screw grooves 22 g and 22 h of the bracket 22 are inserted into the fixing screw grooves 20 c of the louver 20 , respectively. Accordingly, the bracket 22 and the louver 20 can have a firm fixing structure through the coupling using the wedges 184 and the fixing screws 185 , and the wedges 184 and the fixing screws 185 can prevent the louver 20 from being deviated from the holder 182 due to an external impact.
The coupling between the cover vertical frame 172 and the main vertical frame 174 , which constitute each vertical frame 16 or 17 may be implemented to have the same structure as the coupling between the horizontal frame 144 or 154 and the cover horizontal frame 142 or 152 . The main vertical frame 174 and the side vertical frame 176 may also has a structure in which short edges of the main vertical frame 174 and the side vertical frame 176 are engaged with each other so as to support the coupling state between the main vertical frame 174 and the side vertical frame 176 .
A fixing projection 182 b is formed on one surface of the holder 182 , and a pair of link projections 182 a are formed on the other surface of the holder 182 .
The fixing projection 182 b of the holder 182 is fixed to the bracket 22 by being inserted into the fixing port 24 a of the reinforcing beam 24 in the louver 20 while passing through a through-hole formed in the main vertical frame 174 , a through-hole 176 a formed in the side vertical frame 176 and the holder hole 22 d formed in the bracket 22 .
The pair of link projections 182 a of the holder 182 may be rotatably linked to each shaft 180 a or 180 b while passing through each shaft 180 a or 180 b . If the shaft 180 a is ascended by the linkage described above, the shaft 180 b is descended, and accordingly, the holders 182 respectively disposed in the vertical frames 16 and 17 , which form one sides linked with the shafts 180 a and 180 b , can be linked and rotated.
The opening/closing mechanism 18 may be mounted to any one of the vertical frames 16 and 17 described above. Although it has been illustrated in the embodiment of the present invention that the opening/closing mechanism 18 is mounted to the vertical frame 16 constituting a left side of the frame 10 , the opening/closing mechanism 18 may be mounted to the vertical frame 17 constituting a right side of the frame 10 as shown in FIG. 22 .
The opening/closing mechanism 18 of FIG. 22 will be described in detail with reference to FIGS. 23 to 25 .
The opening/closing mechanism 18 includes a knob 200 , and a worm 204 and wheels 206 and 208 are included in a case 202 . The knob 200 is shaft-coupled to the worm 204 . If a user rotates the knob 200 , the worm 204 may be rotated in connection with the knob 200 . The worm 204 and wheel 206 are tooth-combined with each other, and the rotational directions of the worm 204 and the wheel 206 vertically intersect with each other. Accordingly, the torque of the worm 204 is generated by the original driving force of the knob 200 , and the torque of which direction is vertically changed by the wheel 206 is generated by the wheel 206 . The wheels 206 and 208 are disposed in parallel, and are connected to each other through a shaft 210 . The torque of the wheel 206 is horizontally transmitted to the wheel 208 .
Here, the worm 204 and wheel 206 may be disposed at the exterior of the cover vertical frame 176 , and the wheel 208 may be disposed between the cover vertical frame 176 and the main vertical frame 178 . A pair of link holes 212 are formed in the wheel 208 , and the pair of link projections 182 a of the holder 182 are inserted into the pair of link holes 212 , respectively.
A specific holder 182 is correspondingly coupled to the wheel 208 , and the link projections 182 a of the specific holder 182 are inserted into the link holes 212 by passing through the pair of shafts 180 a and 180 b , respectively.
The power transmitting mechanism including the opening/closing mechanism 18 , the holder and the shaft is configured as described above. Thus, if a user rotates the knob 200 so as to open/close the louvers 20 , an original driving force is transmitted to the knob 200 by the user, and the worm 204 is rotated in connection with the knob 200 by rotating the knob 200 . Then, torque in the direction vertical to the worm 204 is generated by the wheel 206 , and the wheel 206 transmits the torque to the wheel 208 . The wheel 208 rotates the specific holder 182 coupled thereto.
The specific holder 182 drives the pair of shafts 180 a and 180 b within the vertical frame, in which the specific holder 182 is included, in opposite directions to each other. The driving of the pair of shafts 180 a and 180 b causes rotations of other holders 182 linked with the specific holder 182 , and the holders 182 are rotated, so that the louvers 20 and the brackets 22 coupled to the respective holders 182 are rotated. In this case, the louvers 20 and brackets 22 are rotated using the respective holders 182 as rotary axes so as to be closed or opened according to the rotational direction of the louvers 20 .
That is, the state of FIG. 26 is developed into the states of FIGS. 27 and 28 , so that the louver 20 and bracket 22 can be opened. On the contrary, the state of FIG. 28 is developed into the states of FIGS. 27 and 25 , so that the louver 20 and the bracket 22 can be closed.
In the configuration described above, an electric motor operated under a user's switch operation may be used other than the knob. In this case, the vibration motor may be configured so that the original driving force of which rotational direction is determined by the user's switch operation is transmitted to the worm by the electric motor.
As describe above, in the louver module according to the embodiment of the present invention, the louver 20 included in the louver unit is operated by a worm gear including the gear coupling between the worm 204 and the wheel 206 , so that the opening/closing of the louver 20 can be controlled at a minute angle.
Since the worm 204 and the wheel 206 are engaged with each other through the gear coupling, the opening/closing state of the louver 20 is not easily changed even in the situation in which external pressure caused by a draft of air, etc. is applied to the louver 20 . Thus, the opening/closing state of the louver 20 can be stably maintained.
Since the louver of the louver module according to the embodiment of the present invention is configured so that at least one surface of the louver has a streamline shape, an upward force is generated in air ventilated by the structure of the louver, and thus the flow velocity of the air can be increased. Accordingly, smooth ventilation can be achieved.
The louver module according to the embodiment of the present invention may have a configuration shown in FIG. 29 . FIG. 29 illustrates a state in which a louver module 300 is coupled to a chassis 400 .
Here, the chassis 400 corresponds to a chassis to which a ventilation window or smoke ventilation window of an apartment building, studio apartment or complex building is coupled. The chassis 400 may be installed to have a structure of a fixed type or a structure in which the window can be opened/closed through sliding.
The louver module 300 according to the embodiment of the present invention may be supported to the chassis 400 so as to be rotatably opened/closed using the vertical or horizontal direction as an axis. In a case where the louver module 300 is supported to the chassis 400 so as to be rotatably opened/closed using the vertical direction as an axis, the opening/closing of the louver module 200 can be performed as shown in FIG. 30 .
As described above, the louver module 300 according to the embodiment of the present invention may be variously employed and configured in the louver system.
Although the present invention has been described in connection with the preferred embodiments, the embodiments of the present invention are only for illustrative purposes and should not be construed as limiting the scope of the present invention. It will be understood by those skilled in the art that various changes and modifications can be made thereto within the technical spirit and scope defined by the appended claims. | A louver module which has an improved ventilation control structure, operating method, material, and shape for imparting heat-resistance and water-tight properties and prevents a louver from deviating through mutual fixation and reinforcement among a plurality of materials, and a louver system employing the same. The louver module of includes a frame, an opening/closing mechanism, a louver unit and power transmission mechanism. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to web processing systems, which may perform operations such as forming an image on a web (e.g. of paper) by printing, copying or other marking process, (hereinafter generally referred to as "printing") and/or handling arrangements such as folding or format adjustment. The present invention is particularly, but not exclusively, concerned with processing systems in which the paper or other material orginates as a continuous web on a roll.
2. Summary of the Prior Art
It is very well known to pass paper from a roll through a printing machine to form a series of images on it and then rewind, sheet or fold it into various formats. However, there are fundamental problems which provide a serious limitation to the efficiency of such machines. There is the problem of "down-time". Once the printing machine has been sep up, and the paper put in motion, printing can occur very rapidly. However, with the known machines long delays can occur when any change is made to the method of delivery or to what is being printed. For example, if a different image is to be printed, or if the repeat length of the image is to be changed, or if a different colour is to be used, or the folded format is to be changed, then the print run has to be stopped. The design of the known printing machines is such that it is extremely difficult to make such changes, and hence it is common for the time such machines are not working (the down-time) to be much longer than the effective working time.
A further problem of existing arrangements is that printing machines are designed for a specific printing application, the machine being available as a single entity. What this means, in practice, is that if the owner of the machine wants to carry out more complex operations than are currently possible on his machine, he must undertake quite major engineering or buy a whole new machine.
SUMMARY OF THE INVENTION
The present invention is therefore concerned with overcoming, or at least ameliorating, these problems to design a web processing system in which many changes can be made whilst the system is in operation (can be made "on the fly") and which may also have the advantage of being modular so that the system may be expanded in capability if required.
The web processing system with which the present invention is concerned may be divided into three parts. Firstly, there is the part of the system which takes the web from a roll or reel and feeds it to the rest of the system. Secondly, there is the part which forms an image on the web, and thirdly there is a handling arrangement for the printed web. The present invention has several aspects, each concerned with various parts of such a system.
The first aspect is concerned with the handling of rolls and the input of a web to a printing machine or other imaging apparatus. When webs are input into a printing machine, problems occur at the end of the web. If the machine is not to be stopped, then some splicing arrangement is necessary to attach the end of one web to the beginning of the next. There are two known systems for achieving this. Firstly, there is a system known as a "flying splice" in which joining is carried out with the surface of the new roll moving at the same speed as the running web. The second system is known as a "zero-speed splice" in which the join is effected while both the new roll and the running web are stationary but the press is kept running by means of a reservoir of web such as a festoon.
The first aspect of the present invention seeks to improve the efficiency of the roll handling and the splicing system. In its most general form, this aspect moves rolls of web material on suitable supports, e.g. mobile unwind stands relative to a splicer of a web processing apparatus. With one roll of web material being drawn into the web processing apparatus, another web we may be brought up the splicer, the two webs spliced together, and the web from the second roll drawn into the machine. Splicing may be achieved by flying or zero-speed splicing.
Thus according to this aspect, there may be provided a method of feeding web material to a web processing apparatus, the method comprising, moving, relative to a splicing position, a first reel of the web material from an initial position of that reel towards a final position for that reel; withdrawing web material from the first reel into the web processing apparatus; moving, relative to the splicing position, a second reel of the web material from an initial position of that second reel to a final position for that reel; splicing the web material of the first reel to the web material of the second reel at the splicing position, separating the splice from the web material remaining on the first reel, and then withdrawing web material from the second reel into the web processing apparatus; and completing the movement of the first reel to its final position.
Also there may be provided a mobile unwind stand for a reel of web material, having a movable base, means for supporting the reel such that it is rotatable about its longitudinal axis, and means for controlling the rate of that rotation, and a system for feeding web material to a web processing apparatus, having a plurality of such mobile reel stands, and a splicer adjacent an entrance to the web processing apparatus, the splicer being adapted to splice web material of a reel on one of the mobile unwind stands which is being fed to the entrance to the web processing apparatus to web material of a reel on another of the mobile unwind stands.
The mobile unwind stands provide: the transport systems between the paper store and the machine; the roll stand from which the web is unwound; and the means for returning part-used or reject rolls to the store. In use, successive reel stands may be positioned sequentially adjacent the splicing unit, and moved so that as the required amount of material has been unwound from one roll, the next can be in position. Thus, a replacement roll can be positioned, and the original roll removed, with the printing machine continuing its operation throughout. This reduces the amount of roll handling, facilitates the organisation of work at this part of the machine so as to fit in more flexibly with other machine operating tasks; and permits a machine layout with a better material flow, particularly in situations where part-used or reject rolls are to be removed from the machine.
The next three aspects of the invention are concerned with the imaging arrangements. These aspects are particularly, but not exclusively, concerned with web fed offset press. Such presses typically comprise, for each colour to be printed, and each repeat length: a pair of blanket cylinders between which the web passes (blanket-to-blanket formation); a pair of plate cylinders in contact with a corresponding blanket cylinder, and on which the image to be printed is mounted; and an inking and dampening system for each plate cylinder. Such a system is known as a "perfecting" press, as it prints on both side of the web. It is also known to provide an impression cylinder, and a single blanket cylinder, plate cylinder, and inking and dampening system, if only one side of the web is to be printed.
The second aspect of the present invention purposes an imaging apparatus such as a web-fed offset perfecting press, comprising a plurality of cartridges in an array or stack, or even a plurality of stacks. A common unit for printing medium is then provided in common for several cartridges. Thus, this aspect may provide a web-fed printing apparatus comprising a plurality of cartridges in an array, for printing a web feedable through the array, and at least one unit containing printing medium, each cartridges having means for transferring the printing medium from the unit to the web; wherein the at least one unit is mounted relative to the array so that the at least one unit and the cartridges of the array are capable of relative movement, thereby to permit successive interaction of the at least one unit with at least two of the cartridges. The cartridges may form a web-fed offset printing press, in which case each cartridge may have a pair of blanket cylinders, and a corresponding pair of plate cylinders. The common unit may then be an inking and dampening unit displaceable relative to the cartridges to supply selectively the plate cylinders of at least some of those cartridges, or alternatively the cartridges, themselves may be movable. Thus, it becomes possible to have a printing sequence that can be varied in detail in which the following features can be carried out: the inking the dampening unit is placed in an operative position for a first cartridge and a print run is carried out for that cartridge; then the blanket cylinders of the first cartridge are moved away from the web; the blanket cylinders of a second cartridge (which has different characteristics such as the nature of the image, the image pitch or colour) are moved into contact with the web when the inking and dampening unit has moved to that cartridge. A new printing run can thus be started at the second cartridge with very little time delay. It then becomes possible to change, e.g., the image on a plate cylinder of the first cartridge, whilst the printing machine is running.
The apparatus may include a plurality of inking and dampening units for supplying respective different colours simultaneously to a plurality of selected cartridges (with, in general, at least an equal plurality of cartridges not the being supplied). There may be a plurality of arrays or stacks with driers interposed as required, or a system in which the cartridges can be exchanged for others stored elsewhere.
It is also possible to achieve the feature of interchangability between one printed image and another, by providing a web-fed printing apparatus comprising a plurality of cartridges in an array for printing a web feedable through the array, each cartridge having means for transferring printing medium from a unit for containing such printing medium to the web, the means including at least one printing cylinder which is adapted to contact the web, wherein the at least one printing cylinder of one of the cartridges has a different circumference from that of the at least one blanket cylinder of at least one other of the cartridges.
The printing cylinder may be a blanket cylinder of an offset press, there then being a plate cylinder between the unit for containing the printing medium and the blanket cylinder. For an offset perfecting press there will then be a blanket cylinder, and a corresponding plate cylinder on each side of the web. For other offset presses there is one blanket cylinder, with an impression cylinder on the other side of the web. For a gravure press, the printing cylinder is etched, and the printing medium is transferred from the unit directly to the printing cylinder. Similarly in a flexographic or letter press, printing medium is transferred directly to the cylinder, which in this case has a raised surface carrying the printing medium. For gravure, flexographic, and letter presses there is again an impression cylinder on the other side of the web to the printing cylinder.
The third aspect of the present invention concerns movement of the blanket cylinders of a printing apparatus into and out of contact with the web and their corresponding plate cylinders. In the known systems, the cylinders are constrained so that the blanket cylinders must be precisely mounted in order to achieve their required setting with respect to one another and their corresponding plate cylinders when printing commences. This aspect of the present invention, however, envisages means for moving one of the blanket cylinders towards and away from the plate cylinder and the other blanket cylinder, and hence away from the web, and biasing means for preventing that other blanket cylinder following completely the movement of the first blanket cylinder.
This aspect may therefore provide a web-fed printing apparatus having at least one cartridge, the or each cartridge having a pair of plate cylinders and a pair of blanket cylinders; wherein: the or each cartridge has means for controlling movement of a first one of the blanket cylinders between a first position and a second position; the first position corresponding to a printing position, in which the first blanket cylinder is in contact with a corresponding one of the plate cylinders, and also applies a force to the other blanket cylinder, which force holds the other blanket cylinder in a first position in contact with the other plate cylinder; the second position corresponding to a withdrawn position, in which the first blanket cylinder is withdrawn from contact with the corresponding plate cylinder, and also from the other blanket cylinder, the withdrawal of the first blanket cylinder from the other blanket cylinder permitting that other blanket cylinder to move from its first position to a second position in which it is withdrawn from contact with its corresponding plate cylinder.
Thus, the blanket cylinders move between inoperative positions, in which no printing occurs, and an operative position in which the web is held between the two blanket cylinders, and the two blanket cylinders bear against the plate cylinders so that an image can be transferred.
The fourth aspect of the invention concerns the relationship between the printing arrangement and the subsequent web handling. The printing industry has developed in two directions. One of them is concerned with the handling of elongate webs, such as described above, whilst the other is concerned with handling material in sheet form. In general, each type has its associated problems, and workers in the art tend to concentrate on their own field. It has been realised, however, that the problems of folding occurring in the field of elongate web handling can be effectively solved using techniques from the sheet handling field, which techniques have been evolved to handle the products of a sheet-fed printing machine. Therefore, the fourth aspect of the present invention proposes that the output of a web printing machine is cut into sheets and is fed to a sheet folding system.
Thus this aspect may provide a method of processing at least one web of material comprising printing on the at least one web, cutting in a time relationship with the printing the or each printed web into a plurality of separate sheets, and folding each sheet by a folder whose action is timed in dependence on the arrival of a sheet at the folder, wherein there is continuous movement of the material from prior to the printing to the commencement of the folding of the sheets.
This aspect may also provide a method of processing at least one web of material, comprising printing on the at least one web, forming a longitudinal fold in the or each printed web, cutting in a timed relationship with the printing the or each web into a plurality of separate sheets, and folding each sheet by a folder whose action is timed in dependence on the arrival of a sheet at the folder.
Furthermore, this aspect may provide a method of processing at least one web of material, comprising printing the at least one web, forming transverse perforations in the printed web, cutting in a timed relationship with the printing of the or each web into a plurality of separate sheets, the folding each sheet by a folder whose action is timed in dependence on the arrival of a sheet at the folder.
In a similar way, the present invention may provide a web processing system comprising an apparatus for printing continuously at least one web of material, means for transferring the printed web continuously to a means for cutting the web into a plurality of separate sheets, which means has an action having a timed relationship with the printing means, and means for transferring the sheets continuously to a means for folding the sheets, which folding means has and action which is timed in dependence on the arrival of a sheet at the folding means;
a web processing system comprising an apparatus for printing at least one web of material, means for forming a longitudinal fold in the or each web, means for cutting the web into a plurality of separate sheets, and means for folding the sheets;
a web processing system comprising an apparatus for printing at least one web of material, means for forming a transverse perforation in the or each web, means for cutting the web into a plurality of separate sheets, and means for folding the sheets.
Once the web has been cut, it can be fed to a buckle, knife, or combination folder which may perform various known folding operations on each sheet. This is particularly advantageous when handling lightweight stock, in that the known sheet systems cannot easily handle such stock, at least not unless they run at very reduced speeds. However, it is easy to make an initial fold in the web from the web printing machine, thereby stiffening the material. It also becomes possible to provide a perforation for the first fold made by the folding machine.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will now be described in detail, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 shows a general view of a paper handling system with which the present invention is concerned;
FIG. 2 shows a schematic view of a paper web input system;
FIGS. 3a and 3b show the alignment arrangement for the system of FIG. 2 in plan and side view respectively;
FIG. 4 shows a first embodiment of a web-fed offset perfecting press embodying the second aspect of the invention;
FIG. 5 shows a plan view of the drive system for the press of FIG. 4;
FIG. 6 shows a side view of the drive system for the press of FIG. 4;
FIG. 7 shows a second embodiment of a web-fed offset perfecting press embodying the second aspect of the present invention;
FIGS. 8 and 9 show a third embodiment of a web-fed offset perfecting press embodying the second aspect of the present invention, FIG. 8 being a side view and FIG. 9 being a plan view;
FIG. 10 shows a detail of the cylinder movement system of the press of FIGS. 4 or 7, 8 and 9, illustrating an embodiment of the third aspect of the present invention;
FIGS. 11 and 12 each show axial and radial views of a cylinder with adjustable diameter;
FIGS. 13 and 14 show alternative paper folding systems;
FIG. 15 shows one form of processing and folding paper from a web printing machine, embodying the fourth aspect of the present invention; and
FIG. 16 shows an alternative paper processing arrangement.
DETAILED DESCRIPTION
Referring first to FIG. 1, a web (in this example, paper) handling system with which the present invention is concerned involved three parts. A first part, generally indicated at 1, takes paper from one or more paper rolls in the form of a web 2 and transports it to a printing unit 3 and an optional drying unit 4. As illustrated in FIG. 1, a right-angled turn in the paper web 2 is achieved by passing the paper round an angled bar 5. After passing through the printing unit 3, and the drying unit 4, the paper web 2 is again turned for convenience through 90° via bar 6, and passed to a cutting and folding arrangement generally indicated at 7. Sheets of paper printed, cut and folded as appropriate then pass for e.g. stacking in the direction indicated by the arrow 8. Of course, any arrangement of paper web input unit 1, printing station 3, drying station 4, and cutting and folding arrangement 7 may be provided, the actual configuration depending on space and similar constraints.
As discussed above, the present invention is concerned with various developments of the components of this system.
FIG. 2 shows one embodiment of a transport and feeding arrangement 1 for material (e.g. paper) on rolls. It consists of a splicing unit generally indicated at 10 and a series of mobile reel stands in the form of roll transportation trolleys 11, 12 (although only two are shown, more may be provided). Each trolley consists of a base 13 with wheels or castors 14 which supports roll-lifting and carrying arms 15. The arms 15 of each trolley 11, 12 carry a roll 16 of paper with its axis generally horizontal so that the web of paper may be drawn from the roll and supplied to the splicing unit 10. Each trolley has means for controlling the unwinding of a roll in e.g. the arms 15 of the trolley 11, 12. The leading end of each trolley 11, 12 may be provided with means for interconnecting with the trailing edge of another trolley, or they may be queued without being connected. In this way, it becomes possible to push the trolleys 11, 12 sequentially under the splicing unit 10, so that as one roll is used up, another may be started. This idea of queued trolleys carrying paper rolls may be used with flying splicing arrangements, but zero-speed arrangements are preferred and the arrangement illustrated in FIG. 2 corresponds to the latter.
The trolleys serve for transport from the paper store to the machine and back, and as roll stands from which the paper is unwound. They can be queued so that they may be positioned sequentially adjacent the splicing unit, and moved so that as one roll finishes (on trolley 12) the next (on trolley 11) can be in position. The running web on the trolley 12 is therefore positioned to pass over a roller 17 at the splicing unit 10 at substantially the same angle, so that each subsequent splice is of a predetermined cut off length and is on the same side of the web. This reduces the amount of roll handling, enables the work at this part of the machine to be fitted in more flexibility with other machine operating tasks; and permits machine layout with a better material flow, particularly in situations where part used or reject rolls are to be removed from the machine.
As shown in FIG. 2, a paper web 18 from the leading trolley 12 passes via the roller 17 and a pressure plate 19 to a festoon system 20. The festoon system 20 has a roller 21 which is movable between the position shown in solid lines and the position shown in dotted lines. The roll 16 carrying the next web 22 of paper to be used is mounted on the second trolley 11, and its leading end mounted on a pivotable unit 23. The pivotable unit 23 has a pressure system 24 into which the leading ends of the paper web 22 is fitted, preferably when the unit 23 is in its withdrawn position shown in dotted lines.
As the first web 18 is run, the roller 21 is moved to the position shown in solid lines so that there is a significant amount of paper running within the featoon unit 20. When the end of the web 18 being withdrawn from the trolley 12 approaches, or it is desired to replace one web with another, the input of the web 18 to the festoon unit 20 is stopped, but the output (in the direction of arrow 25) continues as the roller 21 moves towards its dotted position. With the part of the web 18 adjacent the pressure plate 19 stationary, the unit 23 is swung through the position shown in solid lines until the attachment unit 24 comes in contact with the pressure plate, thereby pressing the end of the web 22 (on which adhesive is provided) onto the web 18, causing a splice. The web 18 is then cut below the pressure plate 19 by a knife 26, unit 23 is then withdrawn, and the web 22 may then be drawn into the festoon unit 20 and the roller 21 moved back to its original position shown by a full line.
The accuracy of the feed of a web 18, 22 into the splicing unit 10 and hence through the festoon unit 20 to a printing machine depends on precise alignment of the axis of the rolls 16. If the axis of rolls 16 is not precisely positioned perpendicular to the direction of arrows 25 of the output from the festoon unit 20, there is the risk that the web 18, 22 may be creased or "track" (i.e. move sideways) in the printing machine. To prevent this, it is desirable that there is an arrangement for aligning the trolleys 11, 12, and hence the rolls 16, below the splicing unit. One such arrangement which may be used is shown in FIGS. 3a and 3b.
There are two different alignments needed: to ensure that the axis of the rolls is precisely transverse to the direction of movement of the web, and to ensure that the axis of the roll is at the correct distance from the splicer 10. FIG. 3a shows the first of these. As illustrated, one of the arms 15 of a trolley 11 has two guide balls 30 rotatably mounted on its outer surface, and the other arm 15 has a single guide ball 31, which is rotatably mounted, but also spring loaded, on its outer surface. When the trolley 11 is passed below the splicer 10 (in FIG. 2) the balls 30, 31 contact a pair of guide rails 32, one of each side of the trolley. The two balls 30 ensure that the corresponding arm 15, and hence the rest of the trolley 11, is precisely aligned with the guide rail 32, and the spring loaded ball 31 ensures adjustment due to slight variations in the width of the trolley. The three-point contact of the balls 30, 31 gives accurate alignment with the guide rails 32, which themselves may be accurately aligned with the direction of movement of the web.
As was mentioned with reference to FIG. 2, the trolleys are mounted on wheels or castors 14 and in theory, if the floor 33 was prefectly flat, and the wheels were precisely made, this would ensure accurate vertical positioning of the axis of a roll 16. In practice, however, such accurate positioning is not possible, and therefore the FIG. 3b shows one way of achieving vertical positioning. Each trolley 11 has a pair of support rollers 35 on each side thereof, and a ramp 36 is positioned on the floor 33 generally below the splicer 10. As the leading wheel 14 of the trolley 11 moves onto the ramp 36, the support rollers 35 engage a pair of guide rails 37, one on each side of the trolley 21. The guide rails 37 slope upwardly in the direction of trolley movement, so as the trolley 11 moves, the action of the support roller 35 and the rail 37 is to lift the rear wheel or castor 14 of the trolley 11 clear of the floor 33. Hence the vertical position of the trolley, and hence the roll 16, is determined primarily by the guide rail 37.
As the trolley moves forwards, the support roller 35 moves through positions A to J shown in FIG. 3b.
The system described above requires the arms 15 of the trolley 11 to be locked in position during the movement of the trolley 11 below the splicer 10. It is also thought possible to achieve accurate vertical positioning by moving the arms 15 to a position determined by a suitable stop, although such an arrangement is not preferred.
Thus, FIGS. 3a and 3b illustrate one embodiment of the first aspect of the present invention, embodiment as queuing trolleys for paper rolls.
As explained with reference to FIG. 1, the paper web then passes to a printing unit 3, FIG. 4 illustrates an embodiment of such a unit 3, being a web-fed offset perfecting press according to the second aspect of the present invention. As illustrated, the press has three cartridges 40, 41, 42, with each cartridge having a pair of blanket cylinders 43, 44 in blanket-to-blanket configuration, and a pair of plate cylinders 45, 46 the outer surface of each of which is formed by a printing plate in contact with a corresponding one of the blanket cylinders 43, 44; i.e. each cartridge contains a "printing couple". Normally the plate and blanket cylinders have the same diameter, but it is also known to have plate cylinders of half the circumference of the corresponding blanket cylinder. As illustrated, the cartridges 40, 41, 42 are immediately adjoining each other, as this gives the array of cartridges 40, 41, 42 a small size. It would be possible, however, for the cartridges 40, 41 42 to be in a spaced-apart array. The web 2 passes round a roller 47 and between the pair of blanket cylinders 43, 44 of each cartridge 40, 41, 42. It is preferable if the cartridges 40, 41, and 42 are stacked substantially vertically but substantially horizontal arrangements are also possible including arrangements in which the cartridges are movable transverse to the web. The image to be printed on the web 2 is carried on the plate cylinders 45 and 46, and transferred via the blanket cylinders (hence "offset" printing) to the web. This, in itself, is known.
As shown in FIG. 4, a unit containing printing medium, e.g. an inking and dampening train 48, 49 is provided on each side of the web. The inking and dampening train 48, 49 are capable of moving vertically separately or together and each may contain throw-off mechanisms to facilitate that vertical movement (compare trains 48 and 49).
When printing is to occur, the inking and dampening trains 48, 49 are moved in the vertical direction to register with one of the cartridges 40, 41, 42. The inking and dampening rollers 50 are brought into contact with the plate cylinders 45, 46 by means of mechanisms which ensure correct operating geometries and pressures. As illustrated, the inking and dampening trains 48, 49 are provided on each side of the web 11, but are common to all three cartridges 40, 41, 42. If the cartridge 41 is to print, the trains 48, 49 are operated so that the inking and dampening rollers 50, move into contact with the two plate cylinders 45, 46 of that cartridge 41. A printing run then occurs. At the end of that printing run, the inking and dampening trains 48, 49 are moved to their thrown-off configurations (as shown for 48) and the trains 48, 49 are moved vertically until they are adjacent one of the other two cartridges 40, 42. By moving the inking and dampening rollers 50 into contact with the plate cylinders 45, 46 of another cartridge 40 or 42, a new print sequence can operate.
It is also possible for the cartridges to move vertically, with the trains remaining stationary, but this is mechanically more difficult to achieve. Note also that this arrangement permits "in machine" storage of the cartridges, which is more efficient than the known arrangements.
A suitable drive system for the press of FIG. 4 will now be described with reference to FIGS. 5 and 6. As shown in the plan view of FIG. 5, the inking and dampening trains 48, 49 are mounted on a support frame 51 movable relative to the main frame 52 of the press which supports the cylinders 43, 44, 45, 46 via end supports 52a. The mechanism for horizontal movement of the inking and dampening trains 48, 49 is not shown, but FIG. 4 shows that a stop 53 may be provided on the support frame 51 to limit this horizontal movement.
The vertical movement of the support frame 51, and hence of the inking and dampening trains 48, 49 is controlled by a hoist motor 54 mounted on the support frame 51. That motor 54 drives a shaft 53 extending across the support frame 51 and connected via bevel gears 56, 57 to two shafts 58, 59. Shaft 58 drives a pinion 60 engaging a toothed rack 61 on the main frame 52. Similarly, shaft 59 drives two pinions 62, 63 also attached to the main frame 52 which engage corresponding toothed racks 64, 65 on the opposite side of the main frame 52. Thus rotation of the motor 54 drives shafts 55, 58, 59 causing the pinions 60, 62, 63 top move either up or down on the corresponding racks 61, 62, 65, hence moving the support frame 51 relative to the main frame 52. In this arrangement, a three-point mounting is used, but it would also be possible to provide a four or more point mounting by providing pinions additional on the shafts 58, 59 with corresponding racks on the main frame 52. Accurate vertical positioning of the support frame may be achieved either by accurate control of the motor 54 or by providing a stop 66 (see FIG. 4) on the main frame 52. The stop 66 may be spring-loaded so that it moves out from the main frame 52 when the support frame 51 moves past it, and the support frame 51 then lowered onto the stop 66. Clearly the stop 66 has to be depressed to permit downward movement of the support frame 51, e.g. to operate cartridge 40 in FIG. 4.
The drive for the cylinders 43, 44, 45, 46 will now be described. In fact, the drive train for cylinders 43, 45 and the train for cylinders 44, 46 are the same and the following refers only to the cylinders 43, 45.
A shaft 67 extends up the main frame 52 and movably on it, but engaged for rotation with it is a gear 68 which meshes with a corresponding gear 69 connected to a shaft 70 which extends to a worm 71 which mates to a worm wheel 72. A shaft 73 is secured to the worm wheel 72 and is supported on the support frame 51 by a support 74. At the end of shaft 73 remote from the cylinders 43, 45 is an air cylinder 75 which is capable of moving the shaft 73 axially. At the other end of the shaft 73 is a clutch plate 76 which engages a corresponding clutch plate 77 on a stub shaft 78 extending from the plate cylinder 45. The clutch plates 76, 77 and their attached shafts 73, 78 pass through an aperture 79 in the main frame 52. At the end of the plate cylinder 45 are gears 80 which mesh with corresponding gears 81 on the blanket cylinder 43.
Thus, when the air cylinder 75 moves the shaft 73 so that the clutch plates 76, 77 are in engagement, drive from the shaft 67 is transmitted via gears 68, 69, shaft 70, worm 71, worm gear 72, shaft 73, clutch plates 76, 77, and the stub shaft 78 to the plate cylinder, and hence via gears 80, 81 to the blanket cylinder.
When the air cylinder 75 moves the shaft 73 to disengage the clutch plates 76, 77 no drive is transmitted. Furthermore, this movement of the shaft 73 is sufficient to move the clutch plate 76 clear of the aperture 79, permitting the whole assembly on the support frame to be moved relative to the main frame 52 to another cartridge. This arrangement has the advantage that cylinders of cartridges not in use cannot have any drive thereto, and therefore can be handled safely, e.g. for replacement of the printing plates of those cylinders. Since the cylinder drive mechanism moves with the inking and dampening trains, it is impossible accidentally to drive cylinders which are not to print at any particular time.
The clutch formed by clutch plates 76, 77 has another function. The clutch plates 76, 77 form a "single position" clutch preset to synchronise the position of the corresponding plate cylinder 45 to the drive. Thus, irrespective of the initial position of the plate cylinder 45, its rotation will be synchronised with the rotation of the shaft 67.
Sometimes, however, it is desired to vary the synchronisation of the shaft 67 and the plate cylinder 45, to advance or retard the printing image relative to the main drive. To do this, the worm 71 is moved along shaft 70 by a linear actuator 82, which normally holds the worm 71 fixed on the shaft 70. This rotates the worm wheel 72 which, via shaft 73, and clutch plates 76, 77 rotates the plate cylinder 45 relative to the position of the drive shaft 67. The movement of the worm 71 may also be achieved using a motor or hydraulic ram. Movement of the other plate cylinder 46 relative to the shaft 67 may be achieved in the same way either simultaneously with or separately from movement of the plate cylinder 45.
The drive to the inking and dampening cylinders 50 of the inking and dampening trains 48, 49 will now be described with reference to FIG. 6. Although FIG. 6 is an equivalent view to that of FIG. 4, the cartridges 40, 41, 42 have been omitted for the sake of clarity, as has the drive from hoist motor 54 to move the support frame 51 relative to the main frame 52.
As can be seen from FIG. 6, gears 83 extend from the shaft 70 from gear 69 to the worm 71. These gears 83 engage on an epicyclic gearing 84 on a further shaft 85. Each end of the shaft 85 carries gears 86 which engage gears 87 which connect to the drive system within the inking and dampening units in a conventional way. Thus the shaft 70 is connected to shaft 85 and the drive from shaft 69 which drives the cylinders 43, 44, 45, 46 as discussed with reference to FIG. 5 also drives the inking and dampening rollers 50.
However, this synchronisation depends on the diameter of the plate cylinders 45, 46, and if the press has two different sizes of cylinders, the drive system discussed above can only be in synchronisation for one size, and printing would be out of synchronisation when the inking and dampening units 48, 49 were moved to a cartridge having cylinders of a different size. The arrangement of FIG. 6 overcomes this by providing an auxiliary drive motor 88 connected via the epicyclic gearing 84 to the shaft 85. The speed of rotation of that auxiliary motor 88 is sensed, and the result fed to a comparator 89 which compares that speed with the speed of rotation of rollers 90 between which the paper web passes. These rollers 90 may also be associated with epicyclic gearing. If it is found that the drive is not synchronised, then the motor 88 is speeded up or slowed down until synchronisation is achieved. Thus the drive to the motor 88 modifies the drive transmitted by the gearing 83 to the shaft 85.
FIG. 6 illustrates a further feature of the system, namely that the shaft 67 which drives the plate and blanket cylinder is driven from a shaft 91 which extends beyond the printing station. Thus, additional printing stations may be connected to the shaft or, as illustrated in FIG. 6, may be connected to the perforating tool of a pre-folder 92, or the perforator and cutter of a cutting station. These will be described in detail later, but as can be seen the main shaft 91 has gears 93 drining a shaft 94 of the pre-folder 92 which rotates a perforating tool 95. Again, epicyclic gearing 96 may be provided, linked to the comparator 89.
As illustrated in FIG. 4, one pair of inking and dampening trains 48, 49 is provided in common for three cartridges. In general, therefore, the three cartridges may have different images on their plate cylinders, or even different sizes of cylinders, so that by changing from one cartridge to another, the pring length may be varied. Other arrangements are also possible, however, FIG. 7 illustrates an example of this having four cartridges 100, 101, 102, 103, each of which is similar to the cartridges 40, 41, 42 of the arrangement shown in FIG. 4. The web 2 of paper passes up the middle of the cartridge 100, 101, 102, 103. Four inking and dampening trains are provided, an upper pair 104, 105 serving the upper two cartridges 100, 101 and a lower pair 106, 107 serving the lower two cartridges 102, 103. In this way, for example, it is possible to print two different colours in like size print cylinders, and yet still maintain the possibility of change of image and/or repeat length. Also, as shown in FIG. 7, the cylinders of the cartridges may be different sizes, e.g. with the cylinders of cartridges 100, 102 being smaller than the cylinders of cartridges 101, 103. The press shown in FIG. 7, apart from having four cartridges, as discussed above, may be generally similar to the press of FIG. 4, and have a drive similar to that described with reference to FIGS. 5 and 6. Thereafter, further detailed description of the arrangement of FIG. 7 will be omitted.
One feature of this system is that by adding additional cartridges, and possibly additional inking and dampening trains 48, 49, the number of different printing operations can be increased.
The embodiment described above with reference to FIGS. 4 to 7 have the inking and dampening units moving vertically relative to a vertically stacked array of cartridges. It is also possible to have a horizontal arrangement in which cartridges are in a fixed horizontal array and the inking and dampening units are movable relative to the cartridges on which printing is to commence. One or two inking and dampening units may be used. The drive to the plate cylinders and the inking and dampening units is as described in the vertical unit shown in FIG. 5. The difference lies in the fact that a horizontal power shaft running parallel to the main power shaft may be used to drive the plate cylinders. The drive from the main power shaft may be provided by a vertical shaft connecting the power shaft to the horizontal shaft through two pairs of bevel gears.
As described above, the array of cartridges is fixed and the inking and dampening units are movable. Since the present invention depends on relative movement, it is also possible to have the inking dampening units fixed and move the cartridges of the array. The cartridges may be moved by many ways, such as rollers, guide rails, or pneumatic jacks, and the drive to the plate cylinders of the cartridges may be achieved by single toothed clutches as described with reference to FIG. 6. The advantage of an arrangement using movable cartridges is that the inking and dampening units are fixed and hence the drive to the system may be fixed. However, it is currently considered to be more difficult to move the cartridges than to move the inking and dampening units.
A further embodiment involving fixed inking and dampening units and movable cartridges is shown in FIGS. 8 and 9. This embodiment has four cartridges 111, 112, 113, 114 such as to form a carousel 115. As illustrated in FIG. 8, each cartridge has a pair of plate cylinders 116 and a pair of blanket cylinders 117 in a manner generally similar to the plate and blanket cylinders of the cartridges 40, 41, 42 of the embodiment of FIG. 4. However, it can be seen from FIG. 8 that the plate and blanket cylinders 116, 117 of the cartridges 111, 113, are smaller than the blanket cylinders 116, 117 of the cartridges 112, 114. This enables the cartridges 111, 113, and the cartridges 112, 114 to give different point repeat lengths.
A web 2 of paper enters the printing machine via rollers 118, 119 to move along a horizontal path through two 114, 112 of the four cartridges 111, 112, 113, 114 of the carousel 115. The carousel is rotatably supported on a frame 120 and a second frame 121 supports one or two inking and dampening units 122 (one inking and dampening unit is shown more clearly in FIG. 9). Where one inking and dampening unit is provided it is preferably on the side of the carousel 115 into which the web is fed. Where two inking and dampening units are provided they are normally on opposite sides of the carousel 115 to permit the cartridges 111, 113 or the cartridges 112, 114 to be driven.
The printing machine shown in FIGS. 8 and 9 may operate in one of several ways. For example, it is possible to carry out a print run using only cartridge 114, and during that print run, cartridge 112 may be prepared for a different print run. When the print run through cartridge 114 is completed, the blanket cylinders 117 of cartridge 114, may be withdrawn from the web 2, and the drive to that cartridge removed and then the blanket cylinders 117 of cartridge 112 moved into contact with the web and a drive applied to cartridge 112. A print run may then be carried out using cartridge 112 and cartridge 114 prepared. If cartridges 112 and 114 have the same printing repeat length or printing diameter, it is possible to carry out two colour operation with cartridges 112 and 114 working in tandem.
To change printing to cartridges 111, 113, a motor 123 drives the carousel 115 and turns it on its frame 120, through 90° so that the cartridges 111, 113 are aligned with the web 2. Accurate positioning of the carousel may be achieved by steps (not shown). This rotation of the carousel 115 means that the web 2 must be broken in order to change from one pair of cartridges to the other, and hence this embodiment is less advantageous than the embodiment of FIG. 4. As shown by arrow 124, the carousel 115 may be rotated clockwise or anticlockwise, as desired.
The drive arrangement for the embodiment of FIGS. 8 and 9 will now be described. Referring particularly to FIG. 9, a shaft 125 (which may be connected to a drive system for an entire printing system as discussed with reference to FIG. 6) drives via gears 126 a shaft 127, and hence via gears 128 to a drive arrangement 129 for the inking and dampening unit 122. The drive arrangement 129 may be similar to that described with reference to FIG. 6, i.e. the drive may pass via epicyclic gearing 130 which may be acted on by an auxiliary motor 131 enabling the synchronisation of the drive.
The shaft 127 also has a further gear 132 which connects to a worm 133 acting on a worm wheel 134. The worm wheel turns a shaft 135, at one end of which is a linear actuator 136 and at the other end of which is a clutch 137. The clutch 137 connects to a shaft 138 which drives a plate cylinder 116 of one of the cartridges 111, 112, 113, 114. Thus the drive to the cartridge of this embodiment is generally similar to that described with reference to FIG. 5, and its operation will therefore be immediately apparent.
As shown schematically on the right hand side of FIG. 9, the shaft 127 may also extend to the opposite edge of the carousel 115, to drive another inking and dampening unit (not shown).
A further development of the arrangement shown in FIG. 4 (or FIGS. 7 or 8 and 9) is concerned with the mounting of the cylinders within the cartridges 40, 41, 42 (100, 101, 102, 103 or 111, 112, 113, 114). Clearly, if the cylinders were mounted in a conventional manner each time a cartridge is required to be changed, the printing positions would require precise and lengthy re-setting. Therefore, the third aspect of the present invention concerns an arrangement for moving the blanket cylinders easily into and out of their precise contact positions. When they are in contact, printing can occur. When they are moved out of contact they can then not hamper continuous printing, e.g. by a different cartridge. Furthermore, a cartridge may be removed from a press and replaced e.g. by a cartridge having cylinders of different size, and brought into precise running setting quickly and easily. In this way, many changes may be made to the machine with minimum downtime.
One embodiment of the system for moving the blanket cylinders 43, 44 into and out of contact with the web and their adjacent cylinders is shown in FIG. 10. The solid lines represent the position of the cylinders when they are printing, the dotted lines when they are not. One blanket cylinder 44 is pressed into contact with its associated plate cylinder 46, with the gears 79, 80 in FIG. 5 engaged, and also bears against the other blanket cylinder 43 (the web being then nipped between the blanket cylinders 43 and 44 to ensure good contact for printing). The blanket cylinder 43 then bears against its plate cylinder 45. Normally, a slight freedom is provided in the mounting of the blanket cylinders 43, 44, so that when blanket cylinder 44 is pressed into contact with its adjacent cylinders, both cylinders will automatically position themselves into their precise printing positions by the reactions of the contact pressures to their associated plate cylinders and their co-acting blanket cylinder.
To engage the blanket cylinders 43, 44 one of them (cylinder 44 in FIG. 10) is movable so that its axis moves between positions B and A. This may be achieved, e.g. by mounting the end so the support on which the cylinder rests in a slot, with one end of the slot corresponding to cylinder axis in position B and the other formed in such a way as to allow the cylinder axis to have freedom from the slot sides when in position A. The cylinder axis is pressed into position B by a loaded plunger 140 when printing is not taking place, so that blanket cylinder 44 is in the position shown in dotted lines, and is also out of contact with its corresponding plate cylinder 46 and the other blanket cylinder 43.
The other blanket cylinder 43 is carried on a pivoted support 141 which allows the cylinder axis to move along a restricted arc within an oversize hole (not shown). The boundary of this hole does not influence the axis position when the blanket cylinder 43 is in contact with plate cylinder 45 but does restrict the amount of movement away from the plate cylinder. This permits a gap to open between blanket cylinder 43 and plate cylinder 45 as blanket cylinder 44 moves to position B and also a gap between blanket cylinder 43 and 44 by cylinder 43 being able to follow cylinder 44 but not far enough to maintain contact with it. A similar effect can also be achieved by mounting the support of the blanket cylinder 43 in a slot arranged to allow contact with plate cylinder 45 but restrict movement away from it. If nothing holds the cylinder 43 in contact with plate cylinder 45 it moves away on its pivoted support 141 under a separating force which may be provided by gravity. It is required that the separating force should not exceed a threshold value. If the gravitational (or other) force on the roll 43 exceeds this value, the separating force is reduced by means of a spring 142 or other biasing means such as an air cylinder acting on the pivoted support 141.
As shown in FIG. 10, the blanket cylinder 44 is also mounted on a bracket 143 which is connected to a lever 144 pivoting at point 145. When lever 144 is moved, e.g. by a pneumatic system 146, to the position shown in solid lines, a force is applied to blanket cylinder 44 which moves its axis against the pressure of plunger 140 away from position B towards position A (i.e. the printing position). The blanket cylinder 44 abuts its plate cylinder 46, and also contacts the other blanket cylinder 43, moving it to contact the other plate cylinder 45. The precise positioning and pressure achieved is finally determined by the reactions of the blanket cylinders to their adjacent cylinders and the controlled forces moving them into position (and no longer by the influence of their mounting slots or holes).
Thus, by providing means for moving one of the cylinders into and out of a printing position, and means for the other cylinder to follow over a restricted distance controlled by force reactions, at the "on" position and slot or hole limits at the "off" position, printing may be disengaged and re-engaged quickly and simply, even after a different cartridge has been installed in the press. That is to say, the system provides force loading and self-setting. Ideally the cylinder should run on a continuous surface, and this is best achieved by cylinder bearers (to be discussed later).
The printing machines discussed with reference to FIGS. 4 to 10 thus generally permit printing to occur continuously, but also permit changes of cartridges to be made with quick and easy establishment of the precise settings required. This is very important in minimising down-time. The arrangement shown in FIG. 4 is particularly applicable to single colour (including black) printing. It is also applicable to colour printing although then difficulties may occur in having common inking and dampening trains, and a large number of cartridges and inking and dampening trains may become necessary.
FIGS. 11 and 12 illustrate a design of cylinder which is particularly useful in the present invention. Each cylinder has a core 150 of a given size to which rim units of differing thicknesses may be fitted, as desired. FIG. 11 shows a cylinder with a relatively thick rim unit 151 and FIG. 12 shows a cylinder with a relatively thin rim unit 152. By interchanging the rim units the effective diameter of the cylinder can be changed, without removing the core 150 from the press. The rim units 151, 152 are anti-corrosive (acid gum in the damping fluid may otherwise cause corrosion) and removal of the rim units also allows easy maintenance.
As shown in FIGS. 11 and 12, the rim unit 151, 152 supports a printing plate 153, connected to it by clips 154, 155 which enable the printing plate 153 to be stretched around the cylinder. FIGS. 11 and 12 also show the end rings 156 and clamps 157 at the end of the cylinder for holding the rim unit 151, 152 onto the core 150. The rings 156 act as bearers to ensure smooth rotation of the cylinders, as has been mentioned previously. Note that the rings 156 are slightly thicker than the rim units 151, 152, so that their radially outer surface corresponds exactly with the outer surface of the printing plate 153.
Once the paper web has been printed, then another aspect of the invention comes into play. In most cases, the possibilities for folding of paper whilst in web form are limited (although one or more longitudinal folds may be made as will be described later), but few complicated folding combinations are practicable with the output from web printing machines. On the other hand, there are various techniques for folding paper sheets in e.g. gate folds, multiple transverse folds and longitudinal folds; two are ilustrated in FIGS. 13 and 14.
FIG. 13 shows an arrangement known as a knife fold in which the paper sheet 160 passes over a pair of contrarotating rollers 161, 162. With the sheet 160 stationary in that position, a knife 163 is lowered, forcing the sheet 160 into the "nip" 164, thereby providing a firm fold. The sheet 160 is then drawn down between the rollers 161, 162 for subsequent use. The knife 163 will normally be connected to a photocell or similar detector which detects the presence of sheet 160 below the knife. In this way the folding operation can by synchronised with the arrival of the paper sheet 160 at the folder, rather than synchronised with e.g. an earlier stage of the printing operation.
FIG. 14 shows an arrangement known as a buckle folder in which a sheet of paper 170 passes between a first pair of contra-rotating rollers 171, 172 and its leading edge strikes a ramp 173. The action of the rollers 171, 172 forces the paper sheet 170 up the ramp 173, until its leading edge strikes a stop 174, the position of which is determined by the desired position of fold. When paper strikes the stop 174, it can no longer move up the ramp, and so the action of rollers 171, 172 is force the paper sheet 170 into the nip defined between roller 172 and another roller 175. This forms a sharp fold in the paper, which then passes downwardly due to the action of rollers 172 and 175. It may then strike another ramp 176 and move downwardly to another stop 177. In this position the sheet 170 is then acted on by rollers 175 and 178, between which is another nip causing further folding. It is also possible to perforate the folder paper longitudinally by passing it through a perforating nip formed by rollers 179. Thus, the system in FIG. 14 permits successive transverse folding and perforating of the sheet, and by providing several such units with one or two ramps, any number of transverse folds may be provided. If the direction of movement of the sheet is changed between one buckle folder and the next, both longitudinal and transverse folds may be provided. However, the first fold is generally a transverse one, or extra equipment would be needed. Again the folding of the sheet 170 is in timed dependence on its arrival at the folder, not in dependence of the timing of the printing operation.
It is also possible to provide folders which are a combination of knife and buckle folders.
Referring now to FIGS. 15 and 16, a paper web 2 from a web printing machine (e.g. as in FIG. 4) is cut into sheets by a knife arrangement 180. FIG. 15 shows a perspective view of the arrangement, and the web 2 from the printing machine is first turned through 90° by a bar 6 as has already been described with reference to FIG. 1. Of course, this is not essential and the web path to the knife arrangement 180 may be straight as shown by dotted lines in FIG. 15. This knife unit 180 may be powered from a drive shaft common with the printing station, as described with reference to FIG. 6, i.e. the knife unit 180 shown in FIGS. 15 and 16 corresponding to the element 91 in FIG. 6. A drier unit may also be provided as discussed with reference to FIG. 1. Once the knife arrangement 180 has cut the web 2 into sheets, they may be passed to a folder 181 which may be e.g. a buckle folder such as shown in FIG. 14, although a knife folder as shown in FIG. 13 may also be used. One factor to bear in mind is that the speed of the web from the printing machine may be faster than can be handled by the known sheet folding systems, and it may be necessary to divide the sheet flow so that sub-streams follow two or more routes. In this example a divider 183 is provided so that some sheets pass straight on to the folder 181, and others are diverted to another folder 182. Further changes in direction may occur at units 184 and 185. Such two-route handling of paper sheets is known, and therefore it is unnecessary to discuss it in greater detail here. Clearly, it is possible to provide for any number of folds, depending on the use to which the paper is to be put.
Whereas, as explained above, the first fold is generally a transverse fold in sheet fed systems. FIG. 16 shows a simple way of providing a first, longitudinal, fold in the paper. This is particularly important with thin paper which cannot easily be handled by buckle folders such as shown in FIG. 14. The paper web 2 from the printer machine and (possibly) the drier passes to a former 190 which is triangularly shaped so that a longitudinal fold is placed in the paper as it moves downwardly from a roller 191 to a pair of guide rollers 192, between which a throat is formed. Thus, the paper fed to a buckle folder generally indicated at 193 has already been folded once, in the longitudinal direction, and is therefore less subject to malfunctioning in the folder. Again, however, a knife or similar cutter 194 has to be provided before the web enters the buckle folder 193.
As described above, the folds are made directly to the paper. However, to ease the transverse folding, a transverse perforating unit 195 may be provided upstream of the knife or other cutter 194. Furthermore, the use of a web printer permits longitudinal perforation to facilitate the longitudinal folding shown in FIG. 16, by means of the continuous perforating wheel 196 producing perforations 197. Furthermore, this wheel 196 may be powered from the main drive shaft to the printing station, as was described with reference to FIG. 6. Likewise, any other longitudinal fold can be produced on a continuous basis. Perforation also assists quality by permitting air to escape from within the fold. | A printing apparatus has an array of cartridges for printing a web of e.g. paper passing through the array, and one or more units containing printing medium. The cartridges each are capable of transferring the printing medium from the unit(s) to the web. The unit(s) and the cartridges of the array are relatively movable, to allow the unit(s) to interact successively with at least two of the cartridges. In this way it is possible to change printing from one cartridge to another, allowing changes to be made to what is printed, without halting the movement of web significantly. The present invention also proposes that the cartridges may have printing cylinders of different sizes, and furthermore that a mobile unwind stand may be used to move web material to the printing apparatus, and the web output from the printing apparatus processed by sheet folding techniques. | 1 |
TECHNICAL FIELD
The invention relates generally to internet networking and specifically to addressing conflicts caused by network address and port translation.
BACKGROUND OF THE INVENTION
The problems and solutions addressed by the invention are described herein in terms of the Internet and the TCP/IP protocols that form the basis of Internet communications. However, the invention can apply to other communication protocols as well, depending on the specifics of the protocols.
Internet Network Address Translation is used for several reasons. The main reason is to economize on the use of public addresses. The Internet Protocol (IP) address of a Network Address Translator (NAT) is generally a public address. That is, the NAT IP address is known to the outside world, while all of the servers or clients behind the NAT are private addresses, unknown to the outside world. In such a case, the outside world communicates with the NAT and the NAT controls the communications with the appropriate servers and clients behind it. This means that the IP addresses of devices behind the NAT only have to be unique within that family, but can be duplicative of other IP addresses in the rest of the world. NATs involve only the translation of IP addresses. There is a further type of translation known as Network Address Port Translation (NAPT) in which both IP addresses and port numbers are translated. The standards for Network Address Translation (NAT) and Network Address Port Translation (NAPT) are set forth in the Internet Engineering Task Force (IETF) RFC 3022, entitled “Traditional IP Network Address Translation”.
The original Internet was not designed with security as a primary factor. In fact, the Internet was purposely made relatively open as an aid to scientific and educational communication. However, the advent of the Web and its commercial uses has increased the need for secure Internet communications. The Internet Security Protocol, commonly known as IPsec, was defined to address these issues. For example, IPsec provides for the authentication of network devices and/or for the encryption of transmitted data. An IPsec communication between source and destination addresses is administered in accordance with a security association (SA), which is one or more rules that define the IPsec processing that is applied to the communication. IPsec is defined in RFC 2401 and other RFCs. Whether a packet is denied, permitted without IPsec processing or permitted with IPsec processing is determined by matching the attributes of a packet with the security rules in a security policy database (SPD). To make this determination the known art searches both static and dynamic rules in the order of most specific to least specific attributes for both outgoing and incoming packets. A set of static rules is essentially a security policy. Static rules are predefined and generally do not change very often. Dynamic rules are rules that are negotiated between nodes during IKE (Internet Key Exchange) processing and are added to the security policy database in a dynamic fashion as needed. U.S. Pat. No. 6,347,376 to International Business Machines describes a preferred method of searching the static and dynamic rules of an SPD. This patent is incorporated herein by reference in its entirety.
There are inherent incompatibilities between network address or port translation and IPsec processing. These incompatibilities are a barrier to deployment of IPsec. RFC 3715 recognizes and discusses some of these incompatibilities, but offers no general solutions. For example, Section 4.1 of RFC 3715 refers to a limited solution proposed in RFC 3456, “Dynamic Host Configuration Protocol (DHCPv4, Configuration of IPsec Tunnel Mode”), but states that a more general solution is needed. In addition, Section 5 of RFC 3948 entitled “UDP Encapsulation of IPsec ESP Packets” from the IPsec working group of IETF also addresses some of the incompatibility problems. Particularly, Section 5.2 of the RFC describes briefly a problem in determining what IPsec security associations to use on connections to clients served by a NAT. This Section also describes another problem in allowing a clear text connection to a client behind a NAPT when the NAPT also handles IPsec traffic.
The present invention is directed to the problem of avoiding duplicate sources when clients are served by a NAPT. No solutions are provided for this problem by any of the related IETF RFC documents. For purposes of this specification, duplicate sources are defined as packets having the same source address (e.g., an IP address of a NAPT assigned to an IPsec encapsulated original packet), the same transport protocol and the same original source port number (i.e., a port number in the transport header of the IPsec encapsulated packet).
Duplicate sources result in duplicate connections that breech network integrity. For example, packets can be sent to the wrong destination.
RFC 3947 entitled “Negotiation of NAT-Traversal in the IKE” describes what is needed in the IKE (Internet Key Exchange) phases 1 and 2 for the NAT traversal support. This includes detecting if both ends in a packet communication support NAT traversal, and detecting if there are one or more NATs along the path from host to host. It also covers how to negotiate the use of User Datagram Protocol (UDP) encapsulated IPsec packets in the IKE Quick Mode and describes how to transmit an original source IP address to the other end if needed”. The UDP is defined in RFC 768. RFC 3948, “UDP Encapsulation of IPsec ESP Packets”, defines methods to encapsulate and decapsulate ESP (Encapsulating Security Payload) packets inside of UDP packets for the purpose of traversing NATs. ESP is defined in RFC 2406. ESP is designed to provide a mix of security services in IPv4 and IPv6.
SUMMARY OF THE INVENTION
The invention is directed to preventing duplicate sources of packets in connections that use source addresses, protocols and source port numbers to identify source applications that are served by a NAPT. When a packet is received at a server, a determination is made as to whether the packet is a UDP packet that encapsulates an ESP packet whose transmission path contains a network address port translator (NAPT). In such a case, the original packet is decapsulated to obtain an original source port and original transport protocol. A source port mapping table (SPMT) is searched for an association between the NAPT source IP address, the original source port number, and the original transport protocol associated with the NAPT source IP address and translated source port number. If an incorrect association is found the packet is rejected as representing an illegal duplicate source; that is, a second packet from a different host served by a NAPT that has the same source IP address, source port number and protocol.
In the preferred embodiment, Network Address Port Translator (NAPT) host entries in the SPMT at the server are dynamically built in response to Internet Key Exchange (IKE) messages from internet hosts. Each NAPT host entry contains the source IP address of the NAPT, and a source port assigned by the NAPT. Source port entries in the SPMT are dynamically built as encrypted packets arrive and are decrypted and associations are established between the source port entries and the NAPT host entries of the SPMT. Each source port entry contains a source IP address of a NAPT, an original source port number and an original protocol.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood by reference to the drawings in which
FIG. 1 shows a packet progressing from a client, through a NAPT to a destination host and the changes to the packet headers and contents as the packet progresses;
FIG. 2 shows a return packet responsive to the packet of FIG. 1 ;
FIG. 3 shows an illustrative embodiment of the Source Port Mapping Table (SPMT);
FIG. 4 shows a NAPT translated packet that encapsulates an encrypted original packet;
FIG. 5 shows the packet of FIG. 4 after decryption;
FIGS. 6 and 7 correspond to FIGS. 4 and 5 , respectively, and show a second packet on the same path as the earlier packet that represents an illegal duplicate source caused by the inclusion of a NAPT in the transmission path;
FIG. 8 is a flowchart of the creation of NAPT host entries in the SPMT;
FIG. 9 is a flowchart showing options that are available when an inbound packet first arrives at a destination host;
FIG. 10 is a flowchart showing the processing of an inbound packet that both encapsulates an encrypted original packet and has passed through an NAPT; and
FIGS. 11 and 12 are flowcharts that show alternative ways of processing inbound packets that do not satisfy both conditions of encapsulation and passing through an NAPT.
DETAILED DESCRIPTION
The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments of the invention are shown. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Although the problems addressed by the invention exist for both transport mode and tunnel mode in Internet transmissions, the disclosed embodiment is directed to transport mode. A small variation to be described adapts the transport mode disclosure for operation in tunnel mode.
In the preferred embodiment, the invention is implemented in software. As will be appreciated by those of skill in the art, the present invention can take the form of an entirely hardware embodiment, an entirely software (including firmware, resident software, micro-code, etc.) embodiment, or an embodiment containing both software and hardware aspects. Furthermore, the present invention can take the form of a computer program product on a computer-usable or computer-readable storage medium having program code means embodied in the medium for use by or in connection with a computer or any instruction execution system. In the context of this document, a computer-usable or computer-readable medium can be any means that can contain, store, communicate, propagate, or transport the program for use by or in connection with the instruction execution system, apparatus, or device. The medium can be, for example, but is not limited to, an electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system, apparatus, device, or propagation medium. More specific examples (an incomplete list) of the computer-readable medium would include an electrical connection having one or more wires, a removable computer diskette, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or Flash memory), an optical fiber, and a portable compact disc read-only memory (CD-ROM). Note that the computer-usable or computer-readable medium could even be paper or another suitable medium upon which the program is printed, as the program can be electronically captured, via, for instance, optical scanning of the paper or other medium, then compiled, interpreted, or otherwise processed in a suitable manner if necessary, and then stored in a computer memory.
In this description, like numbers refer to like elements throughout.
IPsec processing can be used to authenticate or to encrypt the contents of packets for security purposes. Authentication and encryption can both be applied to a packet or either can be applied separately. To simplify this presentation, the description of IPsec processing discusses the encapsulation and decapsulation of the packets in terms of encryption and decryption. The processing described is equally valid if authentication is being applied either alone or in conjunction with encryption.
When IPsec processing is applied to outgoing packets from a source client, the processing encrypts the original source and destination ports and the protocol field and encapsulates this encrypted material into a UDP packet. The original client source IP address is retained in the UDP packet, but the source port number is set to 4500 as prescribed by RFC 3948 “UDP Encapsulation of IPsec ESP packets”. If the UDP packet then passes through a NAPT, the NAPT performs further transformations. These transformations are described in detail below with respect to FIGS. 1 and 2 . Specifically, the NAPT substitutes it's own IP address for the client source IP address, assigns a new unique port number to the UDP header and keeps track of these translations so that return packets can be mapped to the original source. RFC 3948 describes a scheme in which the original source port number in a TCP or UDP packet is not changed by the NAPT device, since it is part of the original transport header that is now encrypted as part of the IPsec ESP payload. The port number in the UDP header that is added for UDP encapsulation is changed instead as mentioned above. When such an IPsec packet is received by a server and decrypted, the original source and destination ports of the packet are revealed. For packets that are not processed through IPsec, the NAPT device translates the original source IP address and source port. For unencrypted packets, NAPTs ensure that there are no duplicate connections (duplicate sources).
FIG. 1 shows a packet progressing from a client 10 . 1 . 1 . 1 , through a NAPT 210 . 1 . 1 . 1 and a NAT 211 . 1 . 1 . 1 to a destination host 11 . 1 . 1 . 1 and the changes to the packet headers and contents as the packet progresses. FIG. 2 illustrates the progress of the return packet in the reverse direction, from server to client. With reference to FIG. 1 , the client at IP address 10 . 1 . 1 . 1 sends an encrypted packet destined for the server at IP address 11 . 1 . 1 . 1 . The original contents of the packet before processing by IPsec are shown at 100 . The left column of 100 describes a field type of the packet, while the right column shows the field contents. Note that the destination IP address at 100 is 211 . 1 . 1 . 1 , which is the public address of the NAT in front of the real destination server 11 . 1 . 1 . 1 . It is the responsibility of NAT 211 . 1 . 1 . 1 to map packets to its backend servers such as 11 . 1 . 1 . 1 . At 100 , the source and destination ports are illustratively set to 4096 and 21, respectively. The contents of the packet after IPsec processing are shown at 102 . The lightly shaded portion at the bottom of the packet 102 illustrates the portion encrypted by IPsec. The heavier shaded portions of 102 (and the packet contents at other points of the transmission path) illustrate fields that have changed or have been added at that point in the transmission. At 102 , the real source and destination ports are encrypted values of 4096 and 21 by IPsec and are not readable at this point. IPsec processing has added a UDP header to indicate that this is an IPsec packet that encapsulates the ports and protocol of the original client packet. The source and destination ports in the clear text UDP header added by IPsec are set to 4500 as specified in RFC 3948. An SPI (Security Parameter Index) field is illustratively set to 256. The SPI field, together with a security protocol and a destination address, points to a security association between client 10 . 1 . 1 . 1 and server 11 . 1 . 1 . 1 that governs the encryption algorithm and other security parameters between these entities.
The packet at 102 is translated by the NAPT at IP address 210 . 1 . 1 . 1 to result in the packet shown at 104 . At this point the NAPT 210 . 1 . 1 . 1 has changed the source IP address to reflect its own address of 210 . 1 . 1 . 1 . The NAPT also sets a new unique source port number. In FIG. 1 , the selected source port number is illustratively changed from 4500 to 4501. The NAPT 210 . 1 . 1 . 1 keeps track of this translation for return packets from the server 11 . 1 . 1 . 1 and for future outbound packets from client IP 10 . 1 . 1 . 1 and source port 4500 .
The packet at 104 is re-translated by NAT 211 . 1 . 1 . 1 into the input packet for server 11 . 1 . 1 . 1 . This input packet is shown at 106 . Essentially, the destination IP address of the packet is mapped by NAT 211 . 1 . 1 . 1 into the real destination address 11 . 1 . 1 . 1 of the destination server. The IPsec processing of the packet removes the UDP header added by the IPsec processing at the source 10 . 1 . 1 . 1 and restores the real source and destination port numbers. The restored packet, as shown at 108 is then delivered to the destination port (21 in this example) for application processing.
For completeness, FIG. 2 shows a return packet flow from server 211 . 1 . 1 . 1 to the original client 10 . 1 . 1 . 1 . There is no need to discuss this packet flow in any detail because the duplicate source problem addressed by the invention cannot occur for return packets.
With reference again to FIG. 1 , the packet at 108 contains as a source address the address of NAPT 210 . 1 . 1 . 1 and a source port number of 4096. However, it is possible that another client, say 10 . 1 . 1 . 2 , behind NAPT 210 . 1 . 1 . 1 is also sending packets to host 11 . 1 . 1 . 1 from source port 4096 . Therefore, because of the presence of a NAPT in the path between client 10 . 1 . 1 . 1 and host 11 . 1 . 1 . 1 , there is a possibility of an illegal duplicate source that results in a conflict.
According to the invention, a Source Port Mapping Table (SPMT) is used to detect duplicate sources in which packets are received from clients or servers served by a NAPT. An illustrative SPMT is shown in FIG. 3 at 300 . This table is built dynamically as Internet Key Exchange (IKE) packets are received at a server when an IPsec security association is established. With reference to FIG. 3 , when IKE negotiates an IPsec security association that traverses a NAPT, the TCP/IP stack is notified to create a NAPT host entry such as 302 to represent the remote client, which is represented by the NAPT. This entry contains the source IP address of the NAPT ( 210 . 1 . 1 . 1 in this example) and the source port assigned to this client by the NAPT ( 4501 in this example). FIG. 3 shows a second illustrative NAPT client 304 having the same NAPT IP source address 210 . 1 . 1 . 1 and a different source port 4502 assigned by the NAPT. On the right side of SPMT 300 are source port entries. These entries are created as IPsec encoded packets arrive for which there is no existing entry. The process of adding source port entries occurs after IPsec decrypting has occurred. Associations 306 that map source port entries to NAPT host entries are created as the source port entries are created. A NAPT host entry is removed when the last security association is deleted that pertains to the entry. When a packet arrives and is decrypted, the source NAPT address, the source port of the original packet and the protocol of the original packet are available. The source port entries of the SPMT are searched for a match on these attributes. If a match is found, the associated NAPT host entry is checked for a match on the NAPT source address and the source port assigned by the NAPT. If these latter attributes mismatch, this means that two clients behind the source NAPT are attempting to use the same source port numbers. This represents a duplicate source and the second packet is rejected. If these latter attributes match, then the packet is allowed.
FIGS. 4 through 7 help illustrate the above discussion. FIG. 4 shows a packet coming from a source NAPT. The client address and port are assumed to be 10 . 1 . 1 . 1 and 4096 , respectively, for illustration. 400 is the IP header updated by the NAPT. It contains the NAPT address 210 . 1 . 1 . 1 and a host destination host address 11 . 1 . 1 . 1 . 402 is the encapsulating UDP header added by IPsec processing and updated by the NAPT. Source port 4500 has been changed to 4501 by the NAPT. 404 contains the Encapsulated Security Protocol (ESP) header added by IPsec processing. The TCP transport header 406 contains the original client source and destination ports, 4096 and 21 . 408 contains the payload data followed by the ESP trailer. The transport header 406 and payload 408 are encrypted in accordance with IPsec processing. FIG. 5 represents the packet of FIG. 4 after decryption at the destination host. Note now that the source NAPT address 210 . 1 . 1 . 1 (from packet field 500 ), and the client source port 4096 and protocol (TCP) are now available from field 506 . The source port entries of SPMT 300 are searched using these attributes. In this example, a match is found at 308 . The corresponding association 306 points to NAPT host entry 302 . The source NAPT address 210 . 1 . 1 . 1 and NAPT source port 4501 match this packet (the NAPT source port 4501 is available in the clear from field 402 of the incoming packet). Thus, this packet is associated with a correct connection and is accepted.
FIGS. 6 and 7 represent a second arriving duplicate source packet that will be rejected. This is because the NAPT source address 210 . 1 . 1 . 1 from field 700 , the protocol from field 706 and the source client port 4096 match 308 of the source port entries of SPMT 300 , but the associated NAPT entry 302 does not match the NAPT assigned port number of 4502 from field 602 of the incoming packet.
This process is now explained in more detail below in association with appropriate flowcharts.
FIG. 8 illustrates the initializing of the NAPT host entries of SPMT 300 during IKE negotiations. The IKE negotiation is represented at step 802 . After the negotiation, step 804 sends a notification to the TCP/IP stack to create an associated NAPT host entry in SPMT 300 . This notification contains the NAPT source address and port number retrieved from the IKE flows.
FIG. 9 begins the process of detecting a duplicate source when a data packet arrives at the destination host. Step 902 determines if the incoming packet contains an ESP packet encapsulated in a UDP header, and the source port in the UDP header is not the predefined UDP encapsulation port 4500 . If the above is true, then the packet is using IPsec, either for encryption or authentication, and a NAPT is involved in the transmission path. If a packet is using a UDP protocol with a destination port of 4500 and the first four bytes contain non-zero data, then the packet is identified as a UDP encapsulated ESP packet. If the answer at step 902 is negative, then there are two alternative processing options, option 1 at 904 and option 2 at 906 . These are both discussed below. Assuming that the answer at 902 is yes, then 908 continues at A in FIG. 10 . In FIG. 10 , step 1002 performs the required IPsec processing to decrypt the packet. As a result, the NAPT source address, the original client source port number, and the protocol are obtained in the clear as explained above. Step 1004 searches the source port entries of SPMT 300 on these attributes. At 1006 , if a match is not found, a source port entry is created at step 1008 and inbound processing of the packet continues normally. If a match is found at step 1006 , then step 1010 uses the corresponding association 306 to compare the NAPT assigned source address and port number from the corresponding NAPT host entry to the same attributes from the decrypted packet. If this comparison fails, the packet is rejected at 1011 . If a match is obtained, the packet processing continues as normally at 1012 .
Options 1 and 2 from FIG. 9 represent situations in which packets are sent in the clear (no IPsec processing) or there is no address translation (NAPT) in the path. However, duplicate sources are still possible. Both alternative options 1 and 2 detect such duplicate packets. The processing of option 1 begins at B of FIG. 11 . This option processes all data packets through the SPMT table 300 . This is done by adding another single NAPT host entry designated as “NO IPSEC/NAPT”. When a packet arrives, the source port entries of SMPT 300 are searched as explained above. If no match is found, a source port entry is created at 1106 and associated with the “NO IPSEC/NAPT” NAPT host entry. If a matching source port entry is found at 1104 , step 1110 determines if the corresponding association 306 points to the “NO IPSEC/NAPT” NAPT host entry. If so, the packet is allowed at step 1108 . Otherwise, it is rejected at 1112 . The advantage of this option 1 is simplicity. Its disadvantage is that all data traffic is processed through the SPMT table 300 .
Option 2 uses inbound IPsec packet filtering to reject duplicate source packets. Once IPsec is in place at a host, all packets are processed through the IPsec rules table (the SPD), whether any packet is encrypted or not. This is to verify that unencrypted packets on a given connection are in fact allowed by the IPsec rule that governs the connection. The option 2 process begins at C of FIG. 12 . The incoming packet is processed through the IPsec rule table (not shown) at step 1202 . An example of how this is done in a preferred embodiment can be determined from the aforementioned U.S. Pat. No. 6,347,376. This patent is incorporated herein by reference in its entirety. If the packet is encrypted (step 1204 ), then step 1206 determines if the governing IPsec rule requires encryption. Assuming that is the case, the packet is allowed at 1208 . Otherwise, it is rejected at 1210 . If the packet is unencrypted at step 1204 , then a determination is made at 1212 if the governing IPsec rule allows unencrypted packets and the packet is allowed or rejected accordingly.
In tunnel mode, the IPsec SA is not necessarily end-to-end. For example, an SA might be negotiated between a host and a gateway that serves multiple clients or servers. In tunnel mode a single NAPT address (which is the source IP address in the UDP encapsulating header) could potentially represent multiple hosts. In tunnel mode, the encapsulated, encrypted portion of a packet contains both the original IP address of the source and a transport header. For the purpose of this specification, the original IP address of the source in tunnel mode is called the inner source IP address. Because the inner source IP address is not globally unique, it is not usable for packet routing or for representing the source of a connection. The original source port, such as contained in the source port entries of SPMT 300 , and the encapsulating source IP address with the UDP port alone, as described above for transport mode, might not be unique. To solve this, an additional field that contains the inner source IP address is added to the source port entries (e.g., 308 ) of the SPMT 300 in FIG. 3 . The inner source IP address (not available in transport mode) when combined with the other values of the source port entries yield a unique identifier for hosts protected by a tunnel mode IPsec SA. The inner source IP address is added to the source port entry as part of step 1008 . When a tunnel mode packet arrives, the source port entries of SPMT are searched as described in step 1004 to find an association to a NAPT host entry, and step 1010 , in addition to what has already been described, verifies that the inner source client IP address obtained from the decrypted packet is the same as the client IP address in the source port entry. If this verification fails, the packet is rejected
Artisans in the field of this invention will quickly realize that the preferred and disclosed embodiment can have many minor variations that are within the intent and scope of the teaching. It is the intent of the inventor to encompass these variations to the extent possible in accordance with the state of the applicable relevant art in the field of the invention. For example, the ICMP protocol does not use port numbers; rather, they use query identifiers. With respect to the invention as disclosed and claimed, query identifiers are equivalent to port numbers. | Preventing duplicate sources on a protocol connection that uses network addresses, protocols and port numbers to identify source applications that are served by a NAPT. If an arriving packet encapsulates an encrypted packet and has passed through an NAPT en route to the destination host, the encapsulated packet is decrypted to obtain an original source port number and original packet protocol from the decrypted packet. A source port mapping table (SPMT) is searched for an association between the NAPT source address, the original source port, and the original packet protocol associated with the NAPT source address and port number. If an incorrect association is found, the packet is rejected as representing an illegal duplicate source; that is, a second packet from a different host served by a NAPT that is USING the same SOURCE port and protocol. | 7 |
[0001] This application claims the benefit of priority from U.S. provisional application 60/537,571, filed Jan. 20, 2004, which is hereby incorporated by reference in its entirety.
FIELD OF INVENTION
[0002] The present invention relates to the field of prosthetic devise for human joints. The prosthetics are used for partial or total joint replacement, of for the treatment of chronic conditions such as arthritis. The present invention relates to a prosthesis for the human knee, methods of implanting the prosthesis, a kit for facilitating the implantation of the prosthesis, and a method for manufacturing the prosthesis.
BACKGROUND OF THE INVENTION
[0003] The knee joint is divided into three compartments. The medial and lateral compartments are the weight bearing compartments, while the patello-femoral (PF) compartment articulates the patella with the underlying femur, the patella acting as a pulley for the knee extension/quadriceps muscle mechanism. The surfaces of the joint are covered with cartilage, which has two main functions: it both provides a low-friction (LF) bearing surface and acts to absorb and dissipate the loads that are associated with activities such as walking and running.
[0004] The knee joint has two types of cartilage, hyaline and meniscal. Hyaline cartilage is attached to the femur, tibia and patella. Meniscal cartilage is a fibrous type of cartilage; in the knee are found a medial and lateral meniscus, two C-shaped structures, one in each of the medial and lateral compartments, which help absorb the loads that occur with weight-bearing activities.
[0005] Over time, and with injury or overuse, cartilage breaks down. Unfortunately, cartilage has relatively little capacity for repair. As it breaks down the body's natural healing response is activated; however, instead of healing, chronic inflammation occurs. This inflammation in turn causes pain, which is better known as arthritis. Once arthritis sets in a person is susceptible to chronic pain. When the degeneration of the cartilage progresses beyond a tolerable level of pain the joint can be replaced with a prosthesis in order to relieve the pain. A joint prosthesis replaces the degenerated cartilage with artificial components, generally made out of metals, ceramics, plastics and/or elastomers.
[0006] Knee prosthetic devices can be divided into several types, the most common of which is called a total knee arthroplasty (TKA). The TKA replaces all three compartments of the knee. The femur is replaced with one large component that covers the entire medial, lateral and PF compartments. The tibia is covered by one large tibial component. In between the femoral and tibial components, a plastic (often ultra-high molecular weight polyethylene (UHMWPE)) component is inserted and generally secured to the tibial component. The femoral component articulates with the UHMWPE component that is secured to the tibial component. The patellar surface is generally replaced by a UHMWPE patellar “button” component.
[0007] There are several technical problems associated with TKAs. Among these is the fact that UHMWPE undergoes wear over time. The microscopic wear particles that are formed incite inflammation and loosening of all the components, which in turn ultimately requires a revision surgery. TKAs must also be inserted properly, including maintaining ligament tension balance and proper mechanical alignment of the components; when these are not performed properly the rate of eventual wear is higher than normal. Additionally, the procedure itself is very stressful to the patient, requiring several months, or longer, of rehabilitation before full strength and function are regained. Generally speaking, at least 3 days are spent in the hospital.
[0008] TKAs wear more rapidly in young, active patients. Thus, the procedure is usually delayed in young (i.e. less than 50 year-old) patients. These patients must either wait, enduring the accompanying pain, or, alternatively, they may undergo a TKA, with the likelihood that a second procedure will be required 5 to 20 years later. Finally, once a TKA has been performed, there are certain limits to patient's athletic activities, an additional drawback for the active patient wanting to continue such activities.
[0009] Not all patients have arthritic degeneration in all three knee compartments. Many, especially young, patients, generally have degeneration in only one or two compartments. Due to this fact, a uni-compartmental knee arthroplasty (UKA) is sometimes performed. In the most common type of UKA, the medial compartment is replaced with a prosthesis, sparing the lateral and PF compartments from surgical dissection. The advantage to such a procedure is that there is much less surgery involved, leading to a shorter hospital stay and much more rapid rehabilitation. However, this type of prosthesis has the same problems as does a TKA, in that UHMWPE wear and loosening occurs. In addition, the tibial component may subside, leading to failure of the prosthesis. Again, athletic activities must often be curtailed, in order to prevent subsidence of the tibial component and increased wear of the UHMWPE. This limitation of activity is necessary to prolong the useful life of the prosthesis.
[0010] Although lateral UKAs and PF replacements are currently available, they do not have the same generally good, reproducible results of the medial UKA. Additionally, lateral UKAs and PF replacements have the same drawbacks as do TKAs and medial compartment UKAs.
[0011] Another type of replacement in the knee is a meniscal replacement, a device meant to replace a torn or degenerating meniscus. These devices may be completely synthetic, synthetic with fibrous ingrowth at the periphery, or a scaffold for cellular ingrowth with an eventual meniscus made out of collagen and autologous cells.
[0012] Meniscal replacements that are made out of synthetic material and not meant for cellular ingrowth are represented by U.S. Pat. Nos. 4,502,161 (the '161 patent); U.S. Pat. No. 5,171,322 (the '322 patent); and U.S. Pat. No. 5,344,459 (the '459 patent). The '161 patent describes a meniscal replacement made out of a woven fiber with an outer resilient coating; the device is anchored by a screw at the side of the tibia. The '322 patent describes a stabilized meniscus replacement. The patent does not state specific material; it merely indicates that the prosthesis may be made out of a “biocompatible resilient material.” The '459 patent describes an arthroscopically implantable meniscus replacement, a donut-shaped polymeric device meant to cushion the articulation in an arthritic joint, preferably the knee joint. The implant is made from any one of several materials, including polyethylene, polypropylene, polyurethane or polybutyl rubber.
[0013] Meniscal replacements made out of synthetic material, with a porous periphery allowing for fibrous ingrowth to facilitate attachment to surrounding soft tissue are represented by U.S. Pat. Nos. 4,919,667 (the '667 patent); U.S. Pat. No. 4,344,193 (the '193 patent); and U.S. Pat. No. 6,629,997 (the '997 patent). These patents are hereby incorporated by reference in their entirety. The '667 patent describes a meniscus implant made out of woven fiber and a bonding material, with a porous coating allowing for fibrous ingrowth to anchor the prosthesis to surrounding tissue. The '193 patent describes a meniscus which is made out of silicone rubber, potentially with a porous border to allow for fibrous ingrowth. The '997 patent describes a meniscal implant with a hydrogel surface, reinforced by a 3D mesh. The mesh of this implant is interwoven in a hydrogel for strength, where the hydrogel articulates against adjacent joint surfaces; surrounding tissue may or may not ingrow into the implant at its periphery. This particular implant does not use a low-friction material meant to articulate against adjacent joint surfaces, but rather uses a soft hydrogel. Additionally, the patent claims the use of a mixture of a soft hydrogel and a relatively harder hydrogel; the soft component is intended for joint articulation and the harder hydrogel is meant for the interior portion of the device. The patent does not disclose an implant made for an arthritic joint, but rather one meant for replacement of damaged meniscal tissue.
[0014] A third type of meniscus replacement is the kind made out of material that allows for cellular and fibrous ingrowth, eventually forming a new meniscus made out of normal collagen tissue that was synthesized by the autologous cells that “invaded” the scaffold. U.S. Pat. Nos. 4,880,429, 5,007,934, and 5,158,574 are representative of this type of device.
[0015] A major limitation of all of these meniscal replacement devices is that they do not replace hyaline cartilage. In an arthritic degenerating joint both meniscal and hyaline cartilage are damaged. The above-mentioned meniscal replacements do not replace the damaged hyaline cartilage, only meniscal cartilage, and thus these devices are not suitable for an arthritic joint replacement. Furthermore, these devices do not have any low-friction bearing surfaces which mimic the low-friction bearing function of hyaline cartilage; they merely act as cushioning devices.
[0016] Another type of knee implant is known as a knee spacer. This type of implant is meant to replace more than the meniscal cartilage; it is generally indicated for replacement of a degenerating joint. U.S. Pat. No. 4,052,753 describes a surgically implantable knee prosthesis; the device is essentially a supra-patellar knee spacer. Most knee spacers, however, relate to the tibio-femoral articulation. In fact, several of the meniscal replacements referenced above are actually knee spacer devices that are called meniscal replacements.
[0017] U.S. Pat. No. 6,206,927 describes a surgically implantable knee prosthesis which is a tibio-femoral knee spacer device. It is marketed and distributed as the UniSpacer™ device by Sulzer, Inc. The UniSpacer™ device was developed in order to avoid the wear problems associated with polyethylene devices in young active patients with single compartment degeneration. The design of the UniSpacer™ device is based on three premises: correction of the mechanical deformity and replacement of the missing articular material with the implant; replacement of the meniscal function by a translational and rotational load bearing material; and maintenance of correct anatomical kinematics and restored ligament tension throughout the range of motion. The prosthesis consists of a metal, ceramic, or polymer material. It is meant to occupy the space between the tibial plateau and the respective femoral condyle.
[0018] The implantation of tibio-femoral spacers was originally devised by McKeever in 1957 (Figueroa, Luis, et al., from the course on Mechanics of Materials-I, Applications of Engineering Mechanics in Medicine, GED-University of Puerto Rico, Mayaguez, Engineering Biomechanics of Bone and Artery Replacement , May 2004, p. 2.) and later by Macintosh in 1958 (Macintosh, Hemiarthroplasty of the knee using a space occupying prosthesis for painful varus and valgus deformities . Proceedings of the Joint Meeting of Orthopaedic Associations of the English-Speaking World, JBJS 40(A), December 1958:1431). The devices were developed because of problems associated with the original knee prosthetic devices that were attached to bone, developed in the 30s and 40s. These original devices were hinged, and, although they provided relatively good short-term results, they demonstrated poor range of motion and showed severe problems with loosening and infection. For these reasons they were abandoned and the McKeever and Macintosh devices were adopted. These devices demonstrated some success in pain relief, but results were not predictable. Total knee replacements were developed because many patients continued to show symptoms. In 1968 the first metal and plastic knee, secured to bone with cement, was developed. Later, in 1972, Insall designed what has become the prototype for current TKAs.
[0019] The problems associated with current TKAs primarily involve wear and/or loosening of the prosthetic components, which are often especially pronounced in, and of concern to, young and active patients. When revisions are needed, a major problem is the loss of bone, poorer results than obtained in the original surgery, etc.; these problems can occur regardless of patient age.
[0020] Many patients (especially younger ones) with arthritis may have only a single compartment (more often medial vs. lateral) involved with the arthritic degeneration. If such a patient required replacement surgery it would be advantageous to have a procedure in which only the degenerated compartment is replaced. Thus, in order to treat single compartment degenerative disease, uni-compartmental knee arthroplasty (UKA) was developed. Currently, UKA is optimized for the medial compartment. In older designs a major disadvantage of UKA prostheses was that a follow-up TKA was often more difficult to perform, and the TKA results were often compromised. More recent UKAs are designed with the concept of preserving tibial bone so as not to lead to a comprised TKA in the future.
[0021] There are several advantages to such a device. It is relatively easy to insert and is also easy to remove, especially if degeneration develops in other compartments in the future, or if infection sets in. The UniSpacerm device is based on the fact that no bone resection is needed for its insertion, thus bone cuts are not required for proper implant function, though shaving of the tibial surface may indicated. Instead, the implant adapts to the kinematics of the knee. Furthermore, because no bone is resected future TKAs are not complicated. By avoiding cutting the medial tibial bone, the load bearing capacity of the medial compartment is not compromised. Loosening is not likely as a possible mode of failure because the device is not attached to bone.
[0022] In spite of the advantages of such an implant, the UniSpacer™ device has several problems associated with it. Of major concern is the fact that it does not relieve all a patient's pain. The product is marketed as a device that relieves only some of the pain, in anticipation of a TKA in the future. It is only indicated for the relatively younger patient with unicompartmental disease who wants to maintain a high level of activity, but is willing to live with some pain, even after this device is inserted.
[0023] The ABS, Inc. InterCushion™ device is a second type of unattached spacer device, and is meant to be placed between arthritic femoral and tibial surfaces. It resembles the UniSpacer™ device in that it is shaped to fit between the two joint surfaces. This device, however, is not made out of a rigid material such as metal. Instead, it is made out of an elastomer, polyurethane. The advantage of this device is that it acts as a cushion, and dissipates stresses between the joint surfaces. With better stress dissipation it is expected that there would be less post-operative pain than that associated with the UniSpacer™ device. The InterCushion™ device is not, however, a low-friction implant.
[0024] Bonutti describes yet another type of device that is similar to the above knee spacers in U.S. Pat. No. 6,770,078. In this device the final implant is unattached to surrounding tissues. It is designed such that it is free to move about the tibial surface, allowing for 360° of rotation. However, this implant requires two surgical procedures. In the first procedure a biodegradable implant is sutured to surrounding ligaments, allowing for tissue ingrowth. After a period of time, a ‘wall’ of tissue forms at the periphery of the biodegraded implant, which then acts to contain the final implant, which is inserted at the time of the second surgical procedure. It is a disadvantage for the patient that this implant requires two surgical procedures. Additionally, while this invention describes the use of low-friction material such metal, ceramic, and/or porous materials, it does not include the use of any elastomeric materials.
[0025] Accordingly, while conventional implants are useful, they have numerous significant disadvantages in their use; thus a need remains for a prosthesis that uses a combination of materials to achieve both a low-friction surface and a cushioning function to dissipate force.
SUMMARY OF THE INVENTION
[0026] A knee prosthesis, methods of implanting the prosthesis, method of treating arthritis of the knee, and a kit therefore are provided. The prosthesis answers many of the limitations of current knee prosthetic devices by providing a two-component (or optionally, a three component) device, as either a single structure, or as separate pieces. One of the components is constructed of low friction material, while the second is composed of a weight-dissipating cushioning material; the optional third component is constructed of low friction material. The prosthesis is initially attached to surrounding soft tissue in the knee by biodegradable sutures; it is held permanently in place by fibrous ingrowth into a porous collagen rim in the cushioning component. Major improvements provided by the present invention over currently available prostheses include minimal incisions, minimal or no bone cuts, minimal overall dissection (these improvements lead to shorter hospital stays and rapid rehabilitation and fewer potential for side effects), less prosthetic wear, greater longevity, fewer activity restrictions, able to be used on young, large, active patients, ease of revision, ease of conversion into a total knee arthroplasty if needed.
[0027] Knee arthritis is treated with an implant that mimics the function of both meniscus and hyaline cartilage in a knee joint. The implant replaces the two major functions of these two cartilage types, including low friction articulation and weight load dissipation (cushioning). This is accomplished by the use of two materials. The low-friction aspect is accomplished by the use of a low-friction, hard material. The cushioning property is accomplished by the use of an elastomeric compound. The implants are designed such that surgical dissection is minimized. There is either no or minimal bone resection. No component is attached to the tibial surface. The cushioning component essentially glides on the tibial surface, being attached at its periphery by, initially, biodegradable sutures, and permanently, by fibrous ingrowth from the surrounding soft tissues, as the normal meniscus. The implants include separate medial and/or lateral uni-compartmental implants. The femoral portion of the implant may either be unattached to the femoral condyle, or it may be attached to the condyle. In the former case, the unattached low friction unit is actually attached to the cushioning component, and the combined two-material unit glides on the tibia. In this case the femoral condyle articulates against the underlying low friction portion of the implant. In the latter case, because the low friction component is attached to the femoral condyle, it articulates against the cushioning portion of the implant. The cushioning component is unattached and essentially acts as a cushion between the two joint surfaces. In order to decrease friction between this implant and the underlying tibial surface, an additional option is to have a thin layer of the low friction material attached to the undersurface, or lower surface, of the cushioning component, such that there would be a low amount of friction between the mobile cushioning implant and the underlying tibial articular surface. A final option is to use hyaluronic acid-coated surfaces on the implants in order to further decrease friction and provide a more biological bearing surface.
[0028] The implant of the present invention mimics the function of both meniscus and hyaline cartilage in a knee joint. It replaces the two major functions of these two cartilage types, including low friction articulation and weight load dissipation (cushioning). This is accomplished by the use of two materials. The low-friction aspect is accomplished by the use of a low-friction, hard material. The cushioning property is accomplished by the use of an elastomeric compound. The implants are designed such that surgical dissection is minimized. There is either no or minimal bone resection. No component is attached to the tibial surface. The cushioning component essentially glides on the tibial surface, being attached at its periphery by, initially, biodegradable sutures, and permanently, by fibrous ingrowth from the surrounding soft tissues, similar to the attachment of the normal meniscus to the surrounding menisco-tibial ligaments. The implant may have capacity for fibrous ingrowth from surrounding soft tissue all around the periphery, or on only a portion of the periphery, including the anterior, medial/lateral, and/or posterior portions of the implant. The implants include separate medial and/or lateral uni-compartmental implants. The femoral portion of the implant may either be unattached to the femoral condyle, or it may be attached to the condyle. In the former case, the unattached low friction unit is actually attached to the cushioning component, and the combined two-material unit glides on the tibia. In this case the femoral condyle articulates against the underlying low friction portion of the implant. In the latter case, because the low friction component is attached to the femoral condyle, it articulates against the cushioning portion of the implant. The cushioning component is unattached to tibial bone, and is attached only to surrounding soft tissues at its periphery, and essentially acts as a cushion between the two joint surfaces. In order to decrease friction between this implant and the underlying tibial surface, an additional option is to have a thin layer of the low friction material attached to the undersurface of the cushioning component, such that there would be a low amount of friction between the mobile cushioning implant and the underlying tibial articular surface. A final option is to use hyaluronic acid-coated surfaces on the implants in order to further decrease friction and provide a more biological bearing surface. This invention overcomes many of the problems associated with knee prosthetic devices in the past, which include extensive incisions, extensive bone cuts, extensive overall dissection, long hospital stays, slow rehabilitation, high potential for side effects, great prosthetic wear, poor longevity, prosthetic loosening, extensive activity restrictions, poor performance in young, large, active patients, difficulty of revision, and difficulty of conversion into a total knee arthroplasty if needed.
[0029] In accordance with the present invention, there are a number of embodiments herein disclosed.
[0030] Thus in one embodiment of the present invention, a prosthetic device is provided as a single structure, comprising two components: an upper low friction layer and a lower cushioning layer. It is intended that the prosthetic device not be attached to the tibia or the femur. The upper layer is made out of a low friction material. Bound to the undersurface, or lower surface, of the upper layer is the elastomeric cushioning component (CC). The upper, low friction layer is called the femoral low friction component (FLFC). It is contoured to match the shape of the femoral condyle. The CC, which is made out of an elastomeric material, is contoured on its superior, or upper, surface to the exact dimensions of the undersurface, or lower surface, of the FLFC in order that the two could be attached. The undersurface, or lower surface,of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry.
[0031] In an aspect of this embodiment, the FLFC is made from a material selected from the group comprising metal, metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative), ceramic, glass, carbon composites, polymers, ceramic-coated surface materials, diamond-coated surface materials, or pyrolitic carbon-coated surface materials.
[0032] In yet another aspect, the FLFC is made from metal. In a preferred aspect the metal is selected from the group comprising stainless steel, titanium, or cobalt-chrome alloy.
[0033] In yet another aspect, the FLFC is made from ceramic. In a preferred aspect the ceramic is selected from the group comprising alumina, or zirconium oxide.
[0034] In yet another aspect, the FLFC is made from carbon composite. In a preferred aspect the carbon composite is P25-CVD.
[0035] In yet another aspect, the FLFC is made from a polymer. In a preferred aspect the polymer is selected from the group comprising polyetheretherketone, polyetherketoneketone, polyaryletherketone, or polysulfone.
[0036] In yet another aspect, the FLFC is made from a polymer optionally reinforced with fiber.
[0037] In yet another aspect, the FLFC is made from pyrolitic-carbon coated material.
[0038] In yet another aspect, the FLFC is made from a ceramic-coated material.
[0039] In yet another aspect, the FLFC is made from a diamond-coated material.
[0040] In yet another aspect, the FLFC is made from glass.
[0041] In yet another aspect, the FLFC is made from metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative). In a preferred aspect, the alloy is selected from the group comprising titanium-based Liquidmetal® alloy or zirconium-based Liquidmetal® alloy. In an even more preferred aspect the alloy is zirconium-based Liquidmetal® alloy.
[0042] In yet another aspect, the CC is made from an elastomeric material selected from the group comprising polyurethane, polyvinylalcohol, polyacrlyamide, or fiber-reinforced polymer. In a preferred aspect the CC is made from polyurethane.
[0043] In yet another aspect, the CC is made from a capsule comprising a water retaining center surrounded by a supportive outer covering. In a preferred aspect, the water retaining center is made from hydrogel material selected from the group comprising polyacrylamide or polyvinylalcohol.
[0044] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by the entire periphery of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0045] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by only a portion of the periphery of the implant, including the anterior, medial/lateral, and/or posterior portion(s) of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0046] In yet another aspect, the prosthesis is suitable for initial attachment to surrounding soft tissue by glue or sutures.
[0047] In yet another aspect, the CC further comprises a porous collagen ingrowth coating that facilitates permanent attachment via fibrous ingrowth.
[0048] In yet another aspect, the FLFC is contoured to approximate the shape of the femoral condyle.
[0049] In yet another aspect, the FLFC has a radius of curvature equal to or larger than that of the femoral condyle against which it is intended to articulate. In a preferred aspect, the FLFC has a radius of curvature greater than that of the femoral condyle against which it is intended to articulate.
[0050] In yet another aspect, the superior surface of the CC is contoured to exactly match the undersurface of the FLFC.
[0051] In yet another aspect, the CC is slightly larger than the FLFC.
[0052] In yet another aspect, the CC is attached to the FLFC by mechanical interdigitation, glue, or other bonding method.
[0053] In yet another aspect, the CC is attached to the FLFC prior to packaging.
[0054] In yet another aspect, the CC is attached to the FLFC immediately prior to implantation. In a preferred aspect, the method of attachment of the CC to the FLFC is by mechanical interlocking fixation. In a more preferred aspect, the method of attachment is by a snapping mechanism.
[0055] In yet another aspect, the prosthesis comprising a single structure, of three components: an upper low friction layer, a middle cushioning layer and a lower low-friction layer; wherein it is intended that the prosthetic not be attached to the tibia or the femur; the upper layer is made out of a low friction material; bound to the undersurface of the upper layer is the elastomeric cushioning component (CC); the upper, low friction layer is called the femoral low friction component (FLFC); it is contoured to match the shape of the femoral condyle; the CC, which is made out of an elastomeric material, is contoured on its superior surface to the exact dimensions of the undersurface of the FLFC in order that the two could be attached; the undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface; the contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry; further comprises a tibial low friction component (TLFC), said superior, or upper, surface of component being attached to the undersurface of the cushioning component.
[0056] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit by mechanical interdigitation, glue, or other bonding method.
[0057] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit prior to packaging.
[0058] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit immediately prior to implantation. In a preferred aspect, the method of attachment of the TLFC to the CC is by mechanical interlocking fixation. In a more preferred aspect, the method of attachment is by a snapping mechanism.
[0059] In yet another aspect, the prosthesis components are optionally coated with hyaluronic acid.
[0060] In yet another aspect, the FLFC is suitable for attachment to the femoral condyle. In a preferred aspect, the FLFC is suitable for attachment to the femoral condyle by bone cement, or by use of a porous coating, and/or a hydroxy-apatite coating on the implant which allows for bone ingrowth into the implant.
[0061] In yet another aspect, the FLFC is coated with an elastomeric or cushioning material (e.g. polyurethane).
[0062] In another embodiment of the present invention, a prosthetic device is provided as two components which are not attached to each other: an upper low friction layer and a lower cushioning layer. It is intended in this embodiment that the prosthesis not be attached to the tibia, but one component is attached to the femur. The upper layer is made out of a low friction material; its superior, or upper, surface is made to attach to the femoral condyle. The upper, low friction layer is called the femoral low friction component (FLFC). Below the upper layer is the elastomeric cushioning component (CC). Its upper surface is contoured to match the shape of the overlying FLFC, against which it articulates. The undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry.
[0063] In an aspect of this embodiment, the FLFC is made from a material selected from the group comprising metal, metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative), ceramic, glass, carbon composites, polymers, ceramic-coated surface materials, diamond-coated surface materials, or pyrolitic carbon-coated surface materials.
[0064] In yet another aspect, the FLFC is made from metal. In a preferred aspect the metal is selected from the group comprising stainless steel, titanium, or cobalt-chrome alloy.
[0065] In yet another aspect, the FLFC is made from ceramic. In a preferred aspect the ceramic is selected from the group comprising alumina, or zirconium oxide.
[0066] In yet another aspect, the FLFC is made from carbon composite. In a preferred aspect the carbon composite is P25-CVD.
[0067] In yet another aspect, the FLFC is made from a polymer. In a preferred aspect the polymer is selected from the group comprising polyetheretherketone, polyetherketoneketone, polyaryletherketone, or polysulfone.
[0068] In yet another aspect, the FLFC is made from a polymer optionally reinforced with fiber.
[0069] In yet another aspect, the FLFC is made from pyrolitic-carbon coated material.
[0070] In yet another aspect, the FLFC is made from a ceramic-coated material.
[0071] In yet another aspect, the FLFC is made from a diamond-coated material.
[0072] In yet another aspect, the FLFC is made from glass.
[0073] In yet another aspect, the FLFC is made from metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative). In a preferred aspect, the alloy is selected from the group comprising titanium-based Liquidmetal® alloy or zirconium-based Liquidmetal® alloy. In an even more preferred aspect the alloy is zirconium-based Liquidmetal® alloy.
[0074] In yet another aspect, the CC is made from an elastomeric material selected from the group comprising polyurethane, polyvinylalcohol, polyacrlyamide, or fiber-reinforced polymer. In a preferred aspect the CC is made from polyurethane.
[0075] In yet another aspect, the CC is made from a capsule comprising a water retaining center surrounded by a supportive outer covering. In a preferred aspect, the water retaining center is made from hydrogel material selected from the group comprising polyacrylamide and polyvinylalcohol.
[0076] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by the entire periphery of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0077] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by only a portion of the periphery of the implant, including the anterior, medial/lateral, and/or posterior portion(s) of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0078] In yet another aspect, the prosthesis is suitable for initial attachment to surrounding soft tissue by glue or sutures.
[0079] In yet another aspect, the CC further comprises a porous collagen ingrowth coating that facilitates permanent attachment via fibrous ingrowth.
[0080] In yet another aspect, the femoral condyle is cut to exactly match the superior surface of the FLFC, which is suitable for binding with bone cement.
[0081] In yet another aspect, the femoral condyle is cut to exactly match the superior surface of the FLFC, which is porous coated or hydroxy-apatite coated to allow for bone ingrowth.
[0082] In yet another aspect, the undersurface of the FLFC is polished in order to generate a low friction surface.
[0083] In yet another aspect, the CC is contoured to exactly match the undersurface of the FLFC.
[0084] In yet another aspect, the CC is slightly larger than the FLFC.
[0085] In yet another aspect, the prosthesis comprising two components, which are not attached to each other: an upper low friction component, and a single lower component consisting of two materials, a superior cushioning layer attached to a lower low-friction layer; wherein it is intended that the prosthetic not be attached to the tibia, but one component is attached to the femur; the upper low friction component is made out of a low friction material and its superior surface is made to attach to the femoral condyle. The upper, low friction component is called the femoral low friction component (FLFC). Below the upper FLFC layer is the superior part of the lower component, consisting of an elastomeric cushioning component (CC). Its upper surface is contoured to match the shape of the overlying FLFC, against which it articulates. The undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry; further comprises a tibial low friction component (TLFC), said superior surface of said component being attached to the undersurface of the cushioning component.
[0086] In yet another aspect, the TLFC is attached to the cushioning component by mechanical interdigitation, glue, or other bonding method.
[0087] In yet another aspect, the TLFC is attached to the cushioning component prior to packaging.
[0088] In yet another aspect, the TLFC is attached to the cushioning component immediately prior to implantation. In a preferred aspect, the method of attachment of the TLFC to the CC is by mechanical interlocking fixation. In a more preferred aspect, the method of attachment is by a snapping mechanism.
[0089] In another aspect, the prosthesis components are optionally coated with hyaluronic acid.
[0090] In yet another aspect, the FLFC is suitable for attachment to the femoral condyle. In a preferred aspect, the FLFC is suitable for attachment to the femoral condyle by bone cement or by use of a porous coating, and/or hydroxy-apatite coating on the implant which allows for bone ingrowth into the implant.
[0091] In yet another aspect, the FLFC is coated with an elastomeric or cushioning material (e.g. polyurethane).
[0092] In another embodiment, there is provided a method of providing a knee prosthesis to a patient in need thereof, said method comprising: ascertaining the size and shape of the required prosthesis and components thereof by examination of the patient; and providing to the patient a prosthesis according to the present invention.
[0093] In another embodiment, there is provided a method of knee reconstruction of a patient in need thereof, said method comprising: determining the proper size and shape of a prosthesis and components thereof according to the present invention, by examination of the patient; selecting the prosthesis according to the present invention of said proper size and shape; exposing the knee compartment; and implanting the knee prosthesis into the compartment.
[0094] In another embodiment, there is provided a method of making a prosthesis of the present invention comprising CAD/CAM design of molds for casting the prosthesis component.
[0095] In yet another embodiment there is provided a method of making a prosthesis of the present invention comprising CAD/CAM techniques to directly machine the components from blocks of material.
[0096] In another embodiment, there is provided a kit for treating arthritis of the knee comprising a prosthesis of the present invention and means for implanting said prosthesis.
[0097] In another embodiment, there is provided a method of implanting a prosthesis of the present invention, wherein the prosthesis is inserted between the femoral and tibial surfaces.
[0098] In another embodiment, numerous sizes of the components are provided so as to provide a prosthetic device appropriate for a given patient.
[0099] These and other embodiments of the invention will become apparent in light of the Detailed Description below.
BRIEF DESCRIPTION OF DRAWINGS
[0100] FIG. 1 shows a perspective view of the two piece construct. There is a top, or superior, piece ( 1 ), the FLFC (femoral low-friction component), that is made out of a low friction material. Its shape conforms to that of the femoral condyle. This shape resembles the general shape of the meniscus cartilage, but instead of forming a “C” shape with an open central/inner portion as in the normal meniscus, the central or inner portion is solid. The front (anterior) ( 2 ), back (posterior) ( 3 ), and side (lateral) ( 4 ), portions are raised. The undersurface is attached to the elastomeric cushioning component ( 5 ).
[0101] FIG. 2 shows the manner by which the periphery of the CC is to be attached to the menisco-tibial ligaments, with an area for initial biodegradable suture attachment and permanent fibrous ingrowth. The rim ( 7 ) of the CC ( 5 ) has a collagen ingrowth coating ( 7 ). Rings ( 8 ), or a suitable alternative, may be used for suture fixation, which gives initial stability before fibrous ingrowth takes place.
[0102] FIG. 3 demonstrates a frontal view of the manner by which the implant is inserted between the femoral and tibial articular surfaces. Fibrous ingrowth from the peripheral menisco-tibial ligaments ( 10 ) is demonstrated ( 9 ).
[0103] FIG. 4 is a lateral view of the manner by which the implant is inserted between the femoral and tibial articular surfaces.
[0104] FIG. 5 shows a perspective view of the single unit as a three piece combined construct. Here there is a top, superior, piece ( 1 ), the FLFC. The CC has an outer rim for initial biodegradable suture attachment ( 7 ) and for later permanent fibrous ingrowth ( 7 ).
[0105] FIG. 6 demonstrates a lateral view of the attachment of the FLFC ( 12 ) to the femoral condyle. It is attached by either the use of bone cement or by bone ingrowth into a porous coated attachment surface on the FLFC ( 12 ). Pegs ( 13 ) may be added in order to increase fixation stability of the implant into the femoral bone.
[0106] FIG. 7 shows the FLFC attached to bone, with the interdigitating CC attached to a TLFC ( 11 ) piece at its undersurface. The CC portion may be attached to surrounding soft tissue menisco-tibial ligaments ( 9 ) initially by biodegradable sutures and eventually by permanent fibrous ingrowth ( 10 ).
[0107] FIG. 8A shows the hydrogel/supportive outer coating option for the prosthesis. This cushioning hydrogel is relatively elastic, with a modulus of elasticity (MOE) that is between 0.1-50 MPa. The outer covering is made out of a relatively inelastic material, in order to prevent excessive deformation and to maintain a constant negative inside pressure, such that osmotic flow is always directed inwards. It is preferably made out of material with a relatively low MOE such as ultra high molecular weight polyethylene fibers (MOE @ 700 MPa). There is enough elasticity for bending to occur, but very little stretching occurs. The superior surface has a FLFC as disclosed above. The undersurface has a TLFC, as disclosed above. The CC, instead of being composed of one elastomeric material, may consist of two parts: an inner hydrogel component and an outer water-permeable synthetic fiber component ( 14 ). The hydrogel has an affinity for water and will attract water inside, as noted by ( 15 ). This constant inward flow of water puts outward pressure on the outer coating ( 14 ) and both the FLFC ( 1 ) and the TLFC ( 11 ), as depicted by the arrows inside the component. This constant inward flow of water is resisted by the outer coating ( 14 ).
[0108] FIG. 8B shows what would happen if the hydrogel ( 16 ) were not surrounded by the outer coating. Here the unimpeded inward flow of water causes the hydrogel to expand to a much larger size. The inward and outward water flow pressures equilibrate ( 17 ).
[0109] FIG. 8C shows what occurs with weight loads. The weight load ( 18 ) causes the thickness of the cushioning component to decrease ( 19 ). The outward flow of water increases beyond the inward flow ( 20 ).
[0110] FIG. 9 shows the hyaluronic acid coating on the prosthesis.
DETAILED DESCRIPTION OF THE INVENTION
[0111] The invention herein relates to a knee prosthetic implant that overcomes some of the limitations of current TKAs, UKAs, and “spacer” devices, methods of implanting the device, and a kit for implantation of the device. The advantages of the device of the current invention include, by way of illustration only but by no means meant to be a comprehensive list, minimizing surgical procedures, minimizing bone dissection, replacement of meniscal cartilage, mimicry of the function of meniscal cartilage, replacement of hyaline cartilage, mimicry of the function of hyaline cartilage, and usefulness for young, active patients with arthritis of the knees for whom TKAs are relatively contraindicated. It is believed that no other current device is available which accomplishes all of mimicry of both meniscal and hyaline cartilage and function, minimal surgical procedure and minimal or no bone cutting, and the potential for attachment to surrounding soft tissue.
[0112] The device of the current invention mimics both hyaline and meniscal cartilage function. The knee prosthetic device consists of separate medial and lateral implants. Each implant is designed specifically in a manner that mimics the two main functions of joint cartilage. These two properties are:
(a) Low friction articulation; and (b) Dissipation of the stresses of weight bearing.
[0115] The human body satisfies the above two requirements by the unique interaction of the surface of the cartilage extra-cellular matrix (ECM), with hyaluronic acid acting as a lubricant for low friction articulation, with the flow of water molecules acting to disperse weight bearing stresses. The normal architecture of ECM includes negatively charged proteoglycans (PGs) and a collagen network, both of which have an affinity for water. When a load is applied to cartilage, water is pushed out of the ECM and the negatively charged PGs repel each other, dispersing the load, thus decreasing the load to any one area and to the underlying structures. When the load is released, water flows back into the ECM. This flow of water and the repelling nature of the negatively charged groups are thus responsible for the shock-absorbing properties of cartilage. It is current understanding that the PGs contribute to the compressive and/or swelling properties, while the collagen network provides the cohesive properties (resisting the negatively charged swelling pressure of the PGs) and strength in tension. The importance of this cushioning effect is to dissipate weight-bearing stresses to the joint structures, i.e. cartilage and underlying bone. Without a cushioning effect, there is an increased amount of weight bearing stress that is passed on to local areas of bone; this increased stress to bone may be one of the factors that can lead to pain.
[0116] With respect to joint replacement materials, it is difficult, if not impossible, to find a single material, for use in the human body, which provides both low-friction and cushioning. This is because these two properties are in opposition when it comes to mechanical function; the types of materials used to grant either property exemplify this. The best low friction articulating surfaces are generally very hard with little elasticity. Of course, a cushioning effect cannot be provided by a rigid metal device, such as the UniSpacer™ device. Another material which is generally low-friction, ceramic tends to be brittle and thus undergo fatigue failure, which gives it limitations when it is to be used in certain types of implants, and certainly makes it unsuitable for use as a cushioning material. In general, the best bearing surfaces, whether they are ceramic or metal, generally have very low elasticity. Thus the materials with the best bearing surface properties have virtually no, or minimal, stress dissipation (cushioning) effects.
[0117] Materials that dissipate stress well inherently have a certain amount of elasticity in them. When stress is applied to the surface of these materials, some motion occurs at the surface; in other words, there is some microscopic movement of the surface molecules. The overall result of this surface action is that it is associated with a higher level of friction when it glides against an opposing surface. Furthermore, this microscopic movement is associated with the development of microscopic particles that break off when an opposing stress is applied to them, i.e. weight bearing stress. Thus, the materials with the best cushioning properties generally do not work well as low friction bearing surfaces.
[0118] Although a number of implants have been designed for use as knee replacements for arthritis, there is no single device currently available which exhibits both a low friction surface for articulation and a cushioning component for force dissipation. Current TKAs are designed with a polyethylene implant that is attached to bone, the tibial component, and articulates against a femoral component that is made out of a metal or ceramic. Polyethylene has no elastic or cushioning properties, and thus it does not confer either elasticity or cushioning. U.S. Pat. No. 6,302,916 describes the use of polyurethane in place of polyethylene in a TKA, which is an improvement. However, the TKA procedure requires relatively extensive surgical dissection and bone cuts, and it includes implant attachment to the tibial bone; such extensive surgical requirements do not address the need for minimal surgery. The proposed device of the present invention addresses the needs for a low friction surface, weight dissipating cushioning, and can be inserted with minimal surgery and minimal or no bone cuts, and no attachment to the tibial bone.
[0119] One of the problems in standard UKAs is the tibial bone cut. The cut must be made with proper rotation and angulation. Even slightly inaccurate positioning can result in a more rapid rate of wear and loosening. Tibial bone cuts, if made too deep, are associated with subsidence and/or loosening of the tibial component, which leads ultimately to prosthetic failure. Furthermore, by removing some tibial bone, and adding cement into the tibial cancellous bone, a revision TKA becomes more difficult, if one is require in the future.
[0120] (a) Low Friction Material
[0121] In practicing the invention, the phrase “low friction” means a low coefficient of friction (COF); a low COF in the context of the present invention would be about 0.001 to 0.5; preferably 0.1-0.2 or less. The COF is a ratio of the frictional force resisting movement of an object tangentially to a surface and the force pushing the object into the surface (or normal force). Mathematically, it can be expressed by the formula:
μ= F f ÷F n
wherein μ is the COF, F f is the frictional force resisting movement of an object tangentially to a surface, and F n is the normal force.
[0122] By way of example, the COF for cartilage on cartilage is 0.001, metal on normal cartilage is 0.05 (but note the COF escalates for metal on degenerative cartilage to 0.25 (Covert, 2001)), metal on bone is 0.5, metal on polyethylene is 0.1, metal on metal is 0.5, and metal on Teflon™ is 0.02. COF lowers with wettability, indicating a layer of fluid between surfaces decreases friction.
[0123] Suitable, but non-limiting, examples of low friction material include metal; metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative); ceramics; ceramic-coated material; polymers, optionally reinforced with fiber; pyrolitic carbon coated material; carbon composites; and diamond-coated material. Preferred examples include stainless steel, cobalt-chrome alloy, titanium; titanium- and zirconium-based Liquidmetal® alloy; alumina, zirconium oxide; polyetheretherketones, polyetherketoneketones, polyaryletherketones, polysulfones; P25-CVD. Still more preferred examples include stainless steel, cobalt-chrome alloy, titanium, zirconium-based Liquidmetal® alloy, zirconium oxide, polyetheretherketones, polyetherketoneketones, polyaryletherketones, polysulfones, and P25-CVD.
[0124] Cobalt-chrome alloy has been used in joint replacement for over 30 years. It is the most common bearing surface in joint replacement surgery due to its strength, durability, biological tolerance, low reactivity, and relatively low friction articulation against polyethylene, the most common material against which it articulates. In spite of cobalt-chrome's long-term success, there are drawbacks to the use of this material. Cobalt-chrome articulating against polyethylene generates a low, but significant, amount of friction. In fact, it has been calculated by Bankston, et al. ( The Comparison of Polyethylene Wear in Machined vs. Molded Polyethylene , CORR, 317:37-43, August 1995), that the linear wear rate for compression molded polyethylene is 0.05 mm/year and 0.11 mm/yr for ram extruded polyethylene, when cobalt-chrome is used with polyethylene.
[0125] Another class of low friction material used in joint replacement surgery is ceramics. The most common used are alumina and zirconia. Ceramics are advantageous over cobalt-chrome in that the wear rate against polyethylene is only 1-10% that of cobalt-chrome; the wear rate of ceramic on ceramic is even lower. Thus, ceramic surfaces have the potential for long term success with little wear. The problem with ceramics is their relative brittleness and potential for breakage. With advances in ceramic materials technology this problem has been nearly eliminated in hip replacement surgery, where the ceramic replacement of the femoral head and/or acetabular cup has shown little potential for breakage. However, due to the geometry of the knee joint and the difference in how forces are transmitted in the knee, ceramics have not found a role as joint replacement material for the knee joint.
[0126] A method is available in which a layer of zirconium oxide ceramic is formed on the surface of a zirconium metal alloy. The ceramic surface layer is desirable in that it exhibits lower friction and lower generation of heat at the articulating surface than metal alloy, yet the metal alloy maintains the strength, so that the relative brittleness of a zirconium ceramic is avoided. Several U.S. patents have been issued with regards to the zirconium oxide layer including U.S. Pat. Nos. 5,037,438, 5,180,394, and 6,447,550. Additionally, U.S. Pat. No. 6,206,927 discloses as an option that a steel-ceramic composite may be used instead of solid steel, (i.e. cobalt-chrome) for their UniSpacer™-type device.
[0127] An additional type of alloy that could be considered as the surface bearing material is currently being co-developed by DePuy and Liquidmetal® Technologies, Inc. Available data on their zirconium-based alloy suggests that it would have favorable properties for use as a surface bearing implant material. This includes hardness, low-friction, wear resistance, superior strength, and superior elastic limit. Representative patents for this type of material include U.S. Pat. Nos. 5,288,344 and 5,368,659 (to Caltech) and U.S. Pat. Nos. 5,567,251, 5,567,532, 5,866,254, and 6,818,078 to Liquidmetal® Technologies, Inc., all of which are incorporated by reference in their entirety.
[0128] The use of a diamond-coated surfaced has been demonstrated to exhibit a very low coefficient of friction; a diamond-like carbon (DLC) coating on cobalt-chrome metal has reduced wear of adjacent polyethylene. This is disclosed in U.S. Pat. No. 6,171,343, which claims the process of coating a metal alloy with DLC in order to further reduce friction. U.S. Pat. No. 6,800,095 is a representative patent for Diamicron, Inc. (Orem, Utah); Diamicron has several patents claiming a diamond surface in orthopedic implant devices. Lockheed Martin Corp. also has a diamond coating process that may be applied to biological implants. The use of a diamond coating is also described in U.S. Pat. No. 6,626,949 (to BioPro, Inc.).
[0129] Polyetheretherketone (PEEK) is a polymer that, with fiber reinforcement, results in a hard, durable, low-friction, low reactivity material. It has been mostly applied in spinal surgery where the material replaces titanium as an insert between vertebrae, giving stability and thus allowing for spinal fusion to occur. PEEK is one of several polymers, (others include polyetherketoneketone, PEKK, polyaryletherketone, PAEK, and polysulfones) that can be reinforced with fibers, such as carbon or glass, giving the polymers differing properties of strength, hardness, and flexibility. PEEK and related materials have been proposed for use in femoral implants and as intervertebral discs due to the capacity to achieve either a hard, low-friction surface or an elastomeric surface, depending on the fiber reinforcement pattern. The properties of low-friction, along with biocompatibility and strength, make PEEK and its related polymers potentially good candidates for use as material in the implant described herein. A hard outer composite can be mixed with a softer, more elastic, inner composite, which would confer the desired characteristics of the device herein, namely low-friction articulation and cushioning. The use of PEEK in orthopedic implants is represented by U.S. Pat. No. 6,673,075; furthermore, PEEK fibers have been developed by Zyex Corporation (Gloucester, UK).
[0130] Carbon-carbon composites have been suggested for use as material in orthopedic implants. This is due to their strength, biocompatibility, and low wear rates. One compound in particular, P25-CVD, exhibited a very low wear rate when tested for use as a total hip bearing.
[0131] Cobalt-chrome, ceramics and metal-ceramic composites all have a high modulus of elasticity (MOE) as compared to bone. This high MOE imparts inordinate stresses to the articulating bone. Zirconium alloy can be favorable over cobalt-chrome, for example, because its MOE is significantly lower. Cobalt-chrome's MOE is approximately 220 GPa, whereas zirconium alloy has a MOE on the order of 83-100 GPa; titanium has a MOE of approximately 110 GPa. All of these materials are far from subchondral bone, which has a MOE of approximately 2 GPa, whereas cortical bone has a MOE up to 17 GPa.
[0132] In order to find materials which better approximate the MOE of bone, implants made out of pyrolitic carbon have been described; however, they are limited to low-weight bearing joints such as the wrist. Pyrolitic carbon has a MOE between 10-35 GPa. While this overlaps that of cortical bone, it is still higher than that of subchondral bone. Nonetheless, a pyrolitic carbon implant could be advantageous due to its relatively low MOE. In fact, there are patents for pyrolitic carbon coated surfaces, such as U.S. Pat. No. 4,166,292, and for use of pyrolitic carbon as implant material, including U.S. Pat. Nos. 4,457,984, 5,534,033, 6,090,145, and 6,436,146.
[0133] In addition, pyrolitic carbon has a low coefficient of friction; one would expect low wear rates and low heat generation in the opposing articulating surface. This is supported by Kawalee, et al. ( Evaluation of fibrocartilage regeneration and bone response at full - thickness cartilage defects in articulation with pyrolitic carbon or cobalt - chrome alloy hemiarthroplasties . J. Biomed. Res., 1998, 41(4): 534-540), who demonstrate that pyrolitic carbon is better tolerated compared to cobalt-chrome when used as a surface bearing material for articulation with cartilage tissue or damaged cartilage tissue. Surface cracks were seen in only 14% of the cartilage surfaces articulating against carbon, but 100% had cracks when articulating against cobalt-chrome. Furthermore, cartilage defects had an 86% regeneration rate when articulating against carbon, but only a 25% regeneration rate when articulating against cobalt-chrome.
[0134] Due to its favorable MOE and low coefficient of friction, pyrolitic carbon, or implants coated with this material, could be used for joint implants. Pyrolitic carbon is used in joint implants currently, but this use is limited to the hand and wrist joints. This limitation is due to the fact that pyrolitic carbon is simply not strong enough for the larger weight bearing joints. Pyrolitic carbon has the propensity for undergoing cyclic fatigue because cyclic crack growth is possible in this material. Thus, stress is a limiting factor in the use of this material in a weight bearing function because of the potential for breakage and failure of the implant.
[0135] However, due to the stress dissipation properties of the cushioning component, pyrolitic carbon may be used as the low friction component material of the knee implant; because the pyrolitic carbon does not act as the weight-bearing material in the device, the potential for breakage and failure are greatly reduced.
[0136] The final type of low friction bearing surface relates to a biological surface. By this is meant a surface which is coated with a substance that resembles the normal cartilage surface. It is well known that hyaluronic acid (HA) acts as the lubricant in articulating cartilage and that the outer surface of cartilage has an HA coating, intermixed with the PG/collagen matrix. The negatively charged surface molecules and HA lubricant act to repel each other, thereby decreasing contact between adjacent cartilaginous surfaces; this repulsion results in a low friction articulation.
[0137] The use of low friction coatings in medical applications is not new. Most commonly, these consist of an HA coating. They are most often used as coatings for catheters, catheter introducers and tubes. When these devices are HA coated they slide easily within blood vessels and other body orifices. Patents representative of such coatings are U.S. Pat. No. 6,160,032 and U.S. Pat. No. 6,387,450. In addition, there are several products on the market which utilize a process for HA coating for a wide variety of uses. One such product is called Lubril AST™, (U.S. Pat. No. 6,238,799). This product is meant to decrease the COF down to 0.009, which is nearly as good as the best cartilage-on-cartilage articulations. Although it demonstrates durability, this test is performed under “mild conditions;” this may not be the same as in actual joint articulation. Another such product is called HYDAK™, which is a registered trademark of Biocoat. This product claims to have, in addition to thickness, wettability, lubricity and low friction, abrasion resistance, and stability in contact with body fluids. Furthermore, this product may be applied to many different types of materials including polyurethane, PMMA, ceramics, titanium, and more.
[0138] (b) Cushioning Material
[0139] In practicing the invention, the phrase “cushioning” means the ability to absorb and dissipate weight bearing loads by deformation; cushioning in the context of the present invention means a material possessing a modulus of elasticity (MOE) between about 0.1 and 50 MPa. The cushioning material of the present invention is also preferably elastomeric. Elastomeric materials are those that deform when stressed with a load, but return to their original shape when the load is removed. Common elastomeric materials include rubber, synthetic rubber or polymer, and/or plastics. By way of example, the MOEs of some materials include: polyvinylalcohol (PVA) 0.5-10 MPa, rubber ˜7 MPa, and cartilage ˜24 MPa. Suitable, but non-limiting, examples of cushioning material include polyurethane, polyvinylalcohol, polyacrlyamide, fiber-reinforced polymer, and a water retaining center comprising a hydrogel made from a material selected from the group comprising polyvinylalcohol or polyacrylamide, surrounded by a tight outer covering. Preferred examples include polyurethane and a water retaining center comprising a hydrogel made from a material selected from the group comprising polyvinylalcohol or polyacrylamide, surrounded by a tight outer covering.
[0140] The cushioning material of the present invention is optionally made out of an elastomeric compound. The types of compounds that can be used include those made of a single material, such as polyvinyl alcohol, polyurethane and polyacrylamide; alternatively a device constructed from more than one material may be used. This could include a hydrogel material, which is surrounded by a tight, non-elastic covering.
[0141] U.S. Pat. No. 6,224,630 discloses a device for use in vertebral disc repair. PVA is the preferred material, but the patent discloses many materials including polyurethane, polyethylene, polypropylene, etc. U.S. Pat. No. 5,458,643 discloses an artificial intervertebral disc made out of a PVA hydrogel, with a ceramic or metal porous body; it also discloses PVA for use as an artificial articular cartilage repair material. U.S. Pat. Nos. 5,981,826 and 6,231,605 describe PVA for use as tissue scaffolding.
[0142] SaluMedica is marketing a product called SaluCartilage™, which is meant to be a cartilage defect replacement material. Salucartilage is made from a PVA polymer; it is described in U.S. Pat. No. 6,231,605, by David Ku, who is also the CEO and President of SaluMedica. This product's mechanical properties are similar to those of articular cartilage and it is capable of withstanding repetitive loading typical of normal walking conditions. It apparently has a very low friction when articulating against an opposing cartilage surface. Although the mechanical properties and strength appear to be adequate, this substance, when used as a bearing surface, has a relatively high coefficient of friction (COF). Covert and Ku demonstrate (in vitro) (Covert, R. J., and Ku, D. N., Friction and wear testing of a new biomaterial for use as an articular cartilage substitute . BED-Vol. 50, 2001 Bioengineering Conference, ASME 2001) that although the COF of their PVA material appears to be high, 0.184 against bovine cartilage and 0.247 against damaged articular cartilage (for comparison, cartilage on cartilage: 0.01-0.02; metal-on-metal: 0.15-0.35; metal on UHMWPE: 0.05-0.15), this level of friction does not have a direct relationship with wear and should not be used to predict wear rates. Even though it is stated that wear rates may not be a problem in spite of the high friction, one would have to be skeptical until in vivo testing determined that the high friction levels did not cause any problems on the adjacent normal cartilage. Importantly, the SaluCartilage™ device is only being tested as a cartilage defect replacement material, and not as a knee spacer.
[0143] Polyacrylamide has been used for many years in the human body. It has been used as an injectable filler for wrinkles and lip augmentation, and, in the past, as a breast implant filler; thus it has been deemed safe for human implantation (U.S. Pat. No. 5,941,909 to Mentor Corp.; filler for implants such as breast or testicles).
[0144] A disc implant from RayMedica is a hydrogel surrounded by a constraining jacket. (U.S. Pat. No. 5,824,093.) The implant material is made out of acrylamide and acrylnitrile. The second option disclosed in this patent is to use PVA as the hydrogel core, surrounded by a jacket made out of high molecular weight polyethylene weave. The mechanism of action is similar to that of articular cartilage: the core hydrogel material absorbs and releases fluid, similar to the PG component of articular cartilage ECM. The outer “jacket” limits excessive fluid absorption, not unlike the collagen type II effects in cartilage. This type of material, a core of hydrogel surrounded by an outer non-elastic material is proposed only for use in the spine as a disc replacement. There are no references to, nor any implications for, use elsewhere, as in the knee joint.
[0145] Polyurethane is well-known in industrial applications, i.e. wheels, etc., due to its favorable strength and wear properties. It is also known to be well-tolerated by the body, having been successfully employed as an implant for tendons, arteries, and veins.
[0146] In the early 1960 s polyurethane was used to replace the acetabulum, but due to the poor quality of polyurethane available at that time, the implants essentially fell apart, and polyurethane for use in joint replacement was abandoned. In 2001 Townley was issued U.S. Pat. No. 6,302,916, for the use of polyurethane as a material in joint replacement, i.e. tibial tray and acetabular cup. Townley discloses that the polyurethane essentially performs the same function as does UHMWPE in conventional TKAs; it acts as the bearing surface between the fixed femoral and fixed tibial components. It is stated in that patent that the polyurethane has similar, if not better, wear properties than UHMWPE. An additional advantage is that polyurethane can be heat treated, whereas UHMWPE cannot, and thus it can be heat sterilized. It also has a longer shelf-life. The patent does not disclose the use of polyurethane in a UKA; the patent additionally does not describe, nor does it imply, the use of polyurethane in a manner where the tibial or femoral components are unattached to bone. Furthermore, no advantage with respect to smaller incisions or increase in activity, such as running, are described or implied. Thus, the polyurethane is merely a substitute for UHMWPE, with no further advantages such as smaller incision size, less surgical dissection, fewer bone cuts, or an increase in post-operative activity, as compared to a standard TKA using UHMWPE as the bearing surface against metal.
[0147] U.S. Pat. No. 6,248,131 to Felt, et al., discloses a polyurethane implant meant for intervertebral disc replacement. Because the polyurethane material articulates against degenerating cartilage with this device, it could be expected to demonstrate significant wear, and thus would not make an optimal implant due to the poor capacity as a low friction bearing material. Another patent issued to Felt, U.S. Pat. No. 6,652,587 discloses a knee implant, made out of an elastomeric material such as polyurethane, in which the tibial and femoral components are fixed to bone, unlike the present invention.
[0148] Impliant, Ltd. (Ramat Poleg, Israel) has developed a proprietary polycarbonate urethane compound for medical purposes. Specifically, they have developed a hip replacement implant, a femoral head replacement. This femoral prosthesis consists of a titanium stem for insertion into the femoral canal, similar to current femoral stems. A Morse taper is used on the neck component, onto which a titanium head can be attached, again, similar to other femoral head replacements. The implant is unique in that the titanium head is covered with an elastomeric component, which is meant to articulate against the adjacent acetabular cartilage. Prior femoral components do not have an elastomeric surface; rather the metal head articulates with the acetabular cartilage.
[0149] The Impliant elastomeric coating is a proprietary polycarbonate urethane material. Furthermore, the methods of manufacture and methods of attachment are also proprietary. This implant is meant for the hip only; the company literature gives no mention of a knee implant, even though it mentions other uses for polyurethanes in medical devices, including spinal disc implants, intra-aortic pumps, and pacemaker leads.
[0150] Impliant has described elastomeric implants in WO 2004/014261 (femoral head prosthesis), and WO 03/047470 (hip, shoulder, knee implants). With respect to the knee, the Impliant invention describes a meniscal replacement type of prosthesis; it is not used as an implant for arthritic joint replacement. Indeed, because the implant is C-shaped the center part allows for opposing joint surfaces to make contact, unlike the invention disclosed herein.
[0151] Of the above materials, polyurethane holds the most promise, stemming from its favorable rheological properties, tolerance by the body as an implant, low wear rate, and overall strength. A more physiological cushioning represented by an acrylamide hydrogel and with an inelastic outer covering is also a good option.
[0152] Manufacturing of the FLFC involves CAD/CAM (computer assisted design/computer assisted manufacturing) techniques. The overall shape of each femoral condyle for humans can be determined for numerous sizes, with a range of individuals from 90 lbs. to over 300 lbs. One millimeter to 1½ mm increments in the overall size of the implants can be used to provide all of the varying size ranges in humans. CAD/CAM techniques are used to create molds for these sizes. The implants can then be made within these molds and polished as needed. When the use of molds is not practical, CAD/CAM techniques can be used to machine the implants from a solid block. The machined implants are then polished as needed.
[0153] The CC is manufactured as described by prior art. U.S. Pat. No. 6,302,916, to Townley describes proprietary polyurethane, while U.S. Pat. Nos. 6,306,177 and 6,652,587 (to Advanced Bio-Surfaces, Inc.) describe a method of manufacturing a polyurethane implant. Impliant, Ltd. (Netanya, Isreal) is a company with a proprietary polyurethane material currently being used for a femoral head prosthesis. The Impliant material is described in numerous PCT patents, as represented by WO 03/047470. Alternative cushioning materials include PVA, which is described in U.S. Pat. No. 6,231,605, and PEEK, which involves the inclusion of a fiber mesh within the PEEK material in order to generate elastomeric properties.
[0154] The shape of the cushioning material is such that it matches each different size of the low friction implant. Mechanical interlocking is used to ‘lock’ and stabilize the cushioning material into the low friction portion of the implant.
[0155] In one embodiment of the present invention, a prosthetic device is provided as a single structure, comprising two components: an upper low friction layer and a lower cushioning layer. It is intended that the prosthetic not be attached to the tibia. The upper layer is made out of a low friction material. Bound to the undersurface of the upper layer is the elastomeric cushioning component (CC). The upper, low friction layer is called the femoral low friction component (FLFC). It is contoured to match the shape of the femoral condyle. The CC, which is made out of an elastomeric material, is contoured on its superior surface to the exact dimensions of the undersurface of the FLFC in order that the two could be attached. The undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry. For example, FIG. 1 shows a perspective view of a representative two-piece construct. There is a top, or superior, piece ( 1 ), the FLFC (femoral low-friction component), that is made out of a low friction material. Its shape conforms to that of the femoral condyle. This shape resembles the general shape of the meniscus cartilage, but instead of forming a “C” shape with an open central/inner portion as in the normal meniscus, the central or inner portion is solid. The front (anterior) ( 2 ), back (posterior) ( 3 ), and side (lateral) ( 4 ), portions are raised to provide for some stability and also to add to the total surface area where weight load is transferred. The radius of curvature is equal to and/or preferably slightly greater than that of the opposing femoral condyle. Furthermore, the posterior portion is generally wider than is the anterior portion. The undersurface is attached to the elastomeric cushioning component ( 5 ). The CC ( 5 ) may be attached to the FLFC ( 1 ) by mechanical interdigitation, molecular fixation or glue. Mechanical interdigitation can include any one of a number of locking mechanisms, with or without the use of a separate ring or pin device that acts as the locking agent. Furthermore, the entire two-component construct may optionally be manufactured together, or the pieces may be manufactured separately where the surgeon attaches them together at the time of surgery. In this latter option a simple snap on mechanism may be used for attachment of the two components.
[0156] In an aspect of this embodiment, the FLFC is made from a material selected from the group comprising metal, metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative), ceramic, glass, carbon composites, polymers, ceramic-coated surface materials, diamond-coated surface materials, pyrolitic carbon-coated surface materials.
[0157] In another aspect, the FLFC is made from metal. In a preferred aspect the metal is selected from the group comprising stainless steel, titanium, cobalt-chrome alloy.
[0158] In yet another aspect, the FLFC is made from ceramic. In a preferred aspect the ceramic is selected from the group comprising alumina, zirconium oxide.
[0159] In yet another aspect, the FLFC is made from carbon composite. In a preferred aspect the carbon composite is P25-CVD.
[0160] In yet another aspect, the FLFC is made from a polymer. In a preferred aspect the polymer is selected from the group comprising polyetheretherketone, polyetherketoneketone, polyaryletherketone, polysulfone.
[0161] In yet another aspect, the FLFC is made from a polymer optionally reinforced with fiber.
[0162] In yet another aspect, the FLFC is made from pyrolitic-carbon coated material.
[0163] In yet another aspect, the FLFC is made from a ceramic-coated material.
[0164] In yet another aspect, the FLFC is made from a diamond-coated material.
[0165] In yet another aspect, the FLFC is made from glass.
[0166] In yet another aspect, the FLFC is made from metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative). In a preferred aspect the alloy is selected from the group comprising titanium-based Liquidmetal® alloy or zirconium-based Liquidmetal® alloy. In an even more preferred aspect the alloy is zirconium-based Liquidmetal® alloy.
[0167] In another aspect, the CC is made from an elastomeric material selected from the group comprising polyurethane, polyvinylalcohol, polyacrlyamide, fiber-reinforced polymer. In a preferred aspect the CC is made from polyurethane.
[0168] In yet another aspect, the CC is made from a capsule comprising a water retaining center surrounded by a supportive outer covering. In a preferred aspect the water retaining center is made from hydrogel material selected from the group comprising polyacrylamide and polyvinylalcohol. For example, FIG. 8A shows a representative hydrogel/tight outer coating option for the prosthesis. The superior surface has a FLFC as disclosed above. The undersurface has a TLFC, as disclosed above. The CC, instead of being composed of one elastomeric material, may consist of two parts: an inner hydrogel component and an outer water-permeable synthetic fiber component ( 14 ). The hydrogel has an affinity for water and will attract water inside, as noted by ( 15 ) in FIG. 8A . This constant inward flow of water puts outward pressure on the outer coating ( 14 ) and both the FLFC ( 1 ) and the TLFC ( 11 ), as depicted by the arrows inside the component. This constant inward flow of water is resisted by the outer coating ( 14 ). The inward force is constant because the outer coating is made smaller/tighter than the full expansile extent of the inner hydroge. This inward force is responsible for the cushioning effect. FIG. 8B demonstrates what would happen if the hydrogel ( 16 ) were not surrounded by the outer coating. Here the unimpeded inward flow of water causes the hydrogel to expand to a much larger size. The inward and outward water flow pressures equilibrate ( 17 ). FIG. 8C demonstrates what occurs with weight loads. The weight load ( 18 ) causes the thickness of the cushioning component to decrease ( 19 ). The outward flow of water increases beyond the inward flow ( 20 ). The inward flow of water, along with the tension created in the outer coating of fibers, resists complete outward flow of water. This resistance and the inward and outward flow of water are responsible for the cushioning properties. This mimics what occurs in normal hyaline cartilage, where cushioning is also provided by the inward and outward flow of water. In normal hyaline it is the PG portion of the matrix that acts as the hydrogel, attracting water into the matrix. The type II collagen fibers of the matrix resist tension, just as does the outer fibrous coating of the implant. The hydrogel may be composed of an acrylamide or PVA. The outer coating may be composed of non-elastic fibers, such as polyethylene. One skilled in the art will recognize that other materials will possess properties making them appropriate or desirable materials for use in the outer coating.
[0169] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by the entire periphery of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments. In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by only a portion of the periphery of the implant, including the anterior, medial/lateral, and/or posterior portion(s) of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments. FIG. 2 is representative of the manner by which the periphery of the CC is to be attached to the menisco-tibial ligaments, with an area for initial suture attachment and later permanent fibrous ingrowth. The rim ( 7 ) of the CC ( 5 ) has a collagen ingrowth coating ( 7 ). Rings ( 8 ), or a suitable alternative, may be used for suture fixation, which gives initial stability before fibrous ingrowth takes place.
[0170] In yet another aspect, the prosthesis is suitable for initial attachment to surrounding soft tissue by glue or sutures.
[0171] In yet another aspect, the CC further comprises a porous collagen ingrowth coating to facilitate permanent attachment via fibrous ingrowth. FIG. 6 shows the CC outer rim for initial biodegradable suture attachment and permanent fibrous ingrowth ( 9 ).
[0172] In yet another aspect, the FLFC is contoured to approximate the shape of the femoral condyle.
[0173] In yet another aspect, the FLFC has a radius of curvature equal to or larger than that of the femoral condyle against which it is intended to articulate. It is preferred that the FLFC has a radius of curvature greater than that of the femoral condyle against which it is intended to articulate.
[0174] In yet another aspect, the CC is contoured to exactly match the undersurface of the FLFC.
[0175] In yet another aspect, the CC is slightly larger than the FLFC. FIG. 6 shows an example of both of these aspects: the CC ( 5 ) may glide (see arrows pointing how the CC glides back and forth in the lateral view) on top of the tibial articular surface, guided by the attached menisco-tibial ligaments ( 10 ). The size of the CC is chosen so that it may articulate with the underlying tibial articular surface and with numerous different sizes of the attached FLFC.
[0176] In yet another aspect, the CC is attached to the FLFC by mechanical interdigitation, glue, or other bonding method.
[0177] In yet another aspect, the CC is attached to the FLFC prior to packaging.
[0178] In yet another aspect, the CC is attached to the FLFC immediately prior to implantation. In a preferred aspect the method of attachment of the CC to the FLFC is by a snapping mechanism.
[0179] In yet another aspect, the prosthesis comprising a single structure, of three components: an upper low friction layer, a middle cushioning layer and a lower low-friction layer; wherein it is intended that the prosthetic not be attached to the tibia or the femur; the upper layer is made out of a low friction material; bound to the undersurface of the upper layer is the elastomeric cushioning component (CC); the upper, low friction layer is called the femoral low friction component (FLFC); it is contoured to match the shape of the femoral condyle; the CC, which is made out of an elastomeric material, is contoured on its superior surface to the exact dimensions of the undersurface of the FLFC in order that the two could be attached; the undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface; the contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry; further comprises a tibial low friction component (TLFC), said component being attached to the undersurface of the cushioning component. For example, the CC may optionally have a low friction material attached to its undersurface. In this way the tibial articular surface articulates against a low friction bearing surface, rather than against the CC material, where there is the potential for wear of the CC component. FIG. 5 demonstrates a perspective view of the representative single unit as a three-piece combined construct. Here there is a top, superior, piece ( 1 ), the FLFC. The components may be manufactured as one single unit, or they may be separate pieces that are put together by the surgeon at the time of surgery. The CC has an outer rim for initial biodegradable suture attachment ( 7 ) and for later permanent fibrous ingrowth ( 7 ). The tibial low friction component, TLFC ( 11 ) may be attached to the undersurface of the CC. Its superior surface is the same size and shape as the undersurface of the CC. If attached, it is attached to the CC just as the FLFC is attached. The undersurface, or lower surface, of the TLFC is relatively flat to coincide with the tibial articular surface. Alternately, the under surface may be gently curved as is the tibial surface. This implant is inserted between the two articular surfaces just as in FIG. 3 .
[0180] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit by mechanical interdigitation, glue, or other bonding method.
[0181] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit prior to packaging.
[0182] In yet another aspect, the TLFC is attached to the cushioning component-femoral low friction component unit immediately prior to implantation. In a preferred aspect the method of attachment of the TLFC to the CC is by a snapping mechanism.
[0183] In yet another aspect, the prosthesis components are optionally coated with hyaluronic acid. The hyaluronic acid coating may be applied to the hard, low friction components (FLFC and/or TLFC), to the cushioning elastomeric component, or both types of components; this is depicted in FIG. 9 .
[0184] In yet another aspect, the FLFC is suitable for attachment to the femoral condyle. In a preferred aspect the FLFC is suitable for attachment to the femoral condyle by bone cement or by use of a porous coating, and/or hydroxy-apatite coating on the implant which allows for bone ingrowth into the implant. FIG. 6 demonstrates a lateral view of representative attachment of the FLFC ( 12 ) to the femoral condyle. It may be attached by either the use of bone cement or by bone ingrowth into a porous coated attachment surface on the FLFC ( 12 ). Pegs ( 13 ) are added in order to increase fixation stability of the implant into the femoral bone. The bone is cut according to a guiding jig. The proper sized component is inserted into place where it fits with contact on all attachment surfaces.
[0185] In yet another aspect, the FLFC is coated with an elastomeric or cushioning material (e.g. polyurethane).
[0186] In another embodiment of the present invention, a prosthetic device is provided as two components which are not attached to each other: an upper low friction layer and a lower cushioning layer. It is intended that the prosthesis not be attached to the tibia, but one component is attached to the femur. The upper layer is made out of a low friction material; its superior surface is made to attach to the femoral condyle. The upper, low friction layer is called the femoral low friction component (FLFC). Below the upper layer is the elastomeric cushioning component (CC); its upper surface is contoured to match the shape of the overlying FLFC, against which it articulates. The undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry.
[0187] In an aspect of this embodiment, the FLFC is made from a material selected from the group comprising metal, metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative), ceramic, glass, carbon composites, polymers, ceramic-coated surface materials, diamond-coated surface materials, or pyrolitic carbon-coated surface materials.
[0188] In yet another aspect, the FLFC is made from metal. In a preferred aspect the metal is selected from the group comprising stainless steel, titanium, or cobalt-chrome alloy.
[0189] In yet another aspect, the FLFC is made from ceramic. In a preferred aspect the ceramic is selected from the group comprising alumina, or zirconium oxide.
[0190] In yet another aspect, the FLFC is made from carbon composite. In a preferred aspect the carbon composite is P25-CVD.
[0191] In yet another aspect, the FLFC is made from a polymer. In a preferred aspect the polymer is selected from the group comprising polyetheretherketone, polyetherketoneketone, polyaryletherketone, or polysulfone.
[0192] In yet another aspect, the FLFC is made from a polymer optionally reinforced with fiber.
[0193] In yet another aspect, the FLFC is made from pyrolitic-carbon coated material.
[0194] In yet another aspect, the FLFC is made from a ceramic-coated material.
[0195] In yet another aspect, the FLFC is made from a diamond-coated material.
[0196] In yet another aspect, the FLFC is made from glass.
[0197] In yet another aspect, the FLFC is made from metal alloy with an amorphous atomic structure (of which Liquidmetal® alloys from Liquidmetal® Technologies of Lake Forest, Calif. are representative). In a preferred aspect, the alloy is selected from the group comprising titanium-based Liquidmetal® alloy or zirconium-based Liquidmetal® alloy. In an even more preferred aspect the alloy is zirconium-based Liquidmetal® alloy.
[0198] In yet another aspect, the CC is made from an elastomeric material selected from the group comprising polyurethane, polyvinylalcohol, polyacrlyamide, or fiber-reinforced polymer. In a preferred aspect the CC is made from polyurethane.
[0199] In yet another aspect, the CC is made from a capsule comprising a water retaining center surrounded by a supportive outer covering. In a preferred aspect, the water retaining center is made from hydrogel material selected from the group comprising polyacrylamide and polyvinylalcohol.
[0200] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by the entire periphery of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0201] In yet another aspect, the prosthesis is suitable for attachment to surrounding soft tissue by only a portion of the periphery of the implant, including the anterior, medial/lateral, and/or posterior portion(s) of the implant. In a preferred aspect, the prosthesis is attached to the menisco-tibial ligaments.
[0202] In yet another aspect, the prosthesis is suitable for initial attachment to surrounding soft tissue by glue or sutures.
[0203] In yet another aspect, the CC further comprises a porous collagen ingrowth coating that facilitates permanent attachment via fibrous ingrowth.
[0204] In yet another aspect, the femoral condyle is cut to exactly match the superior surface of the FLFC, which is suitable for binding with bone cement.
[0205] In yet another aspect, the femoral condyle is cut to exactly match the superior surface of the FLFC, which is porous coated or hydroxy-apatite coated to allow for bone ingrowth.
[0206] In yet another aspect, the undersurface of the FLFC is polished in order to generate a low friction surface.
[0207] In yet another aspect, the CC is contoured to exactly match the undersurface of the FLFC.
[0208] In yet another aspect, the CC is slightly larger than the FLFC.
[0209] In yet another aspect, the prosthesis comprising two components, which are not attached to each other: a separate upper low friction component, and a single lower component consisting of two materials, a superior cushioning layer which is attached to a lower low-friction layer; wherein it is intended that the prosthetic not be attached to the tibia, but one component is attached to the femur; the upper low friction component is made out of a low friction material. Its superior surface is made to attach to the femoral condyle. The upper, low friction component is called the femoral low friction component (FLFC). Below the upper FLFC layer is the superior part of the lower component, consisting of an elastomeric cushioning component (CC). Its upper surface is contoured to match the shape of the overlying FLFC, against which it articulates. The undersurface of the CC is generally flat with a slight convexity, in order to coincide with the relatively flat, slightly convex tibial articular surface. The contour is given a slight variation in order to better mimic the shape of the medial vs. the lateral tibial surface geometry; further comprises a tibial low friction component (TLFC), said superior surface of said component being attached to the undersurface of the cushioning component.
[0210] In yet another aspect, the TLFC is attached to the cushioning component by mechanical interdigitation, glue, or other bonding method.
[0211] In yet another aspect, the TLFC is attached to the cushioning component prior to packaging.
[0212] In yet another aspect, the TLFC is attached to the cushioning component immediately prior to implantation. In a preferred aspect, the method of attachment of the TLFC to the CC is by a snapping mechanism.
[0213] In yet another aspect, the prosthesis components are optionally coated with hyaluronic acid.
[0214] In yet another aspect, the FLFC is suitable for attachment to the femoral condyle. In a preferred aspect, the FLFC is suitable for attachment to the femoral condyle by bone cement or by use of a porous coating, and/or hydroxy-apatite coating on the implant which allows for bone ingrowth into the implant.
[0215] In yet another aspect, the FLFC is coated with an elastomeric or cushioning material (e.g. polyurethane).
[0216] In yet another embodiment, there is provided a method of providing a knee prosthesis to a patient in need thereof, said method comprising: ascertaining the size and shape of the required prosthesis and components thereof by examination of the patient; and providing to the patient a prosthesis according to the present invention.
[0217] In yet another embodiment, there is provided a method of knee reconstruction of a patient in need thereof, said method comprising: determining the proper size and shape of a prosthesis and components thereof according to the present invention, by examination of the patient; selecting the prosthesis according to the present invention of said proper size and shape; exposing the knee compartment; and implanting the knee prosthesis into the compartment. The tibial articular surface may at times have irregularities. The tibial spines, which are located toward the center of the joint, may at times encroach upon the medial or lateral compartment. It is within the scope of this invention that the tibial articular surface may have to be shaved, or straightened out, in order to obtain proper and optimal prosthetic gliding without impingement upon the spines.
[0218] In yet another embodiment there is provided a method of making a prosthesis of the present invention comprising CAD/CAM design of molds for casting the prosthesis component.
[0219] In yet another embodiment there is provided a method of making a prosthesis of the present invention comprising CAD/CAM techniques to directly machine the components from blocks of material.
[0220] In yet another embodiment there is provided a kit for treating arthritis of the knee comprising a prosthesis of the present invention and means for implanting said prosthesis.
[0221] In yet another embodiment there is provided a method of implanting the prosthesis of the present invention, wherein the prosthesis is inserted between the femoral and tibial surfaces. FIG. 3 demonstrates a frontal view of a representative manner by which the implant may be inserted between the femoral and tibial articular surfaces. Fibrous ingrowth from the peripheral menisco-tibial ligaments ( 10 ) is demonstrated ( 9 ). FIG. 4 is a lateral view of a representative manner by which the implant is inserted between the femoral and tibial articular surfaces.
[0222] In yet another embodiment, numerous sizes of the components are provided so as to provide a prosthetic device appropriate for a given patient. | A knee prosthesis, methods of implanting the prosthesis, method of treating arthritis of the knee, and a kit therefore are provided. The prosthesis answers many of the limitations of current knee prosthetic devices by providing a two-component (or alternatively, an optional three-component) device, as either a single structure, or as separate pieces. One of the components is constructed of low friction material, while the second is composed of a weight-dissipating cushioning material; the optional third component is constructed of low friction material. The prosthesis is initially attached to surrounding soft tissue in the knee by biodegradable sutures; it is held permanently in place by fibrous ingrowth into a porous collagen rim in the cushioning component. Major improvements provided by the present invention over currently available prostheses include minimal incisions, minimal or no bone cuts, minimal overall dissection (these improvements lead to shorter hospital stays and rapid rehabilitation and fewer potential for side effects), less prosthetic wear, greater longevity, fewer activity restrictions, able to be used on young, large, active patients, ease of revision, ease of conversion into a total knee arthroplasty if needed. | 0 |
This application is a continuation of now abandoned application Ser. No. 760,978, filed July 31, 1985 now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a device for detecting the residual amount of bobbin thread in a sewing machine and, more particularly, to a device of the type which is simple in arrangement and permits easy detection of the residual amount of such thread.
2. Description of the Prior Art
Generally, in lock stitch sewing machines, a bobbin on which is wound a bobbin thread is placed in a bobbin case, which in turn is mounted to a shuttle disposed below a bed, which in fact prevents a visual observation of the condition of the bobbin thread in the bobbin. Therefore, it is impossible to know the residual amount of bobbin thread at any time during a sewing operation, and accordingly, sewing is continued until the bobbin thread has run out, that is, until stitches can no longer be formed.
Consequently, a fresh supply of bobbin thread is provided only after sewing is discontinued. Such a lock stitch sewing machine is particularly unsuitable for use in sewing a portion of a workpiece which requires continuous stitches. Indeed, operation of the machine has to be discontinued in the course of sewing, or the sewing work has to be redone from the beginning, which will result in a considerable decrease in sewing work efficiency. For this reason, various means have been proposed in order to permit checking of how much of the bobbin thread has been consumed. There are known sewing machines in which a phototube is used to optically or magnetically observe the surface of the bobbin below the bed. Such a sewing machine has a disadvantage in that components, such as the shuttle and bobbin case, often require special treatment and that the machine involves a high cost of manufacture. Another disadvantage is that operation may be rendered inaccurate by thread fraying, lubricating oil, and the like.
SUMMARY OF THE INVENTION
In order to overcome aforesaid problems, the invention has for its object the provision of a novel and improved device for detecting the residual amount of bobbin thread in a lock stitch sewing machine.
Another object of the invention is to provide a device for detecting the residual amount of such thread which is able to perform an accurate detection of the residual amount of bobbin thread in a lock stitch sewing machine.
With a view to accomplishing the aforementioned objects, a device for detecting the residual amount of bobbin thread in a lock stitch sewing machine according to the present invention comprises: a first means for detecting at least one of the number of rotations of an arm shaft and an oscillating shaft, and the number of cycles of vertically reciprocating movement of a needle bar while a lock stitch sewing machine comprising said arm shaft, oscillating shaft, and needle bar is operating, said first means outputting an output corresponding to the detected number; and a second means for detecting the residual amount of bobbin thread wound on a bobbin in a bobbin case based on the output from said first means and for comparing the detected residual amount of bobbin thread with a first predetermined value, said first predetermined value predetermined in dependence on the conditions of thread and needle employed, and of the workpiece.
In a preferred embodiment, said second means causes the lock stitch sewing machine to stop operating when the detected residual amount of bobbin thread reaches said first predetermined value.
In another preferred embodiment, said second means comprises a light emitting indication element, said light emitting indication element being lit up when the detected residual amount of bobbin thread reaches a second predetermined value which is larger than said first predetermined value at which the lock stitch sewing machine is caused to stop operating.
In still another preferred embodiment, said light emitting indication element remains lit up until the detected residual amount of bobbin thread reaches said first predetermined value at which the lock stitch sewing machine is caused to stop operating.
In a further preferred embodiment, said second means comprises a sounding means, said sounding means being actuated to sound when the detected residual amount of bobbin thread reaches a second predetermined value which is larger than said first predetermined value at which the lock stitch sewing machine is caused to stop operating.
Preferably said sounding means remains actuated to sound until the detected residual amount of bobbin thread reaches said first predetermined value at which the lock stitch sewing machine is caused to stop operating.
In accordance with the invention, the detection of the residual amount of bobbin thread is positively effected at a low-cost.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects, features and advantages of the invention will become more apparent upon a reading of the following detailed specification and drawings, in which:
FIG. 1 is a general perspective view showing an embodiment of the invention;
FIG. 2 is a block diagram showing an electrical arrangement of the embodiment of the invention;
FIG. 3 is a flowchart illustrating the procedures for the arrangement of FIG. 2;
FIG. 4 is a general perspective view of another embodiment of the invention;
FIG. 5 is a general perspective view of still another embodiment of the invention;
FIG. 6 is a block diagram showing an electrical arrangement of yet another embodiment of the invention; and
FIG. 7 is a flowchart illustrating the procedures for the arrangement of FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, the preferred embodiments of the present invention are described below.
FIG. 1 is a perspective view schematically showing a lock stitch sewing machine of an embodiment according to the present invention. In an upper portion of a machine body 1 there is provided an arm shaft 2 to which is fixed a pulley 3 known as hand wheel. A needle bar 4 is interlocked with the arm shaft 2 to perform the vertically reciprocating motion. A shuttle 6 is mounted to an oscillating shaft 5 which is interlocked with the arm shaft 2. A needle 7 is mounted to the needle bar 4, with a needle thread passed through the needle 7. A bobbin having a bobbin thread wound thereon is mounted to the shuttle 6.
Now, it is assumed that when the bobbon is full, the amount of bobbin thread thereon is x cm. As the arm shaft 2 makes one rotation, the pulley 3 makes one rotation as well, and accordingly the needle bar 4 makes one cycle of vertically reciprocating movement, with the result that one stitch is formed. Assuming that the amount of bobbin thread consumed in forming one stitch, which is formed by one rotation of the pulley 3, is y cm, and that the number of rotations of the pulley 3 required in consuming one package of bobbin thread is α, the number of rotations α of the pulley 3 per package of bobbin thread is:
α=x/y (1)
Accordingly, the number of rotations β of the pulley 3 as made when such an amount as that except for z cm of bobbin thread has been consumed before the bobbin becomes empty, or when a residual amount z cm of bobbin thread is reached, is expressed by the following equation:
β=(x-z)/y (2)
During one rotation of the pulley 3, the arm shaft 2 also makes one rotation, the needle bar makes one cycle of vertically reciprocating movement, and the oscillating shaft 5 makes two rotations.
Inasmuch as certain conditions such as type of bobbin thread used, type of needle 7 used, type of workpiece as cloth, and pitch of or distance between stitches, are same, the amount of bobbin yarn x wound fully on a bobbin and the amount of bobbin yarn y required in forming one stitch are both almost constant. Where value z is set under these condition, the number of rotations β of the pulley 3 is directly proportional to (x-z)/y, and the aforesaid equation (2) thus holds true. In this way it is possible to know the residual amount of bobbin thread corresponding to the number of rotations β, and accordingly to stop the operation of the lock stitch sewing mahcine when the predetermined residual value z is reached.
Generally, cotton thread is wound on a bobbin to its fully winding capacity, whereas polyester thread is wound only 80% or so relative to the bobbin capacity. For example, if the bobbin is of an ordinary TA type for straight lock stitch sewing machines, the amount x of thread wound on the bobbin may be determined as being approximately 55-57 m in the case of cotton 60's, and as being approximately 53-54 m in the case of polyester thread 60's. The number of rotations of the pulley 3 required to consume the amount x of bobbin thread is approximately 17,000-20,000 when the thread is cotton, is approximately 18,000-20,000 when the thread is polyester. Therefore, if operation of the sewing machine is to be stopped before the bobbin thread is completely consumed, a value for the residual amount z of bobbin thread may be set at a level corresponding to 500-1,000 rotations of the pulley, for example, and accordingly the operation of the lock stitch sewing machine may be stopped when the number of rotations of the pulley 3 has reached 16,500 or so in the case of cotton thread, or 17,500 or so in the case of polyester thread.
FIG. 2 shows a block diagram of an embodiment for detecting such a residual amount of bobbin thread in accordance with the present invention. The pulley 3 has an optical reflective piece 8, such as aluminum foil, fixed thereto. The reflective piece 8 is detected by an optical detector element 10. The optical detector element 10 emits light to the pulley 3 and detects reflected light from the reflective piece 8. An output from the detector element 10 is supplied through a flexible line 16 to a counter 11 by which it is counted. The machine body 1 is provided with key input means 12 which have numbers 0-9 and other pushbuttons for motion control. Signals from the counter 11 and key input means 12 are input to a processing circuit 13 incorporating a microcomputer or the like. Through the operation of the processing circuit 13, an indicator 14 indicates a residual amount of bobbin thread corresponding to an integrated number of rotations of the arm shaft 2, pulley 3, and oscillating shaft 5. The operation of a motor 15 is controlled through an output from the processing circuit 13. The motor 15 actuates the arm shaft 2, pulley 3, and oscillating shaft 5.
In a casing 17 are housed the counter 11, key input means 12, processing circuit 13, and indicator 14. The processing circuit 13 is connected to the motor 15 through the flexible line 18. The casing 17 is preferably of such size as may be gripped by one hand and is of a socalled desk top type electronic calculator construction.
The manner of operation of the processing circuit 13 and the associated components will now be explained with reference to FIG. 3. Operation proceeds from step n1 to step n2, at which the value of key input is read. Values corresponding to predetermined conditions as shown in Table 1 below are input into the processing circuit 13 by the key input means 12.
TABLE 1______________________________________ Size of bobbin thread (count) 50 60______________________________________Material of Cotton thread Z1 Z2 . . .bobbin thread Polyester thread Z3 Z4 . . . . . .______________________________________
The value shown in Table 1 corresponds to the residual amount of bobbin thread z (z represents z1-z4 collectively) at which the run of the motor 15 is to be stoppped to stop operation of the lock stitch sewing machine. As stated above, the bobbin mounted to the shuttle 6 has a bobbin thread wound fully thereon, if the thread is cotton, or a bobbin thread wound 80% or so relative to the winding capacity of the bobbin, if the thread is polyester. The residual amount of bobbin thread z at which the motor 15 is to be stopped depends upon such factors as material and size of the bobbin thread. At step n3, the number of rotations of the pulley 3 as detected by the detector element 10 is read. At step n4, a residual amount of bobbin thread corresponding to the number of rotations is calculated. At step n5, the residual amount of bobbin thread is indicated by the indicator 14. At step n6, detection is made as to whether the number of rotations corresponding to the predetermined amount of bobbin thread z has been reached or not, and if the detection is affirmative, operation proceeds to step n7, at which the run of the motor 15 is stopped.
At the indicator 14, the residual amount of bobbin thread corresponding to the number of rotations may be indicated in absolute value, or may be indicated in terms of converted value as calculated against the initial amount of bobbin thread taken as 100 or 1000 and the completely consumed state of bobbin thread taken as zero. In another embodiment, arrangement may be made such that the number of rotations is detected of the arm shaft 2 or of the oscillating shaft 5, or the number of cycles of vertically reciprocating movements of the needle bar 4 is detected. For the purpose of detection, magnetic or other suitable means may be used instead of the optical detector element 10.
FIG. 4 is a general perspective view showing another embodiment of the invention. In an upper housing 19 there are mounted key input means 12 and indicator 14, both exposed outside. The counter 11 and processing circuit 13 are contained in the housing 19. The detector element 10 is connected to the counter 11, and the processing circuit 13 is connected to the motor 15. These and other connections are made within the housing 19.
FIG. 5 is a general perspective view of a still another embodiment of the invention. In this embodiment, the detector means 10, counter 11, key input means 12, processing circuit 13, and indicator 14 are all housed in a casing 20, which is removably tied to the housing 19 by means of a mounting belt 21 so that the detector element 10 is positioned so as to face the reflective piece 8. According to this embodiment, the invention may be applied to an existing sewing machine with substantial improvements not being made in the latter.
FIG. 6 is a block diagram showing yet another embodiment of the invention. The processing circuit 13 is connected to a light emitting diode 22 and also to a buzzer 23. The processing circuit 13 actuates the light emitting diode 22 to light up and the buzzer 23 to sound, during a time period of from the time that there is reached a predetermined value Z 0 (Z 0 >Z) which precedes the arrival of the residual amount of bobbin thread Z and at which sewing is still possible, to the time that the residual amount of bobbin thread Z is reached at which operation of the sewing machine is to be stopped.
By recognizing such a visual indication by the light emitting diode 22 and such acoustic indication by the buzzer 23, therefore, the operator engaged in sewing is able to know that a fresh supply of bobbin thread is needed. Thus, it is possible to replenish the supply of bobbin thread before the residual amount of bobbin thread z is reached and before the operation of the sewing machine is stopped, in order to prevent sewing operation from being stopped at an inconvenient sewing position. The predetermined value Z0 is input to the processing circuit 13 by the key input 12 in the same fashion as that of the predetermined value Z.
A decision as to whether or not the value Z 0 for bobbin yarn has been reached is made after steps m4 and m5 and before step m6, that is, at step m5a, as illustrated in the FIG. 7 flowchart. After the decision is made at step m5a that the value Z 0 has been reached, the light emitting diode 22 emits light and the buzzer 23 sounds at step m5b.
Steps m1-m5, m6, and m7 correspond respectively to steps n1-n5, n6, and n7 explained with reference to FIG. 3, and similar operations are performed in both series of steps.
The light emitting diode 22 and the buzzer 23 are both shown by virtual lines in FIGS. 1, 4, and 5. They are mounted on the casings 17 and 20 respectively shown in FIGS. 1 and 5, and on the upper housing 19 in FIG. 4.
The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description and all changes which come within the meaning and the range of equivalency of the claims are therefore intended to be embraced therein. | A device for detecting the residual amount of bobbin thread in a lock stitch sewing machine is arranged such that a detector detect the number of rotations of an arm shaft or oscillating shaft, or the number of cycles of vertically reciprocating movement of a needle bar of a lock stitch sewing machine including the arm shaft, and oscillating shaft, and needle bar. The detector provides an output for the detected of rotations. The residual amount of bobbin thread wound on a bobbin in a bobbin case is then detected based on the detected number of rotation output. The detected residual amount of bobbin thread is then compared with a predetermined value which is predetermined in dependence on conditions such as the thread and needle to be employed, and the workpiece. | 3 |
FIELD OF THE INVENTION
This invention relates generally to collapsible structures and more particularly to portable tents that are constructed to be easily constructed and collapsed.
BACKGROUND OF THE INVENTION
A variety of portable tents and similar collapsible structures have heretofore been known, includint those described in U.S. Pat. No. 6,209,557 Zheng), U.S. Pat. No. 5,038,812 (Norman), U.S. Pat. No. 5,467,794 (Zheng) and U.S. Pat. No. 5,560,385 (Zheng). These portable tents and similar collapsible structures may be used by children or adults for temporary shelter, camping, as beach cabanas, play houses, etc.
The ease with which portable tents or other collapsible structures may be constructed and collapsed is a significant factor that determines their desirability for use in applications that require rapid or frequent construction and collapsing or easy portability, such as when these collapsible structures are used as beach cabanas, temporary play houses or while hiking, backpacking, rock climbing, etc.
Also, two or more portable tents or other collapsible structures are sometimes used in conjunction with one another and, in at least some applications, it may be desirable to connect two or more portable tents or other collapsible structures to one another to facilitate easy passage of humans, animals or objects from the interior of one structure to the interior of another structure.
Although the portable tents and similar collapsible structures have included a number of different designs, no one prior design is believed to be optimal and their remains a need in the art for the development of new and different portable tents and similar collapsible structures that are useable in new ways or are more easily collapsed/constructed or more easily portable than those of the prior art.
SUMMARY OF THE INVENTION
The present invention provides a collapsible structure (e.g., a tent, cabana, play hose, etc.) that generally comprises a plurality of pole members, a flexible covering disposed on the pole members, a plurality of strut members that are connected to the pole members and a hub assembly having upper and lower hub members, the hub assembly being attached to the pole members and the strut members. The structure is alternately disposable in a) a constructed configuration wherein the lower hub member is in abutment with the upper hub member and the flexible covering is drawn taut between the pole members and b) a collapsed configuration wherein the lower hub member is a spaced distance below the upper hub member, the pole members are closer together than they are when the structure is in its constructed configuration and the flexible covering is loosely disposed between the pole members.
Further in accordance with the invention, the strut members may be configured to exert an upward bias on the hub assembly when the structure is in its constructed configuration, thereby holding the hub members in substantially fixed vertical positions relative to one another and preventing the structure form inadvertently collapsing during use. When downward pressure is applied to the hub assembly, the upward bias of the strut memebrs is overcome, thereby releasing the hub assembly, allowing the upper and lower hub members to separate from one another and allowing the structure to assume its collapsed configuration.
Still further in accordance with the invention, the hub assembly may incorporate or be provided with locking structure(s) which mechanically lock the upper and lower hub members together when the structure is in its constructed configuration. These locating structures may be unlocked when it is desired to convert the structure to its collapsed configurations, thereby allowing the upper and lower hub members to move apart from one another and allowing the structure to assume the desired collapsed configuration.
Still further in accordance with the present invention, there are provided systems for attaching a plurality of collapsible structures of the forgoing type (or of any other type) to one another to form a multiple-structure assembly comprising a plurality of collapsible structures that are interconnects or linked to one another. Openings are formed in the individual collapsible structures and tunnel members are attachable to those openings so as to link the individual structures together and to provide enclosed or partially enclosed passageways between the individual collapsible structures that make up the multiple-structure assembly.
Still further in accordance with the present invention, collapsible structures of the forgoing type (or of any other type) may be provided with decorative markings or decorative items to impart entertaining or desired appearance(s) to the structure. For example, collapsible structures my have the appearance of a character (e.g., an animal or cartoon character). The decorative markings may be situated such that a door or flap which provides for passage into and out of the collapsible structure is positioned within an opening of the decorative object (e.g., the mouth of an animal or fish, the opening of a cave or volcano, etc.), thereby giving rise to the appearance that children or other users of the structure are passing into the opening of the decorative object as the enter the collapsible structure. In multi-unit embodiments, the decorative markings formed on each individual unit of the multi-unit assembly may fit together to give rise to a single decorative object (e.g. an elongate animal such as a snake or eel).
Further aspects and elements of the present invention will be appreciable to those of skill in the art upon reading the detailed descriptions of embodiments set forth herebelow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a collapsible structure of the present invention in its fully constructed state.
FIG. 2 is a perspective view of the collapsible structure of FIG. 1 in its collapsed state, immediately after removal from its optional carrying case.
FIG. 3 is a perspective view of the collapsible structure of FIG. 2 in a partially constructed yet still partially collapsed state.
FIG. 4 is an enlarged view of portion 4 - 4 of FIG. 3 .
FIG. 5 is an enlarged view of portion 5 — 5 of FIG. 3 .
FIG. 6 is a perspective view of the top portion of the collapsible structure of FIGS. 1-5 in a nearly fully constructed state.
FIG. 7 is a perspective view of the top portion of the collapsible structure of FIGS. 1-5 in its fully constructed state.
FIG. 8 is sectional view taken vertically through the upper and lower hub members of the upper assembly of the collapsible structure shown in FIG. 1 .
FIG. 9 is another sectional view taken vertically through the upper and lower hub members of the upper assembly of the collapsible structure shown in FIG. 1 .
FIG. 10 is a sectional view taken vertically through the upper and lower hub members of the upper assembly of the collapsible structure shown in FIG. 1 while in its locked in its constructed configuration.
FIG. 11 is a sectional view taken vertically through the upper and lower hub members of the upper assembly of the collapsible structure shown in FIG. 1 after downward pressure has been applied to the upper hub member so as to cause the lower hub member to separate from the upper hub member and causing the structure to begin to transition from its constructed configuration to its collapsed configuration.
FIG. 12 is a collection of perspective views of multiple unit embodiments oc the persent invention with and without decorative markings formed thereon.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
The following detailed description is provided for the purpose of describing only selected embodiments or examples of the invention and is not intended to describe all possible embodiments and examples of the invention.
FIGS. 1 and 12 show an examples of a collapsible structures 10 of the present invention in their fully constructed configurations. As shown in FIG. 1 , each collapsible structure 10 generally comprises a) a support frame formed of a plurality of pole members 14 , a plurality of strut members 16 and upper and lower hub members 38 , 32 and b) a flexible covering 22 formed of woven nylon, plastic sheet or similar material. As shown in FIG. 12 , flexible covering 22 has a flap opening 21 , such flap 21 being securable in a closed position by a zipper 23 .
Optionally, as shown in FIG. 1 , a removable panel 24 may be formed in the flexible cover 20 to and such removable panel 24 may be secured to the flexible cover by a zipper 25 . When the removable panel 24 is removed and opening is formed in the flexible cover 22 of the collapsible structure 10 . As shown in FIG. 12 , and optional tunnel members 60 may be used in conjunction with two of the collapsible structures 10 that have optional removable panels 24 to form a multi-unit collapsible structure. The optional total member 60 preferably comprises a to the formed of flexible material such as woven by a line, plastic sheet or other suitable material. Zippers may be formed around the either end of the tunnel member 60 and may be mated or meshed with the portions of the zippers 25 that remainin on the flexible covers 22 of the collapsible structures 10 after their optional removable panels 44 have been removed. In this manner, one end of a tunnel member 60 may be connected to an opening formed in one collapsible structure 10 and the other end of that tunnel member may be connected to an opening formed in another collapsible structure 10 , thereby forming a multi-unit collapsible structure wherein the tunnel member 60 acts as a passageway between two collapsible structures 10 . Although the embodiments shown in FIG. 12 utilize only two collapsible structures 10 , it will be appreciated that more than one removable panel 24 may be formed in some collapsible structures 10 and three or more of the collapsible structures 10 may be joined by tunnel members 60 to form multi-unit collapsible structures of this invention that incorporate more than two of the individual collapsible structures 10 of the type shown in FIG. 1 .
Also, and shown in FIG. 12 , decorative markings 62 may be formed on the flexible covers 22 and/or on the optional tunnel members 60 to impart a desired appearance. These optional decorative markings 62 may be used on single-unit or multi-unit collapsible structures 10 of this invention and may be particularly desirable when the collapsible structures 10 are intended for use as children's beach cabanas, children's playhouses, doll houses or otherwise for the entertainment of children. In these types of applications, it may be desirable for the decorative markings 62 to impart the appearance of an insect or animal. In this regard, the decorative markings 62 may be in the nature of facial features such as eyes, nose and mouth and the opened mouth of the creature may appear around the entry flap 21 of a collapsible structure 10 to give the appearance of entering through the mouth of the creature as a child passes through the entry flap 21 .
The collapsible structures 10 of the present invention may be easily constructed and easily collapsed and folded to a stowable configuration. When in their fully collapsed states, the collapsible structures may be inserted in two caring cases or bags. A desired carrying case (not shown) comprises a light weight, woven nylon case that has carrying handles and a zipper for opening and closing the carrying case.
To fully appreciate the manner in which the collapsible structure 10 may be constructed and collapsed, it is helpful to consider and understand the components, design and function of the support structure and the manner in which the flexible cover 22 is disposed upon the support structure. The support structure generally comprises a plurality of pole members 14 , a plurality of strut members 16 which extend through loops 26 , a hub assembly 29 comprising an upper hub member 38 , a lower hub member 32 and an actuator 30 . The pole members 14 extend through elongate receiving channels 15 formed in the corners of the flexible cover 22 and the bottom ends of the pole members 14 are inserted into tabs 19 that are attached to and extend from the bottoms of the corners of the flexible cover 22 . Each tab preferably comprises a pocket formed of durable fabric and having an opening in its top edge such that the bottom end of a pole member 14 may be received within the pocket as shown in FIG. 5 . When the structure 10 is collapsed, as shown in FIGS. 2 and 3 , the pole members 14 are substantially straight, the upper and lower hub members 38 , 32 are separated and spaced apart, and the flexible cover 22 is loosely disposed. Also, hinged joints 20 , as shown in FIG. 4 , are formed in the pole members 14 approximately midway along their length. When the hinged joints 20 are extended as shown in FIG. 3 , they reside within the receiving channels 15 of the cover 22 between notches or cut out areas 66 formed in the fabric that defines the channels 15 . These hinged joints 20 may be folded over in the manner shown in FIG. 2 to further collapse the structure 10 . The presence of the notches or cut away areas 66 facilitates such folding of the pole members 14 at their hinged joints 20 by preventing the fabric of the cover 22 that forms the channels 15 from bunching or binding the hinged joints 20 .
The process of converting the collapsible structure 10 from its collapsed configuration shown in FIG. 2 to its constructed configuration shown in FIG. 1 begins with unfolding of the hinged joints 20 to convert the fully collapsed structure shown in FIG. 2 to a partially collapsed states as shown in FIG. 3 . Thereafter, with the bottom ends of the pole members 14 inserted into their receiving tabs 19 , the user may grasp the free ends of the two cords 34 , pulling them in opposite, horizontal, outward directions as illustrated in FIG. 6 . The cords 34 are knotted within the lower hub member 32 as shown in FIG. 8 . Thus, as the cords 34 are pulled outwardly, the lower hub member 32 will be drawn upwardly toward the upper hub member 38 such that the upper projecting portion 40 of the lower hub member 32 will be received within a bore or concavity 39 formed in the upper hub member 38 , and the upper and lower hub members 38 , 32 will be in abutting contact with one another. Also, as shown in FIG. 10 , when the lower hub member 32 reaches its uppermost position in full abutment with the upper hub member 38 , the inner ends IE of strut members 16 may be slightly elevated above the outer ends OE of the strut members 16 and such upward slanting of the strut members will serve to exert a biasing force in the upward direction against the lower hub member holding it in abutting contact with the upper hub member 30 even after the user releases the cords 34 . Also, as the tub members 38 , 32 are pulled into abutting contact with each other, the pole members 14 will bow to an arcuate configuration, giving the fully constructed structure 10 the configuration shown in FIG. 1 .
When it is desired to return the structure to its collapsed state, the user may simply push downwardly on the actuator knob 30 to flex the upper assembly 12 and poles 14 downwardly to a position where the inner ends IE of the strut members 16 are now lower than the outer ends OE of those strut members 16 . This results in a loss of the upward bias on the lower hub member 32 and allows the lower hub member 32 to separate from the upper hub member 30 , as shown in FIG. 11 . The structure may then be picked up vertically by the actuator knob 30 without constraining or preventing free retraction of the cords 34 and the structure will assume the partially collapsed configuration shown in FIG. 3 . Thereafter, the hinged joints 20 may be folded over to place the structure 10 in its fully collapsed state as shown in FIG. 2 . The fully collapsed structure may then be placed in an optional carrying case (not shown) or otherwise carried or transported with ease.
As shown in FIGS. 10 and 11 , when the hub assembly 29 is vertically situated, a hub axis, which in the drawings is shown as a vertical axis VA, is projectable through the center of upper and lower hub members 38 , 32 . Also, a strut axis SA is projectable through each of the strut members 16 . An internal angle A is definable between the strut axis SA and the vertical axis VA. When the structure 10 is locked in the constructed configuration shown in FIG. 10 , angle A is more than 90 degrees and the outer ends OE of the strut members 16 are lower than or below the inner ends IE of the strut members 16 . When the structure 10 is in the unlocked configuration shown in FIG. 11 (e.g., as it is being collapsed or constructed), angle A is less than 90 degrees and the outer ends OE of the strut members 16 are above or higher than the inner ends IE of the strut members.
In alternative embodiments, an alternative hub assembly may be utilized to mechanically or frictionally lock the structure 10 in its constructed configuration without requiring angle A to be more than 90 degrees and without requiring the outer ends OE of the strut members 16 to be above or higher than their inner ends IE.
An alternative hub assembly is useable in embodiments where the internal angle A between the strut axis SA and the vertical axis VA is less than or equal to 90° when the structure is in its fully opened or fully constructed configuration. In this alternative hub assembly, one or more downwardly extending legs are formed on an actuator cap and the actuator cap is at least partially rotatable. Receiving slots are formed in the downwardly extending legs and protruding keys are slidably received within the receiving slots to stabilize and guide the up and down motion of the actuator cap. The corner surface of each leg contacts a protruding key formed on the lower hub member. A side slot is also formed on a lower portion of a leg to receive another key member that protrudes from the lower hub member. When it is desired to convert the structure from its open or constructed configuration to its collapsed configuration, the actuator cap is turned in the counter-clockwise direction to a position wherein one of the keys resides within the slot adjacent to but not within a locking side slot, and the other key resides adjacent to but not within the other slot. The actuator cap is pressed downwardly to exert downward force on the lower hub member, causing the lower hub member to separate from upper hub member, and allowing the structure to assume its collapsed configuration. When it is desired to convert the structure from its collapsed configuration back to its open or constructed configuration, the various elements of the structure will be manipulated into a configuration whrerein the hub assembly is once again in its open or constructed configuration. Thereafter, the actuator cap is turned in the clockwise direction causing one key to slide into locking side slot, and the other key to slide into the slot, thereby locking the upper and lower hub members in fixed vertical positions relative to one another and preventing the structure from inadvertently collapsing during use.
Another alternative hub assembly is useable in embodiments where, when the structure is in its fully opened or fully constructed state, the internal angle A between the strut axis SA and the vertical axis VA is greater than 90°. In this alternative hub assembly, one or more downwardly extending legs are formed on actuator cap. When the user presses downwardly on the actuator cap, the legs extend downwardly into abutment with s flange on the lower hub member. Slots are formed in the legs and protruding keys are slidably received within the slots, thereby guiding the up and down motion of the actuator cap.
Although exemplary embodiments of the invention have been shown and described, many changes, modifications and substitutions may be made by those having ordinary skill in the art without necessarily departing from the spirit and scope of this invention. Specifically, elements or attributes described in connection with one embodiment may also be used in connection with another embodiment provided that the inclusion or use of such element or attribute would not render the embodiment in which it is incorporated unuseable or otherwise undesirable for an intended application. Accordingly, all such additions, deletions, modifications and variations to the above-described embodiments are to be included within the scope of the following claims. | A collapsible structure comprising a collapsible support structure having a flexible covering disposed thereon. The support structure comprises a plurality of pole members that emanate from an upper assembly. The upper assembly has first and second hub members that, when brought into abutting contact with each other, cause the structure to assume a fully constructed configuration but when separated from each other allow the structure to become collapsed. In many embodiments, the structure can be converted from its constructed configuration to its collapsed configuration substantially with the use of a single hand. In some embodiments, 2 or more of the collapsible structures may be joined together to form a multi-unit structure. These collapsible structures may include decorative markings on the flexible cover, especially in embodiments intended for use by or entertainment of children. | 4 |
BACKGROUND OF THE INVENTION
1. The Field Of The Invention
The present invention relates generally to an electrical floor fixture of improved construction for use in a wire distribution system. More specifically, the floor fixture is intended to provide electrical service above the floor covering without regard to in-wall wiring or structural mounting limitation. The present device is particularly adapted for use with under carpet power distribution systems.
Under carpet power distribution systems differ from the normal underfloor conduit systems in that the former system uses flat ribbon cable, having a plurality of flat conductors embedded therein, which is placed directly on the flooring surface and beneath the floor covering. In this manner, electrical power may be routed without regard to the structural walls or conduit systems. The expanded use of under carpet power systems is a relatively recent innovation which is generally restricted to commercial buildings where frequent relocation of outlets or interior alterations render conduit systems impractical. Along with the frequent location changes, there is often a need to have position flexibility, that is, it is frequently necessary to rotate an outlet for practical as well as aesthetic reasons.
2. The Prior Art
There are a number of prior art floor fixtures which provide a rotation feature when coupled with underfloor conduit systems or mounted on floor plates related with the underfloor conduit systems which are embedded in concrete. However, to date there has been no offering of a rotatable floor fixture suitable for use with the under carpet power distribution systems.
SUMMARY OF THE INVENTION
The disclosed device provides a floor fixture having arcuate slot mounting which provides a rotatable fixture especially adapted for use with under carpet power systems. Additionally, the face plates of the fixture are secured by a novel mounting means which eliminates the need for screws in securing the face plate to the floor fixture.
It is an object of this invention to provide a floor fixture for use in under carpet power distribution systems.
It is an object of this invention to provide an improved rotatable floor fixture.
It is an object of this invention to provide a floor fixture having a face plate devoid of any separate means of securing said face plate to said fixture.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an assembled floor fixture.
FIG. 2 is an exploded perspective view of the floor fixture and an under carpet wiring system.
FIG. 2A is a plan view of the floor plate.
FIG. 3 is a graphic representation of the steps in mounting the housing.
FIG. 4 is a section through the lines 4--4 of FIG. 1.
FIGS. 5-9 depict the assembly of the face plate to housing for a floor fixture.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to the attached figures, a preferred embodiment will be described in detail. FIG. 1 shows a floor fixture 4 positioned on a carpet square 2 which has been cut and trimmed. Floor fixture 4 has exposed housing 20, standard duplex receptacle 88, and face plates 70.
Since housing 20 is symmetric about the centerline c--c, FIG. 2, the numerals accompanying the description will be limited to those necessary to call out the features on one side of the fixture.
Housing 20 is die cast as a one piece unit having generally an upper frame 22 and a base 40. Frame 22 is comprised of a rectangular bight 24 flanked by vertically disposed sidewalls 26 which cant outward from the perpendicular to bight 24 and join base 40 at sides 42. Edges 28 cant at approximately five degrees (5°) from a plane normal to the sidewalls 26 and the bight 24. Ridge 32 extends squarely around the inner surface of frame 22 and sides 42 and is recessed from edge 30 of bight 24 by approximately 0.120.
Faces 44 of base 40 are rectangular in shape and extend between sides 42. Sides 42 have lower edges 46 which are perpendicular to face 44 and upper edges 48 which extend from face 44 to edges 28 at a fifteen degree (15°) angle to edges 46.
Floor 50 is generally "C"-shaped and positioned approximately 0.050 below the top edge 45 of face 44. At either end of floor 50 is a platform 52 which has an arcuate slot 54 which is positioned diagonally between face 44 and side 42. A post 56 extends upwardly from each platform 52 on the concave side of slot 54 opposite face 44 and side 42. Post 56 is tapped at 58 to accept a standard screw for mounting a standard duplex receptacle thereon. Mounts 60 are right triangular in shape and are located on the inner surfaces of sides 42. Mount 60 has its altitude at an inner edge of platform 52 and its hypotenuse approximately 0.095 below edge 48 of side 42. Skirt 62 extends parallel to face 44 and provides support for platform 52.
Face plate 70 is molded of acrylonitrile-butadiene-styrene in the preferred embodiment, however, any suitable material providing sufficient flexibility side members 74 may be used. Side member 74 is constructed to complement the structure of housing 20 and achieve a locking therewith. The overall height of side member 74 from top to heel 76 is received within housing 20. Heel 76 is dimensioned to be received between ridge 32 and mount 60 of housing 20.
Sole 78 is dimensioned to complement mount 60 and toe 80 is dimensioned to rest on platform 52 adjacent face 44. The combination of face plate 70 and housing 20 will be more fully explained in the assembly details hereinafter. Rib 82 has a void 84, shown in FIG. 5, which has been found to be beneficial in flexing during assembly, however, the rib 82 is not essential to the operation of the invention. The openings 86 are dimensioned to accept a standard duplex receptacle 88.
Turning now to FIG. 2, there is shown the preferred embodiment of the present invention with the associated hardware for use in a flat conductor system. The system comprises a ribbon cable 90 with three flat conductors 92 embedded therein, a terminal block 94 for transition from flat conductors to round conductors, a flat stock ground shield 98 and a floorplate 100. Terminal block 94 is described in U.S. Pat. application Ser. No. 43,769, filed May 30, 1979. Flat conductor ribbon cable 90 and ground shield 98 are known in the art.
Floor plate 100 is stamped and formed sheet metal having a thickness of 0.063, see FIG. 2A.
Opening 104 is generally centered in base 102 of floor plate 100. The use of a modified elliptical opening provides additional clearance at either end of terminal block 94; its purpose will be explained hereinafter. A series of upstanding members 106, integral with base 102 and generally perpendicular thereto, surrounding opening 104 are provided as strengthening members. Opposed tabs 108 are integral with base 102 and are bent back parallel to base 102 in a U-shaped fashion. Hole 110 is punched in tab 108 to accept a self-tapping standard sheet metal screw. Arcuate slots 112 and 114 are positioned adjacent the elliptical ends of opening 104 and extend across the centerline of plate 100 from points on the diagonal of plate 100. Posts 120 and 122 (FIG. 2) having threaded bores therein are affixed to plate 100 on the other diagonal at either end of opening 104 in prepunched holes 116 and 118.
Assembly
Referring now to FIG. 3, ribbon cable 90 with terminal block 94 attached is positioned on the flooring and floor plate 100 is located over the terminal block 94 in the desired orientation. Floor plate 100 is secured to the flooring via suitable fasteners 130 through arcuate slots 112 and 114. Ground shield 98 is fitted to floor plate 100 and electrically interconnected to tab 108 via a machine screw 134 in hole 110. Referring now to FIG. 4, suitable lengths of round conductors 96 are secured to terminal block 94. Housing 20 is then positioned over floor plate 100 with selected diagonally opposed arcuate slots 54 over the posts 120 and 122. Suitable fasteners 132 are placed through arcuate slots 54 and threaded into the bores in posts 120 and 122 respectively to secure housing 20 to floor plate 100. A standard duplex receptacle 88 is connected in the usual fashion to round conductor 96 and mounted on posts 56. Adjustment or rotation of the assembly may be accomplished by loosening fasteners 130 and 132 and rotating the respective arcuate slots. If additional adjustment is desired, fasteners 132 may be removed and housing 20 rotated to locate the second set of diagonally opposed platforms 52 over the respective threaded posts 120 and 122.
Face plates 70 are mounted on housing 20 by squeezing side members 74 inward, locating toe 80 behind face 44 and moving top 72 of face plate 70 against ridge 32 and under bight 24 of housing 20. Side members 74 are then released which will cause heel 76 and sole 78 to locate on and behind mount 60. The mounting sequence is shown sectionally in FIGS. 5 through 9. | A floor fixture adapted for use with flat undercarpet power distribution systems has a face plate with a snap-in retaining feature requiring no screws and a mounting arrangement which allows for rotation of the fixture after installation. | 8 |
BACKGROUND OF THE INVENTION
The present invention generally relates to ink jet recording methods and apparatuses, and more particularly to an ink jet recording method which enables gradation recording and an ink jet recording apparatus which employs such an ink jet recording method.
Recently, there is growing interest in non-impact recording methods because noise generated at the time of the recording is negligibly small according to these methods. Among such non-impact recording methods, the so-called ink jet recording method is an effective method because a high-speed recording is possible and the recording can be made on an ordinary paper without the need for a special fixing process. Various kinds of ink jet recording methods have been proposed in the past, and some have already been reduced to practice while others are still being modified.
The ink jet recording methods eject droplets of ink and adhere the droplets onto a recording medium such as paper. The ink jet recording methods can be categorized into several systems depending on the methods of generating the droplets of ink and the methods of controlling the ejecting direction of the droplets.
A first method is disclosed in a U.S. Pat. No. 3,060,429, for example. According to this first method, the droplets of ink are generated by electrostatic suction and the droplets are controlled by an electric field depending on a recording signal so that the droplets are selectively adhered on the recording medium. More particularly, the electric field is applied between a nozzle and an accelerating electrode, and the nozzle ejects uniformly charged droplets of ink. These droplets are ejected between x-y deflection electrodes which are electrically controlled depending on the recording signal, and the droplets are selectively adhered on the recording medium depending on the intensity change of the electric field.
A second method is disclosed in U.S. Pat. Nos. 3,596,275 and 3,298,030, for example. According to this second method, charge-controlled droplets of ink are generated by a continuous vibration generating method, and the droplets are ejected between deflection electrodes applied with a uniform electric field and adhered on the recording medium. More particularly, a recording head having a piezo vibration element and a nozzle is employed, and a charging electrode applied with a recording signal is arranged in front of an orifice of the nozzle at a predetermined distance from the orifice. An electric signal having a constant frequency is applied to the piezo vibration element so as to mechanically vibrate the piezo vibration element, and the droplets of ink are ejected via the orifice. The droplets which are ejected are charged by the charging electrode due to electrostatic induction, and the droplets are charged by an amount dependent on the recording signal. The charge-controlled droplets are deflected depending on the amount of charge as they are ejected between deflection electrodes which apply a uniform electric field, and only the droplets which carry the recording signal are adhered on the recording medium.
A third method is disclosed in a U.S. Pat. No. 3,416,153, for example. According to this third method, an electric field is applied between a nozzle and a ring-shaped charging electrode, and the droplets of ink are generated in the form of mist by the continuous vibration generating method. In other words, according to this third method, the mist state of the droplets is controlled by modulating the field intensity applied between the nozzle and the charging electrode depending on the recording signal, and the recording is made on the recording medium with gradation.
A fourth method is disclosed in a U.S. Pat. No. 3,747,120, for example. The operating principle of this fourth method differs completely from those of the first, second and third methods described above. In other words, the first through third methods electrically control the droplets of ink ejected from the nozzle, and the droplets carrying the recording signal are selectively adhered on the recording medium. But according to the fourth method, the droplets of ink are ejected from the nozzle depending on the recording signal. That is, the electric recording signal is applied to the piezo vibration element of the recording head which has the nozzle so as to convert the electric recording signal into the mechanical vibration of the piezo vibration element, and the droplets of ink are ejected from the nozzle depending on this mechanical vibration so as to adhere the droplets on the recording medium.
However, each of the four methods described above have problems to be solved, as will be described hereinafter.
According to the first through third methods, the droplets of ink are generated directly from electrical energy, and the deflection control of the droplets is made by the electric field. For this reason, the first method uses a simple construction, but a large voltage is required to generate small droplets of ink. In addition, the first method is unsuited for a high-speed recording because it is difficult to provide a multi-nozzle on the recording head.
As for the second method, the high-speed recording is possible because the multi-nozzle may be provided on the recording head. However, the construction needed to generate the droplets of ink becomes complex, and it is difficult to electrically control the small droplets. Furthermore, the so-called satellite dots are easily formed on the recording medium.
The third method can record a satisfactory image with gradation by forming a mist of the droplets of ink. But in this case, it is difficult to control the mist state, and smear is easily formed on the recording medium. Furthermore, it is difficult to provide the multi-nozzle on the recording head, and the third method is unsuited for carrying out the high-speed recording.
Compared to the first through third methods, the fourth method has a relatively large number of advantageous points. In other words, the fourth method uses a simple construction. In addition, since the droplets of ink are ejected from the nozzle in an on-demand manner, it is unnecessary to recover the droplets which are not used for the recording, unlike the first through third methods. Moreover, unlike the first and second methods, the fourth method does not require the use of a conductive ink, and the material and composition of the ink can be selected with a large degree of freedom. But on the other hand, it is difficult to form the recording head required by the fourth method. Furthermore, it is difficult to provide the multi-nozzle on the recording head because the downsizing of the piezo vibration element having a desired resonance frequency is extremely difficult. The fourth method is also unsuited for carrying out the high-speed recording because the droplets of ink are ejected by the mechanical energy, that is, the mechanical vibration of the piezo vibration element.
Therefore, there is a problem in that the first through fourth methods can only be used in applications where the disadvantages of each method can substantially be neglected.
An ink jet recording apparatus was previously proposed in a Japanese Laid-Open Patent Application No. 54-51837 to reduce the problems described above. According to this proposed ink jet recording apparatus, the ink within an ink chamber is heated so as to generate air bubbles and the pressure of the ink is increased. As a result, the ink is ejected from a fine capillary tube nozzle and transferred onto a recording medium such as paper. Using the operating principle of this proposed ink jet recording apparatus, various modifications have been made.
A Japanese Laid-Open Patent Application No. 2-23349 proposes one of such modifications. According to this modification, a thermal ink jet recording head ejects droplets of ink from a capillary tube region in response to an electrical signal. The thermal ink jet recording head is provided with a head resistor which generates heat in response to the electrical signal and is provided at a position such that the heat is applied within the capillary tube region. The head resistor includes a resistor region and a conductor region which surrounds the resistor region. At least a part of the conductor region is electrically connected to the resistor region. By providing the conductor region at the central part of the resistor region, the air bubbles are generated in a ring shape when a current pulse is applied, and a cool point is generated at the center of the head resistor. As a result, the air bubbles are destroyed into smaller air bubbles and the smaller air bubbles are distributed at random on the surface of the head resistor due to the shock of this destruction, thereby making it possible to minimize the damage caused by the cavitation of the head resistor.
The durability of the ink jet recording apparatus proposed in the Japanese Laid-Open Patent Application No. 54-51837 has also been improved recently and reduced to practice. However, the demand to more finely control the amount of ink ejection is increasing so that it is possible to obtain an even finer image quality. A Japanese Laid-Open Patent Application No. 55-132259 proposes one method of satisfying such a demand.
According to the method proposed in the Japanese Laid-Open Patent Application No. 55-132259, a sudden state transition is caused in the ink by the action of the thermal energy, and droplets of ink are ejected by the action based on this state transition so as to adhere the ink on the recording medium. More particularly, an ejection orifice for ejecting the ink in a predetermined direction is provided at a terminal end of a conduit, and a thermal action part is arranged to communicate with the ejection orifice and to effectively transmit the action force generated therein in the direction of the ejection orifice. This thermal action part is formed by at least two electric-to-heat converters capable of independently receiving signals, and a gradation recording is carried out by appropriately shifting the timings of the signals input to the electric-to-heat converters. As may be understood from the teaching in the Japanese Laid-Open Patent Application No. 55-132259, a control electrode and a ground (common) electrode are formed on the same plane. For this reason, there is a problem in that it is difficult to arrange the electrodes with a high density.
On the other hand, Japanese Laid-Open Patent Applications No. 55-73568 and No. 55-73569 propose selecting a predetermined number of heaters out of a plurality of heaters arranged in one conduit or, selecting one heater from a plurality of heaters having mutually different heat values, so as to vary the size of the air bubbles which are generated and to control the amount of ink which is ejected. However, the air bubbles generated in the thermal ink jet recording apparatus displays a binary behavior ("1" or "0"), that is, the ink is either ejected or not ejected. Therefore, the amount of ink which is ejected inevitably changes in steps, and a smooth change cannot be realized. For this reason, there is a problem in that it is difficult to make the recording with a high image quality.
SUMMARY OF THE INVENTION
Accordingly, it is a general object of the present invention to provide novel and useful ink jet recording method and apparatus in which the problems described above are eliminated.
Another and more specific object of the present invention is to provide an ink jet recording apparatus comprising an ink jet recording head which includes at least one nozzle for ejecting ink, a heating layer, and a ground electrode and a plurality of control electrodes electrically connected to the heating layer, and a thermal energy action part, formed in the heating layer in correspondence with the nozzle, for heating the ink and causing a state transition so as to eject the ink from the nozzle when a voltage is applied across at least one pair of the ground electrode and the control electrode, where the ground electrode electrically connects to the heating layer within a region of the thermal energy action part, and the control electrodes electrically connects to the heating layer outside the region of the thermal energy action part. According to the ink jet recording apparatus of the present invention, it is possible to continuously vary the amount of ink which is ejected in an extremely smooth manner.
Still another object of the present invention is to provide an ink jet recording head comprising at least one nozzle for ejecting ink, a heating layer, a ground electrode and a plurality of control electrodes electrically connected to the heating layer, and a thermal energy action part, formed in the heating layer in correspondence with the nozzle, for heating the ink and causing a state transition so as to eject the ink from the nozzle when a voltage is applied across at least one pair of the ground electrode and the control electrode, where the ground electrode electrically connects to the heating layer within a region of the thermal energy action part, and the control electrodes electrically connects to the heating layer outside the region of the thermal energy action part. According to the ink jet recording head of the present invention, the construction becomes simple compared to the conventional head having a plurality of thermal energy action parts with respect to one nozzle.
A further object of the present invention is to provide an ink jet recording method which uses an ink jet recording head including at least one nozzle for ejecting ink, a heating layer, a ground electrode and a plurality of control electrodes electrically connected to the heating layer, and a thermal energy action part, formed in the heating layer in correspondence with the nozzle, for heating the ink and causing a state transition so as to eject the ink from the nozzle when a voltage is applied across at least one pair of the ground electrode and the control electrode, the ground electrode electrically connecting to the heating layer within a region of the thermal energy action part, the control electrodes electrically connecting to the heating layer outside the region of the thermal energy action part, where the ink jet recording method comprises the steps of (a) setting resistances between the ground electrode and the control electrodes mutually different, and (b) applying a voltage across the ground electrode and a selected one of the control electrodes depending on a level of a signal which describes information to be recorded. According to the ink jet recording method of the present invention, it is possible to continuously vary the amount of ink which is ejected in an extremely smooth manner.
Another object of the present invention is to provide an ink jet recording method which uses an ink jet recording head including at least one nozzle for ejecting ink, a heating layer, a ground electrode and a plurality of control electrodes electrically connected to the heating layer, and a thermal energy action part, formed in the heating layer in correspondence with the nozzle, for heating the ink and causing a state transition so as to eject the ink from the nozzle when a voltage is applied across at least one pair of the ground electrode and the control electrode, the ground electrode electrically connecting to the heating layer within a region of the thermal energy action part, the control electrodes electrically connecting to the heating layer outside the region of the thermal energy action part, where the ink jet recording method comprises the steps of (a) selecting an arbitrary number of control electrodes depending on a level of a signal which describes information to be recorded, and (b) applying a voltage across the ground electrode and the selected arbitrary number of control electrodes. According to the ink jet recording method of the present invention, it is possible to continuously vary the amount of ink which is ejected in an extremely smooth manner.
Other objects and further features of the present invention will be apparent from the following detailed description when read in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-1G (referred to collectively as FIG. 1 below) are diagrams for explaining the operation of a bubble ink jet head to which the present invention may be applied;
FIG. 2 is a perspective view showing the bubble ink jet head;
FIG. 3 is a perspective view showing a lid substrate and a heater substrate of the bubble ink jet head shown in FIG. 2 in a disassembled state;
FIG. 4 is a perspective view showing the lid substrate viewed from the bottom in FIG. 3;
FIGS. 5A-5D (referred to collectively as FIG. 5 below) are diagrams for explaining a method of producing an embodiment of a heat energy action part of a head of an ink jet recording apparatus according to the present invention;
FIGS. 6A-6E (referred to collectively as FIG. 6 below) are diagrams for explaining a method of forming a heating layer and a control electrode;
FIGS. 7A-7E (referred to collectively as FIG. 7 below) are diagrams for explaining a method of producing another embodiment of the heat energy action part of the head of the ink jet recording apparatus according to the present invention;
FIG. 8 is a diagram for explaining the operation of the ink jet recording apparatus according to the present invention;
FIGS. 9A and 9B (referred to collectively as FIG. 9 below) are diagrams for explaining an air bubble which is generated when a driving pulse is input to a control electrode;
FIG. 10 is a diagram for explaining an air bubble which is generated when another control electrode is used;
FIGS. 11A-11C (referred to collectively as FIG. 11 below) show pattern of the thermal energy action part; and
FIGS. 12A and 12B are diagrams for explaining a method of varying the amount of ink which is ejected by driving two control electrodes.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a diagram for explaining the operation of a bubble ink jet head to which the present invention may be applied, and FIG. 2 is a perspective view showing the bubble ink jet head. FIG. 3 is a perspective view showing a lid substrate and a heater substrate of the bubble ink jet head shown in FIG. 2 in a disassembled state, and FIG. 4 is a perspective view showing the lid substrate viewed from the bottom in FIG. 3. In FIGS. 1 through 4, the bubble ink jet head includes a lid substrate 21, a heater substrate 22, an ink inlet 23, an orifice 24, a conduit 25, a region 26 for forming an ink chamber, an independent electrode 27, a common electrode 28 and a heater 29. An air bubble 31 is formed in an ink 30, and this ink 30 is ejected in the form of a droplet 32.
First, a description will be given of the operation of the bubble ink jet head, by referring to FIG. 3.
In FIG. 1, (a) shows a stationary state in which the surface tension of the ink 30 at the orifice surface is balanced with the external pressure.
In FIG. 1, (b) shows a state in which the surface temperature of the heater 29 rises rapidly to a temperature at which the boiling phenomenon occurs in the adjacent ink layer and the ink 30 is studded with fine air bubbles 31.
In FIG. 1, (c) shows a state in which the rapidly heated adjacent ink layer instantaneously evaporates at the entire surface of the heater 29 to form a boiling film and the air bubbles 31 are grown. In this state, the pressure within the nozzle is raised by the amount by which the air bubbles 31 grow. For this reason, the surface tension at the orifice surface and the external pressure become unbalanced, and a column of the ink 30 starts to grow at the orifice 24.
In FIG. 1, (d) shows a state in which the air bubbles 31 are grown to a maximum and an amount of the ink 30 corresponding to the volume of the air bubbles 31 is pushed out from the orifice surface. In this state, no current is supplied to the heater 29 and the surface temperature of the heater 29 is about to fall. The volume of the air bubbles 31 reaches the maximum value at a time which is slightly delayed from the time when an electrical pulse is applied to the head.
In FIG. 1, (e) shows a state in which the air bubbles 31 are cooled by the ink 30 and the like and start to contract. The tip end part of the ink column continues to move to the left in FIG. 3 while maintaining the velocity at which the ink 30 is pushed out of the orifice 24. On the other hand, a constriction is formed in the ink column at the rear end part of the ink column because the pressure within the nozzle decreases due to the contraction of the air bubbles 31 and the ink flows backward into the nozzle from the orifice surface.
In FIG. 1, (f) shows a state in which the air bubbles 31 further contract and the ink 30 makes contact with the heater surface thereby further and rapidly cooling the heater surface. At the orifice surface, the meniscus is large because the external pressure becomes higher than the pressure within the nozzle, and the meniscus enters within the nozzle. The tip end part of the ink column becomes a droplet and is ejected towards the recording paper at a velocity of approximately 5 to 10 m/sec.
In FIG. 1, (g) shows a state in which the ink 30 is refilled to the orifice 24 by the capillary phenomena and the air bubbles 31 are completely eliminated. This state (g) corresponds to the process of returning to the initial state shown in (a).
In the present invention, the size of the air bubbles which are generated or the timing with which the plurality of air bubbles are generated is varied, depending on a level of a signal which describes information to be recorded, in the thermal ink jet recording apparatus which operates under the operating principle such as that described above.
A description will be given of a method of producing an embodiment of a thermal energy action part of a head of the ink jet recording apparatus according to the present invention, by referring to FIG. 5 which shows the characterizing structure of the present invention. In (a) through (d) of FIG. 5, only the pattern part which is formed at that process is indicated by the hatching. A contact hole is denoted by a reference numeral 1, and control electrodes are denoted by reference numerals 2 through 5.
When actually producing the thermal energy action part, it is of course not essential that the shape and the connection of the patterns (heating layer and electrode pattern) shown in FIG. 5 are employed.
In (a) of FIG. 5, a silicon wafer is subjected to a thermal oxidation to form a silicon dioxide ((SiO 2 ) layer having a thickness of 1.5 μm as a heat storage layer. An aluminum (Al) layer having a thickness of 1 μm is formed on the SiO 2 layer as a ground electrode, and this Al layer is formed into a pattern shown by using photolithography and etching techniques.
In (b) of FIG. 5, a SiO 2 layer which is used as an insulator layer is formed to a thickness of 1.2 μm by a sputtering. A contact hole 1 is formed in this SiO 2 layer by using the photolithography and etching techniques, for making contact to the underlying Al layer (ground electrode). In this case, the contact hole 1 has a triangular shape.
In (c) of FIG. 5, a hafnium boride (HfB 2 ) layer which is used as a heating layer is formed to a thickness of 3000 Å by a sputtering. This HfB 2 layer is formed into a shape at a position by using the photolithography technique such that the HfB 2 layer makes contact with the underlying Al layer (ground electrode ) via the contact hole 1.
In (d) of FIG. 5, an Al layer which is used as a control electrode is formed to a thickness of 1 μm by a sputtering. This Al layer is formed into a pattern shown by the photolithograhpy and etching techniques. In this case, four control electrodes 2 through 5 are formed. These control electrodes 2 through 5 can be driven independently with respect to one heating layer.
Finally, although not shown in FIG. 5, a SiO 2 protecting layer is formed to a thickness of 1 μm by a sputtering, so as to protect the heating layer and the electrodes from corrosion caused by the ink. This SiO 2 protecting layer does not cover a region where a bonding pad is formed. In addition, a tantalum (Ta) layer which is used as a cavitation resistant protecting layer is formed to a thickness of 4000 Å by a sputtering in a vicinity of the heating layer. Furthermore, an electrode protecting layer is formed to a thickness of 1.2 μm at the electrode part. For example, this electrode protecting layer is made of Photonith manufactured by Toray, Japan. The pattern of each of the protecting layers can be appropriately controlled by the photolithography and etching techniques.
FIG. 6 is a diagram for explaining a method of forming the heating layer and the control electrode. As described above, FIG. 5 is a diagram for explaining the characterizing structure of the present invention, but the shape and process described in conjunction therewith are not necessarily the same, so as to simplify the description. FIG. 6 shows one example of the actual shape and process related to the heating layer and the control electrode.
When forming the control electrode 3 shown in FIG. 5, HfB 2 is sputtered on the entire surface as shown in (a) of FIG. 6, and Al is sputtered thereon in succession as shown in (b) of FIG. 6. Next, as shown in (c) of FIG. 6, a pattern made up of the band shaped HfB 2 layer and the Al layer stacked thereon is formed by the photolithography and etching techniques. Finally, as shown in (d) of FIG. 6, the HfB 2 layer which becomes the heating part is exposed using the photolithography and etching techniques. In this case, the cross section becomes as shown in (e) of FIG. 6.
A description will be given of a method of producing another embodiment of the thermal energy action part of the head of the ink jet recording apparatus according to the present invention, by referring to FIG. 7 which also shows the characterizing structure of the present invention. In (a) through (d) of FIG. 7, only the pattern part which is formed at that process is indicated by the hatching.
When actually producing the thermal energy action part, it is of course not essential that the shape and the connection of the patterns (heating layer and electrode pattern) shown in FIG. 7 are employed.
In (a) of FIG. 7, a silicon wafer is subjected to a thermal oxidation to form a SiO 2 layer having a thickness of 1.5 μm as a heat storage layer. A HfB 2 layer is sputtered on the SiO 2 layer to a thickness of 3000 Å as a heating layer, and an Al layer is then sputtered to a thickness of 1 μm as an electrode.
In (b) of FIG. 7, the HfB 2 and Al layers are patterned as shown using the photolithography and etching techniques.
In (c) of FIG. 7, the Al layer is partially removed by the photolithography and etching techniques so as to expose the heating layer.
In (d) of FIG. 7, a SiO 2 layer is sputtered as an insulator layer, and by using the photolithography and etching techniques, a contact hole 1 is formed in a region of this SiO 2 layer where the heating layer exists underneath. In this case, the contact hole 1 has a triangular shape.
In (e) of FIG. 7, an Al layer is sputtered to a thickness of 1 μm and is then patterned by the photolithography and etching techniques so as to form a ground electrode 6. This ground electrode 6 makes contact with the heating layer via the contact hole 1.
Finally, although not shown in FIG. 7, a SiO 2 protecting layer is formed to a thickness of 1 μm by a sputtering, so as to protect the heating layer and the electrodes from corrosion caused by the ink. This SiO 2 protecting layer does not cover a region where a bonding pad is formed. In addition, a tantalum (Ta) layer which is used as a cavitation resistant protecting layer is formed to a thickness of 4000 Å by a sputtering in a vicinity of the heating layer. Furthermore, an electrode protecting layer is formed to a thickness of 1.2 μm at the electrode part. For example, this electrode protecting layer is made of Photonith manufactured by Toray, Japan. The pattern of each of the protecting layers can be appropriately controlled by the photolithography and etching techniques.
The positional relationship of the ground electrode and the control electrode is reversed between the embodiments shown in FIGS. 5 and 7. Otherwise, the two embodiments are the same in that the heating layer and the ground electrode are stacked via the insulator layer.
FIG. 8 is a diagram for explaining the operation of the ink jet recording apparatus according to the present invention. In FIG. 8, only the heating layer, the ground electrode and the control electrode are shown, and the illustration of the insulator layer and the protecting layers is omitted so as to facilitate the understanding of the operating principle of the present invention. In addition, the positional relationships of the layers at the connecting parts of the patterns is also omitted in FIG. 8.
The ground electrode 6 and the heating layer are connected via the triangular contact hole 1. When a driving pulse is input to each of the control electrodes 2 through 5, a current flows as indicated by the arrows in FIG. 8.
First, attention is given to the control electrode 2. A boundary line which is formed by the connecting part between the control electrode 2 and the heating layer is not parallel to a boundary line which is formed by the connecting part between the ground electrode 6 and the heating layer and closest to the control electrode 2. Accordingly, when the driving pulse is input to the control electrode 2, a heat gradient is generated on the heating part and the air bubble is first generated at the lower region as shown in (a) of FIG. 9. Next, if the driving pulse voltage is increased, the size of the air bubble becomes larger and the air bubble reaches the upper region as shown in (b) of FIG. 9. In other words, the size of the air bubble which is generated can be varied by varying the input energy.
Next, attention is given to the control electrodes 4 and 5. In this case, the widths of the control electrode 4 and 5 which connect to the heating layer differ. For this reason, if the same driving pulse voltage is input to the control electrodes 4 and 5, the heat values of the respective parts of the heating layer become different, and the sizes of the air bubbles generated thereby also differ. In the case shown in FIG. 8, the control electrode 5 is wider and generates a larger air bubble as shown in FIG. 10.
Similarly, when attention is given to the control electrodes 3 and 4, the widths of the control electrode 3 and 4 which connect to the heating layer differ. However, if the width of the patterns of these control electrodes 3 and 4 were the same, the distance from the connecting part of the control electrode 3 and the heating layer to a boundary line which is formed by the connecting part of the ground electrode 6 and the heating layer closest to the control electrode 3 is different from the distance from the connecting part of the control electrode 4 and the heating layer to a boundary line which is formed by the connecting part of the ground electrode 6 and the heating layer closest to the control electrode 4. For this reason, the resistances of the control electrodes 3 and 4 become different, and similarly, the sizes of the air bubbles which are generated also become different.
The operating principle of the present invention was described above for the patterns shown in FIG. 5, but the present invention is of course not limited to the patterns shown in FIG. 5. FIG. 11 shows another embodiment of the patterns. In FIG. 11, the reference numerals 11, 12 and 13 respectively denote a contact hole, a control electrode and a heating layer.
The patterns shown in FIGS. 5, 7 and (a) and (b) of FIG. 11 are suited for use in the so-called edge shooter type thermal ink jet recording head which ejects the ink in a direction parallel to the heating surface. On the other hand, the pattern shown in (c) of FIG. 11 is suited for use in the so-called side shooter type thermal ink jet recording head which ejects the ink in a direction perpendicular to the heating surface.
As described above, it may be readily seen that the present invention enables the size of the air bubble to be varied on the heating layer which connects to each of the control electrodes.
Next, a description will be given of a preferable application of the present invention. In a most simple application, one control electrode is selected depending on the level of a signal which describes the information to be recorded. Because the size of the air bubble can be varied on the heating layer which connects to each control electrode, the amount of ink which is ejected can easily be varied by appropriately selecting the control electrodes.
Even if it is assumed that the pattern is such that the sizes of the air bubbles generated at each of the control electrodes are the same, one or mode control electrodes can be driven simultaneously depending on the level of the signal which describes the information to be recorded, so as to vary the number of the air bubbles generated on the heating layer. A plurality of air bubbles may be combined into one air bubble, and in this case, the volume of the air bubble is varied and not the number. In any case, the amount of ink which is ejected can be varied in this manner. In this case, if the pattern is such that the size of the air bubble generated at each control electrode is variable, a plurality of control electrodes may be appropriately selected and there are various variations to this selection. As a result, it is possible to continuously vary the amount of ink which is ejected in an extremely smooth manner.
In another application, the timing with which the current is applied to each of the control electrodes may be varied, so as to generate the air bubbles simultaneously or with a time difference. As a result, it is possible to vary the amount of ink which is ejected. FIGS. 12A and 12B are diagrams for explaining the method of varying the amount of ink which is ejected by driving two control electrodes. FIG. 12A shows a case where the driving pulse is simultaneously applied to the two control electrodes. In this case, the two air bubbles which are generated are combined to form a large air bubble. As a result, the amount of ink which is ejected increases and a large pixel is recorded. If the two air bubbles are mutually separated, the two air bubbles are not combined and the two air bubbles are generated as independent air bubbles but at the same time. On the other hand, FIG. 12B shows a case where the driving pulse is applied to the two control electrodes with a time difference. Unlike the case shown in FIG. 12A, the two air bubbles reach the maximum size at different times, and thus, the combined air bubble does not becomes as large as in the case shown in FIG. 12A. Accordingly, the amount of ink which is ejected is smaller and the diameter of the pixel which is recorded is smaller compared to the case shown in FIG. 12A.
In a first embodiment of the ink jet recording apparatus according to the present invention, the head having the structure shown in FIG. 1 is used. This head has the thermal energy action part shown in FIG. 5. The experiment was conducted by applying the driving pulse to each control electrode, where the ejection nozzle has the size of 55 μm×50 μm and the thermal energy action part (region of the heating layer) has the size of 80 μm×200 μm. The contact hole which connects the heating layer and the ground electrode has the triangular shape as shown in FIG. 5, and the size of this contract hole is 15 μm×100 μm×101 μm. The distance from the ejection nozzle formed at approximately the center of the heating layer to the closest thermal energy action part is 180 μm.
The ink used is the ink of "Think Jet" manufactured by Hewlett Packard of the U.S.A. The recording was made on a "Mat Coat Paper NM" manufactured by Mitsubishi Seishi of Japan. The same driving pulse was applied to each of the control electrodes, the voltage being 28 V and the pulse width being 6 μsec. The resistance between the ground electrode 6 and the control electrodes 2 through 5 was 60.7 Ohms for the control electrode 2, 81.2 Ohms for the control electrode 3, 100.3 Ohms for the control electrode 4, and 70.7 Ohms for the control electrode 5. The following Table 1 shows the evaluation results of the diameters of the pixels which are recorded under each of the listed conditions. The diameter of the pixel shown in the Table 1 is an average value of fifty pixels.
TABLE 1______________________________________Case No. Condition Pixel Diameter (μm)______________________________________1. Driving pulse applied 120.6 only to electrode 22. Driving pulse applied 100.5 only to electrode 33. Driving pulse applied 96.1 only to electrode 44. Driving pulse applied 110.2 only to electrode 55. Driving pulse applied to 170.1 electrodes 2 & 3 at same time6. Driving pulse applied to 160.8 electrodes 2 & 4 at same time7. Driving pulse applied to 131.3 electrodes 3 & 4 at same time8. Driving pulse applied to 222.5 electrodes 2 to 5 at same time9. Driving pulse applied to 159.1 electrode 3 3 μsec after applying driving pulse to electrode 210. Driving pulse applied to 146.3 electrode 3 5 μsec after applying driving pulse to electrode 211. Driving pulse applied to 127.7 electrode 3 10 μsec after applying driving pulse to electrode 212. Driving pulse applied to 201.5 electrode 4 3 μsec after applying driving pulse to electrodes 2 & 313. Driving pulse applied to 186.2 electrode 4 5 μsec after applying driving pulse to electrodes 2 & 314. Driving pulse applied to 175.0 electrode 4 10 μsec after applying driving pulse to electrodes 2 & 3______________________________________
Therefore, it is possible to easily continuously vary the diameter of the pixel which is recorded in an extremely smooth manner by independently applying the driving pulse to each of the control electrodes, simultaneously applying the driving pulse to combinations of the control electrodes or, varying the timings with which the driving pulse is applied to each of the control electrodes. Hence, it is possible to record the image on the recording medium (for example, paper) with a high image quality.
In a second embodiment of the ink jet recording apparatus according to the present invention, only the control electrode 2 is used and the recording is carried out by gradually varying the driving pulse (input energy). The following Table 2 shows the evaluation results of the diameters of the pixels which are recorded under each of the listed conditions.
TABLE 2______________________________________Driving Voltage Pulse Width Pixel(V) (μsec) Diameter (μm)______________________________________25 6 95.526 6 101.127 6 112.328 6 120.629 6 140.4______________________________________
Further, the present invention is not limited to these embodiments, but various variations and modifications may be made without departing from the scope of the present invention. | An ink jet recording apparatus is provided with an ink jet recording head which includes at least one nozzle for ejecting ink, a heating layer, and a ground electrode and a plurality of control electrodes electrically connected to the heating layer, and a thermal energy action part, formed in the heating layer in correspondence with the nozzle, for heating the ink and causing a state transition so as to eject the ink from the nozzle when a voltage is applied across at least one pair of the ground electrode and the control electrode. The ground electrode electrically connects to the heating layer within a region of the thermal energy action part, and the control electrodes electrically connects to the heating layer outside the region of the thermal energy action part. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority under 35 U.S.C. § 119 of Provisional Application Ser. No. 60/654,132 filed Feb. 18, 2005, which application is hereby incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
The present invention relates generally to corn heads for use with combines and specifically to an improved corn head using a reel device to reduce debris build-up.
Combines that harvest corn are provided with several snouts for directing rows of corn stalks to ear separation chambers, into an auger, through a feederhouse and into a combine's inner chambers which separate the corn kernels from the corn cob.
Combine operators routinely encounter difficulties when harvesting corn especially with debris building up in front of a feederhouse of the combine. Previously, combines that harvested only 4 or 8 rows encountered this debris build-up only occasionally because the corn yields experienced were low, the varieties of hybrid corn dropped their leaves sooner, thicker plant spacing resulting in more corn fodder to process, the speed of the combine moving through the field was slow, and not as many rows of corn were being harvested.
Advances in plant science have caused an increase in the amount of debris experienced by the combine operator. A modern combine experiences these problems much more frequently because today's corn varieties retain their leaves longer, utilizing corn planted more densely in the rows and more closely together, extremely high corn yields and operating the combine at much faster speeds. Much of the increase in corn yields has come from genetic improvements to the corn plant through biotechnology or genetic modifications. This yield increase has brought with it larger, healthier corn plants that produce larger amounts of debris that may potentially break off the stalk and have to be ingested by the combine. Still further creating problems, the typical size of a feederhouse has remained unchanged relative to the horsepower and threshing capacity of today's modem combines. Today's machines have in excess of 400 hp engines and can process more than 4000 bushels of corn per hour versus machines of 10 years ago that had 200 horsepower and could harvest 2000 bushels of corn per hour. While it would make sense to double the size of the feederhouse opening on these new machines in this process, that has not been the case. Instead the feederhouse opening has remained virtually unchanged.
Further complicating this problem is the plastic material from which much of the “snouts” or row dividers are made. This plastic material when constantly rubbed by plant material may develop a static charge which potentially causes the debris to adhere to the plastic material, to the steel on the backboard of the head, and to other plant material. Relative humidity in the fall typically drops to 20% or less in the corn belt which aids the buildup of this static charge.
Severe debris buildup results from dry harvest conditions. This debris is made up of corn stalks, leaves, and “fluff” which is fine particles of ground up stalks and leaves. The debris is not a problem once it moves past the feederhouse. Debris is processed by the combine into mulch and returned to the field to decay through the winter months. However, getting the debris into the feederhouse may be a problem because the debris and fluff together may form an obstruction which hinders and/or blocks corn from entering into a combine for processing. In order to prevent this obstruction, the operator must slow down or stop, thereby letting the feederhouse remove this debris. If the operator cannot prevent the debris from forming an obstruction, the operator must climb out of the combine cab and try to remove the debris by hand or using a tool. Any type of manual removal of this debris is hazardous to the operator and may cause injury or death to the operator. For example, the operator often must travel in between the snouts and reach up into the debris pile with a broom handle to clear the debris. Should the corn head be left on, the operator has risk of serious injury.
Therefore, the debris problem creates two issues. One, a time issue in which the operator is losing valuable time because they are removing debris or slowing down and stopping to have the machine removes the debris. Two, a safety issue in that the operator is exposed to risk of injury by trying to manually unclog an obstruction of debris in the feederhouse.
Therefore, an objective of the present invention is to overcome the problem of debris build-up in front of the feederhouse.
A further objective of the present invention is to provide an adjustable device which optimizes the removal of debris in front of the feederhouse.
Still another objective of the present invention is the provision of rotating bars which can be actuated from the cab of the combine to unclog debris from the feederhouse.
Yet another objective of the present invention is the provision of a frame with rotatable bars which is moveable between operative and inoperative positions.
Another objective of the present invention is the provision of a debris clearing device which can be retrofit to various combines.
A further objective of the present invention is the provision of a device that is economical to manufacture, simple to install, and effective and durable in use.
These and other objectives will become apparent from the following specification and drawings.
SUMMARY OF THE INVENTION
The foregoing objectives may be obtained using an improved corn head with a reel device that reduces debris build-up. The improved corn head includes a frame defining a feederhouse and a channel leading to the feederhouse, an auger within the channel for directing material toward the feederhouse, and a plurality of crop dividing snouts extending forward from the frame. The reel device is attached to the frame and extends forward from the frame. The reel device has first and second support arms attached to the frame outside the feederhouse and extending forward from the frame, a crossbar rotatably attached in the first and second support arms, radial bars attached to the crossbar positioned over the snouts and on top of the auger, and a crossbar drive to rotate the crossbar and radial bars.
A feature of the present invention includes a 10°-15° bend in the radial bars 5 inches from the attachment point of the radial bars to the cross bar.
A further feature of the present invention is a set of two radial bars for each corn head snout that are separately spaced approximately 180° from one another.
A further feature of the present invention is offsetting adjacent sets of radial bars by 90°.
A further feature of the present invention is a pivotal joint on each of the first and second support arms that permit the reel device to move between a raised position and a lowered position. This pivotal joint has multiple holes where a pin is inserted to allow adjustment of the down position.
A further feature of the present invention are adjustable sections which permit changes in the position of the crossbar relative to the auger, adjustments to the length of the crossbar to permit changes in the position of the support arms relative to the feederhouse, and adjustments to the reel positions to allow changes in the position of the radial bars over the snouts.
A further feature of the present invention is to provide radial bars over at least five snouts that define four crop rows especially those immediately in front of the feederhouse and adjacent the feederhouse. Corn heads configured to harvest 30 inch rows require one set of radial bars per row while 36 and 38 inch rows require 2 sets over the middle 3 snouts or hoods. Corn heads configured for 20 inch rows require one set of radial bars over the middle 7 hoods. The length of the axle or cross bar is the same for both 20″ and 30″ corn heads and longer for the 34″ and 36″ corn heads. Alternatively, the cross bar may have an adjustable length, through telescoping members or extension pieces.
The foregoing objectives may also be achieved by a reel device that may be provided separately from the corn head for later attachment to the corn head. The reel device having support arms attached to the corn head frame, a crossbar rotatably attached between the support arms, radial bars having a first end attached to the crossbar with a 10°-15° bend 5 inches from the attachment point that is designed to move a great amount of debris towards the feederhouse with a minimal propensity to wrap crop debris around the crossbar.
The foregoing objectives may also be achieved with a method of using an improved corn head with a reel device that includes the steps aligning the radial bars over the snouts, harvesting corn using the corn head when environmental conditions produce debris, and operating the reel device to reduce debris build-up.
A further feature of the present invention includes the step of pivoting the reel device to an upper position when not required to remove debris.
A further feature of the present invention is the step comprising adjusting the support bars to place the radial bars over the auger within the range of 1-2″ and preferably 1″ away from the auger flighting and 1-3″ and preferably 2″ away from the hood which is the cover separating each row gathering unit.
A further feature is the provision of radial bars which are non-perpendicular to the axis of the cross bar so as to enhance debris clearance from the feederhouse.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the reel device of the present invention on a corn head of a combine.
FIG. 2A is a side elevation view of the improved corn head with the reel device of the present invention in a lowered, operative position.
FIG. 2B is a side elevation view of the improved corn head with the reel device in a raised, inoperative position.
FIG. 3 is a front elevation view of the improved corn head with the reel device in a lowered position.
FIG. 4 is a front view of an improved corn head with the reel device using radial bars having angled members at an outer end of the radial bars.
FIG. 5 is an enlarged view of the crossbar drive for rotating the cross bar and radial bars and showing an alternative, straight bar embodiment.
FIG. 6 is a view similar to FIG. 3 showing another embodiment of the radial bars oriented at a non-perpendicular angle relative to the cross bar axis.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to the figures and particularly to FIG. 1 , the improved corn head is generally referred to by numeral 10 . The reel device 12 is an improvement to the corn head 10 of a combine 14 that prevents debris build-up in front of the feederhouse 18 .
The corn head 10 has a frame 16 that provides a support structure for the reel 12 . The feederhouse 18 is defined in the frame 16 that provides an opening to move ears of corn and debris from the snouts 23 of the corn head into the internal workings of the combine. A channel 20 is provided on the frame 16 to receive harvested ears of corn and an auger 22 moves the material inwardly from the lateral sides of the corn head 10 to the feederhouse 18 . A hood 21 is the cover in front of the channel that separates each row unit. The frame 16 , feederhouse 18 , channel 20 , hood 21 , auger 22 , and snouts 23 are conventional.
As ears of corn and debris move towards the feederhouse, the corn being heavier than the debris settles into the channel and moves into the feederhouse whereas the debris being lighter than the corn rises to the top of the channel. Under ideal operating conditions, the debris and corn cobs both are fed into the feederhouse simultaneously. Unfortunately, debris may continue to build-up in front of the feederhouse and on top of the hoods until it forms an obstruction and prevents corn from moving into the feederhouse. At this point, an operator would be required to remove the obstruction of debris from the feederhouse. However, with use of the reel device 12 , the debris does not form an obstruction. Instead, as the debris begins to accumulate in front of and on top of the cross auger 22 , it is moved rearward and into the feederhouse 18 .
The reel device 12 has opposite support arms 24 . The support arms 24 are attached to the frame 16 in any convenient manner, such as a bracket or clamp 26 . The bracket or clamp 26 may utilize a threaded fastener, be welded to the frame, and/or utilize other attachment means. Differences in head manufacturer's frame designs are overcome by changing the design of the bracket or clamp 26 . For example, on certain combine models the bracket 26 may be bolted to the front side of the frame directly behind and above the cross auger. Different types of brackets 26 may be used on other corn heads.
Extending between the support arms 24 is a crossbar 30 . The crossbar 30 is rotatably mounted between the support arms 24 . Radial bars 32 extend from the crossbar 30 . As illustrated, each set of two opposing radial bars 32 are spaced 180° apart on the crossbar 30 . These radial bars 32 that comprise a set of crossbars may be offset from one another by 90°. This offsetting provides interaction by the reel device 12 with a debris pile in 90° rotational increments.
As seen in FIGS. 2A and 2B , a pivot point 28 is provided on the support arms 24 that permit the movement of the reel device 12 between a raised inoperative position and a lowered operative position.
The reel device 12 has a variety of different adjustments possible. Each of the support arms 24 is adjustable in length to permit the radial bars 32 to be moved close to or away from the auger 22 . As best seen in FIG. 5 , the arms 24 include telescoping segments 24 A and 24 B with a plurality of holes 25 . A pin or bolt (not shown) extends through one of the holes to secure the segments 24 A and B for a selected length of the arm 24 .
A pair of hinge plates 28 are welded or otherwise fixed to the outer end of the segment 24 B of the support arms 24 , as best seen in FIG. 5 . Each hinge plate has a plurality of holes 29 , which provide numerous pin placements to allow proper positioning or placement of the outer ends of the segments 24 C of the arms 24 relative to the hoods 21 and the auger 22 . More particularly, a pin (not shown) extends through one of the holes 29 , and through the segment 24 C of the arm 24 to pivotally connect the segment 24 C to the hinge plates 28 . A plurality of holes 31 at the forward end of the plates are adapted to receive a pin (not shown) which extends beneath the segment 24 C of the arm 24 to further allow adjustment of the position of the outer end of the segment 24 relative to the hoods 21 and the auger 22 . A hole 31 in the plates 28 is adapted to receive a pin (not shown) to limit upward movement of the reel 12 when the reel is in the lowered, operative position. Another hole 35 on the upper portion of the plates 28 is adapted to receive a pin (not shown) so as to limit rearward movement of the arm segment 24 C when the reel 24 is in the raised, inoperative position. If desired, the arm segments 24 C can be maintained in a substantially vertical position when folded upwardly by a pair of pins received in holes 37 in the upper portion of the hinge plates 28 , with the pins being on opposite sides of the segment 24 C.
As seen in FIGS. 3 and 4 , adjustments may be provided to the crossbar 30 to align the radial bars 32 with the snouts 23 . Additionally, adjustments may be made to the crossbar 30 to assure placement on the outside of the feederhouse 18 .
Each radial bar 32 has a first end 34 connected to the crossbar 30 and a second end spaced outward from the crossbar 30 . The second end may be a blunt end or it may have V-shaped fork 38 which has two angled snouts 40 or may have a single angled snout. In a preferred embodiment, the radial bar is bent approximately 10°-15°, and preferably 12°, 5″ from the attachment point of the ends 34 to the cross bar 30 . This bend in the bars 32 helps to prevent wrapping of cornstalks around the cross bar 30 . The outer end 34 of each radial bar 32 is preferably blunt. In an alternative embodiment, the radial bars 32 A are straight, as seen in FIG. 5 , without the 10°-15° bend. In yet another embodiment, the radial bars 32 B are secured to the cross bar 30 so as to be disposed at a non-perpendicular angle relative to the axis of the cross bar 30 , as seen in FIG. 6 . With such an angle, the bars 32 B cover a wider swath as the cross bar 30 rotates, as compared to the bars 32 .
As illustrated in FIG. 5 , the crossbar 30 is rotated by a drive chain 42 . The drive chain 42 is powered by hydraulic hoses 46 and a hydraulic motor 48 . The hydraulic motor 48 turns the chain 42 which is trained about a sprocket on 44 on the end of the cross bar 30 and a sprocket 50 on the end of the motor 48 . A chain guard 52 prevents the chain from becoming clogged with debris and later falling off and processed through the combine. The hydraulic hoses 46 may be connected to the hydraulic system of the corn head 10 .
In the drawings and specification there has been set forth a preferred embodiment of the invention, and although specific terms are employed, their use is in a generic descriptive sense only and not for purposes of limitation. Changes in the form in proportion and parts as well as in substitution of equivalent are contemplated as a circumstance may suggest or render expedience without departing from the spirit or scope of the invention and various claims. For example, the present invention contemplates variations in the drive system, the number of radial bars utilized, the position of the radial bars 32 relative to the corn head snouts, and other variations in structure and function. | An improved corn head includes a reel device that prevents debris build-up in front of a feederhouse. The reel device includes support arms, a crossbar between the support arms, and a number of radial bars extending from the crossbar. The reel device has a number of adjustments to optimally position the radial bars for removing debris. The reel device rotates to reduce debris build-up in the feederhouse during harvesting. The reel device is moveable between operative and inoperative positions from the combine cab using hydraulics. | 0 |
TECHNICAL FIELD
[0001] The present invention relates to an air conditioner that performs defrosting operation and a defrosting operation method for the air conditioner.
BACKGROUND ART
[0002] When a heat pump type air conditioner is operated for heating, frost is sometimes deposited on the surface of an outdoor heat exchanger (a heat source side heat exchanger). When the frost closes an air duct between fins in the outdoor heat exchanger, heat exchange performance of the outdoor heat exchanger is deteriorated and a sufficient heating capacity cannot be obtained. Therefore, it is necessary to periodically determine a frosting state of the outdoor heat exchanger and remove the frost.
[0003] As a method of removing the frost, there have been known a reverse cycle defrosting operation for switching a four-way valve to a cooling operation side to remove the frost and a hot gas bypass defrosting operation for providing a hot gas bypass circuit bypassed from a compressor discharge side and including an on-off valve, connecting the circuit to an outdoor heat exchanger inlet side, and feeding a part of a compressor discharge gas refrigerant to an outdoor heat exchanger to remove the frost.
[0004] As a conventional technique for switching the hot gas bypass defrosting operation and the reverse cycle defrosting operation to perform defrosting operation, for example, there is a technique described in Patent Literature 1 (JP-A-2008-96033). Patent Literature 1 describes an invention for, when detecting frosting on an outdoor heat exchanger, switching a four-way valve to perform the reverse cycle defrosting operation and, when a pipe heat storage amount serving as a defrosting heat source detected by heat-storage-amount detecting means is equal to or smaller than a set value, switching the four-way valve to a regular cycle side and opening a hot gas bypass on-off valve to perform the hot gas bypass defrosting operation.
[0005] As another conventional technique, there is a technique described in Patent Literature 2 (JP-A-2011-144960). Patent Literature 2 describes an invention for, in an air conditioner including two defrosting operation systems of defrosting operation of a hot gas bypass system and defrosting operation of a reverse (reverse cycle) system, carrying out defrosting by the reverse system when the number of revolutions of a compressor is equal to or larger than a predetermined number of revolutions and increasing the number of revolutions of the compressor and performing the defrosting operation according to the hot gas bypass system when the number of revolutions of the compressor is smaller than the predetermined number of revolutions.
CITATION LIST
Patent Literature
Patent Literature 1: JP-A-2008-96033
Patent Literature 2: JP-A-2011-144960
SUMMARY OF INVENTION
Technical Problem
[0006] In the hot gas bypass defrosting operation, it is possible to simultaneously perform heating operation and defrosting operation by bypassing the refrigerant discharged from the compressor. Since the four-way valve is not switched and a freezing cycle is not switched to a reverse cycle, it is possible to accelerate a rise in a room temperature after the defrosting.
[0007] However, in the hot gas bypass defrosting operation, since energy of the bypassed refrigerant is used for the defrosting, a heating capacity decreases. When a frosting amount is large, the defrosting operation is long compared with the reverse cycle defrosting system. Therefore, there is a problem in that a total heating capacity during air conditioner operation decreases when the frosting amount is large compared with the reverse cycle defrosting system.
[0008] In the reverse cycle defrosting operation, since a flow of the refrigerant is switched to a cooling side to feed the refrigerant having high temperature to the outdoor heat exchanger acting as an evaporator, a high defrosting capacity is obtained. Therefore, when the frosting mount is large, compared with the hot gas bypass defrosting operation, it is possible to complete the defrosting operation in a short time in the reverse cycle defrosting operation. If the defrosting operation can be ended in a short time, it is possible to secure a long heating operation time. Therefore, it is possible to suppress the decrease in the total heating capacity during the air conditioner operation.
[0009] However, when the reverse cycle defrosting operation is performed, it is necessary to switch the freezing cycle from the regular cycle to the reverse cycle. When the freezing cycle is switched to the reverse cycle, the heating operation is suspended. Since an indoor heat exchanger acts as an evaporator during the defrosting operation, temperature drops and a room temperature drop increases. The temperature of a refrigerant pipe connected to the indoor heat exchanger also drops. Therefore, even if the defrosting operation is ended to start the heating operation, time required for startup of the heating operation is longer than the time in the case of the hot gas bypass defrosting operation. Therefore, there is a problem in that, when the frosting amount is small, in the reverse cycle defrosting operation, a total of a defrosting operation time and time required for a room temperature rise after the defrosting is long compared with when the hot gas bypass defrosting operation is performed.
[0010] An object of the present invention is to obtain an air conditioner and a defrosting operation method for the air conditioner that can reduce time for defrosting, which is a total of times required for defrosting operation and heating operation startup after the defrosting operation, to thereby suppress a decrease in a total heating capacity during air conditioner operation.
Solution to Problem
[0011] In order to achieve the object, according to an aspect of the present invention, there is provided an air conditioner in which a compressor, a four-way valve, a use side heat exchanger, an expansion valve, and a heat source side heat exchanger are connected to configure a freezing cycle. The air conditioner includes: a hot gas bypass circuit that connects a discharge side of the compressor and a portion between the heat source side heat exchanger and the expansion valve; an on-off valve that opens and closes a channel of the hot gas bypass circuit; and a control device that performs control to select one of hot gas bypass defrosting operation and reverse cycle defrosting operation according to a frosting amount on the heat source side heat exchanger and perform defrosting operation. When executing the hot gas bypass defrosting operation, the control device performs control to open the on-off valve of the hot gas bypass circuit such that a part of a refrigerant discharged from the compressor is supplied to the heat source side heat exchanger via the hot gas bypass circuit and, when executing the reverse cycle defrosting operation, the control device performs operation to switch the four-way valve such that the refrigerant discharged from the compressor is supplied to the heat source side heat exchanger after passing through the four-way valve.
[0012] According to another aspect of the present invention, there is provided a defrosting operation method for an air conditioner including a heat source side heat exchanger and configured to be capable of performing defrosting operation for frost deposited on the heat source side heat exchanger. The air conditioner is configured to be capable of carrying out both of hot gas bypass defrosting operation and reverse cycle defrosting operation. The defrosting operation method includes: detecting a frosting amount on the heat source side heat exchanger; and selecting one of the hot gas bypass defrosting operation or the reverse cycle defrosting operation to carry out defrosting operation according to the detected frosting amount on the heat source side heat exchanger.
Advantageous Effect of Invention
[0013] According to the present invention, there is an effect that it is possible to obtain an air conditioner and a defrosting operation method for the air conditioner that can reduce time for defrosting, which is a total of times required for defrosting operation and heating operation startup after the defrosting operation, to thereby suppress a decrease in a total heating capacity during air conditioner operation.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a freezing cycle configuration diagram (a refrigerant circuit diagram) showing a first embodiment of an air conditioner of the present invention.
[0015] FIG. 2 is a flowchart showing operation for controlling defrosting operation in the first embodiment.
[0016] FIG. 3 is a flowchart showing operation for controlling defrosting operation in a second embodiment.
[0017] FIG. 4 is a flowchart showing operation for controlling defrosting operation in a third embodiment.
[0018] FIG. 5 is a flowchart showing operation for controlling defrosting operation in a fourth embodiment.
[0019] FIG. 6 is a graph for explaining a method of determining a set value of an outdoor heat exchanger temperature with respect to an outdoor air temperature.
[0020] FIG. 7 is a diagram for explaining selection of a defrosting system based on a power ratio in an outdoor blower before and after frosting and the outdoor heat exchanger temperature.
DESCRIPTION OF EMBODIMENTS
[0021] Specific embodiments of an air conditioner and a defrosting operation method for the air conditioner of the present invention are explained with reference to the drawings. Note that, in the figures, portions denoted by the same reference numerals and signs denote the same or equivalent portions.
First Embodiment
[0022] A first embodiment of the present invention is explained with reference to FIG. 1 and FIG. 2 . FIG. 1 is a freezing cycle configuration diagram (a refrigerant circuit diagram) showing a first embodiment of an air conditioner of the present invention. FIG. 2 is a flowchart showing operation for controlling defrosting operation in the first embodiment.
[0023] First, the configuration of the air conditioner in the first embodiment is explained with reference to FIG. 1 .
[0024] The air conditioner is configured by an outdoor machine (an outdoor unit) 1 and an indoor machine (an indoor unit) 2 connected to the outdoor machine 1 by refrigerant pipes 11 and 12 ( 11 : a gas pipe, 12 : a liquid pipe).
[0025] The outdoor machine 1 is configured by a compressor 3 configured by a scroll compressor or the like, a four-way valve 4 , an outdoor heat exchanger (a heat source side heat exchanger) 5 , an outdoor expansion valve 6 configured by an electronic expansion valve, a throttle opening of which is variable, and the like, an outdoor machine side gas prevention valve 7 connected to the gas pipe 11 side, an outdoor machine side liquid prevention valve 8 connected to the liquid pipe 12 side, and the like. A gas header (a gas branch pipe) 5 a and a liquid header (a liquid branch pipe) 5 b are provided in the outdoor heat exchanger 5 .
[0026] Reference numeral 9 denotes a hot gas bypass circuit that connects a refrigerant pipe between a discharge side of the compressor 3 and the four-way valve 4 and a refrigerant pipe between the outdoor heat exchanger 5 and the outdoor expansion valve 6 . A hot gas bypass on-off valve (an on-off valve) 10 is provided in the hot gas bypass circuit 9 . A channel of the hot gas bypass circuit 9 is opened and closed by the hot gas bypass on-off valve 10 , whereby hot gas bypass defrosting operation can be executed.
[0027] Reference numeral 13 denotes an outdoor blower for blowing outdoor air to the outdoor heat exchanger 5 as indicated by a white arrow in the figure to cause the outdoor air and a refrigerant flowing in a heat transfer pipe (a refrigerant pipe) in the outdoor heat exchanger 5 to exchange heat. Reference numeral 14 denotes an outdoor air temperature thermistor provided on an air (outdoor air) suction side near the outdoor heat exchanger 5 and for detecting an outdoor air temperature (an air temperature). Reference numeral 15 denotes a heat exchanger temperature thermistor that detects the temperature of the refrigerant pipe between the outdoor heat exchanger 5 and the liquid header 5 b of the outdoor heat exchanger 5 . The heat exchanger temperature thermistor 15 is a thermistor for detecting the temperature of the outdoor heat exchanger 5 . The heat exchanger temperature thermistor 15 only has to be provided in a portion where the temperature of the outdoor heat exchanger 5 can be measured. For example, by providing the heat exchanger temperature thermistor 15 in a portion with a large number of liquid phases (the liquid header 5 b side) of the outdoor heat exchanger 5 , it is possible to more stably measure the heat exchanger temperature than when the heat exchanger temperature thermistor 15 is provided on the gas header 5 a side.
[0028] The indoor machine 2 is configured by an indoor heat exchanger (a use side heat exchanger) 16 , an indoor expansion valve 17 configured by an electronic expansion valve, a throttle opening of which is variable, or the like, an indoor machine side gas prevention valve 18 connected to the gas pipe 11 side, an indoor machine side liquid prevention valve 19 connected to the liquid pipe 12 side, and the like. A gas header (a gas branch pipe) 16 a and a liquid header (a liquid branch pipe) 16 b are also provided in the outdoor heat exchanger 16 .
[0029] The outdoor machine 1 and the indoor machine 2 are connected by the refrigerant pipes 11 and 12 , whereby the compressor 3 , the four-way valve 4 , the outdoor heat exchanger 5 , the outdoor expansion valve 6 , the indoor expansion valve 17 , and the indoor heat exchanger 16 are sequentially connected by the refrigerant pipe to configure a freezing cycle.
[0030] The four-way valve 4 is a valve for switching a direction of a flow of the refrigerant. During the heating operation, the four-way valve 4 switches the refrigerant circuit to connect the discharge side of the compressor 3 and the indoor heat exchanger 16 and connect the suction side of the compressor 3 and the outdoor heat exchanger 5 .
[0031] During the cooling operation and during the reverse cycle defrosting operation, the four-way valve 4 switches the refrigerant channel to connect the discharge side of the compressor 3 and the outdoor heat exchanger 5 and connect the suction side of the compressor 3 and the indoor heat exchanger 16 .
[0032] The outdoor heat exchanger 5 is configured by, for example, a fin-and-tube type heat exchanger of a cross fin type configured by a heat transfer pipe and a large number of fins provided to cross the heat transfer pipe. A gas side of the outdoor heat exchanger 5 is connected to the four-way valve 4 and a liquid side of the outdoor heat exchanger 5 is connected to the outdoor expansion valve 6 . The outdoor heat exchanger 5 functions as a condenser for the refrigerant during the cooling operation and functions as an evaporator for the refrigerant during the heating operation.
[0033] The indoor heat exchanger 16 is also configured by, for example, a fin-and-tube type heat exchanger of the cross fin type configured by a heat transfer pipe and a larger number of fins. The indoor heat exchanger 16 functions as an evaporator for the refrigerant during the cooling operation and cools the air in a room. The indoor heat exchanger 16 functions as a condenser for the refrigerant during the heating operation and heats the air in the room.
[0034] The outdoor expansion valve 6 and the indoor expansion valve 17 are disposed in the refrigerant pipe between the outdoor heat exchanger 5 and the indoor heat exchanger 16 . The outdoor expansion valve 6 and the indoor expansion valve 17 adjust the throttle openings thereof to thereby perform, for example, adjustment of a flow rate of the refrigerant flowing to the refrigerant circuit.
[0035] The air conditioner is configured to be capable of performing the hot gas bypass defrosting operation and the reverse cycle defrosting operation in order to melt and remove frost deposited on the outdoor heat exchanger 5 . In this embodiment, the air conditioner is controlled by a control device (not shown in the figure) to detect or estimate a frosting amount on the outdoor heat exchanger 5 and perform the hot gas bypass defrosting operation when the frosting amount is relatively small and carry out the reverse cycle defrosting operation when the frosting amount is large.
[0036] For example, if a ratio of an area of frosting (hereinafter referred to as frosted area) is less than 20 to 30% with respect to a heat transfer area in the outdoor heat exchanger 5 , the air conditioner determines that frosting is little and continues the heating operation. If the ratio is 20 to 30% or more, the air conditioner carries out the defrosting operation. When the defrosting operation is carried out, in this embodiment, the air conditioner carries out the hot gas bypass defrosting operation when the frosting amount is relatively small (when the ratio is approximately 20 to 80%) and carries out the reverse cycle defrosting operation when the frosting amount is large (when the ratio is 80% or more).
[0037] In the air conditioner configured as explained above, during the heating operation, the refrigerant flows and circulates as indicated by solid line arrows. That is, during the heating operation, the refrigerant having high temperature and high pressure discharged from the compressor 7 flows into the indoor heat exchanger 16 through the four-way valve 4 switched to the heating side. The air sucked by the indoor machine 2 and the refrigerant flowing in the heat transfer pipe perform heat exchange, whereby the refrigerant condenses and changes to a liquid refrigerant. At this point, heat radiated from the refrigerant is given to the air on the indoor side, whereby heating is performed. The liquid refrigerant flowing out from the indoor heat exchanger 16 expands when flowing through the indoor expansion valve 17 and the outdoor expansion valve 6 and flows into the outdoor heat exchanger 5 in a low-temperature and low-pressure state. The outdoor heat exchanger 5 functions as an evaporator. The refrigerant evaporates and changes to a gas refrigerant by performing heat exchange with the air outside the room (the outdoor air) sucked by the outdoor machine 1 . Therefore, the refrigerant is sucked by the compressor 3 again through the four-way valve 4 .
[0038] During the hot gas bypass defrosting operation, a part of the high-temperature refrigerant discharged from the compressor 3 flows to the hot gas bypass circuit 9 as indicated by arrows of alternate long and two short dashes lines. The gas refrigerant having high temperature is fed to the outdoor heat exchanger 5 to defrost the outdoor heat exchanger 5 .
[0039] During the reverse cycle defrosting operation and during the cooling operation, the refrigerant circulates as indicated by arrows of dotted lines. That is, the gas refrigerant having high temperature and high pressure discharged from the compressor 3 flows to the outdoor heat exchanger 5 and condenses. During the reverse cycle defrosting operation, the gas refrigerant heats and defrosts the outdoor heat exchanger 5 with condensation heat during the condensation. Thereafter, the refrigerant flows to the indoor heat exchanger 16 side and evaporates, changes to the gas refrigerant, and circulates to return to the compressor 3 again.
[0040] Operation for controlling, in the air conditioner in this embodiment, when frost is deposited on the outdoor heat exchanger 3 by the heating operation, the defrosting operation for removing the frost is explained according to FIG. 2 with reference to FIG. 1 as well.
[0041] FIG. 2 is a flowchart showing operation for controlling the defrosting operation in this embodiment. The operation is explained below according to the flowchart.
[0042] First, the air conditioner is started (step S 0 ) and the heating operation is started (step S 1 ). Thereafter, in step S 2 , the air conditioner detects a frosting amount on the outdoor heat exchanger 5 due to the heating operation with, for example, means for detecting the temperature of the outdoor heat exchanger 5 . That is, in step S 2 , frosting amount detection is performed by means for, for example, calculating a correlation between temperature and a frosting amount of the outdoor heat exchanger 5 in advance through an experiment or the like and estimating, on the basis of the correlation, a frosting amount from temperature detected by the heat exchanger temperature thermistor 15 .
[0043] Subsequently, the air conditioner shifts to step S 3 , the air conditioner determines whether the detected frosting amount is equal to or smaller than a predetermined set temperature. In step S 3 , when the detected frosting amount is equal to or smaller than the set value (in the case of YES), the air conditioner determines that the frosting amount is small, shifts to step S 4 , and performs the defrosting operation in the hot gas bypass system, that is, the hot gas bypass defrosting operation. If the hot gas bypass defrosting operation ends (step S 5 ), the air conditioner returns to S 1 and returns to the heating operation.
[0044] On the other hand, when the detected frosting amount exceeds the predetermined set value in step S 3 (in the case of NO), the air conditioner determines that the frosting amount is large, shifts to step S 6 , and performs the defrosting operation in the reverse cycle system, that is, the reverse cycle defrosting operation. If the reverse cycle defrosting operation ends (step S 7 ), the air conditioner returns to step S 1 and returns to the heating operation.
[0045] In this way, in this embodiment, in starting the defrosting operation, the air conditioner detects (estimates) a frosting amount on the outdoor heat exchanger 5 , according to the frosting amount, selects and carries out the hot gas bypass defrosting operation when the frosting amount is small and selects and carries out the reverse cycle defrosting operation when the frosting amount is larger than the predetermined set value. Therefore, it is possible to suppress a decrease in the total heating capacity during the air conditioner operation by the defrosting operation.
[0046] That is, in this embodiment, the defrosting system is selected according to the frosting amount such that time for defrosting, which is a total of times required for the defrosting operation and the heating operation startup after the defrosting operation, decreases.
[0047] Explaining more in detail, in the reverse cycle defrosting operation, although the defrosting operation time can be reduced, the time required for the heating startup after the defrosting operation is long. Therefore, the reverse cycle defrosting operation is carried out when the frosting amount is large. When the frosting amount is small, the hot gas bypass defrosting operation is carried out. In the hot gas bypass defrosting operation, although the defrosting operation time is long, a room temperature rise after the defrosting operation can be accelerated and the heating operation startup is fast. Therefore, when the frosting amount is small, the times required for the defrosting operation and the heating operation startup after the defrosting operation can be reduced to be shorter than when the reverse cycle defrosting operation is selected.
[0048] Note that, in step S 2 , if the air conditioner continues the frosting amount detection after the heating start and proceeds to step S 3 when the detected frosting amount exceeds a reference value or the heating operation time exceeds a fixed time, it is possible to prevent the defrosting operation from being frequently repeated. The frosting amount detection in step S 2 may be performed in every fixed time. Further, in order to carry out the defrosting operation when the frosting amount is small, it is also possible to set the set value in step S 3 in two stages and, when frosting is absent or extremely little, return to step S 1 without performing the defrosting operation and, only in the case of a frosting amount in which the defrosting operation should be performed, select step S 4 or S 6 to perform the defrosting operation.
[0049] Concerning means for detecting (estimating) a frosting amount, besides means for, for example, detecting the temperature of the outdoor heat exchanger 5 , it is also possible to estimate the frosting amount by detecting a compressor suction pressure closely related to an outdoor heat exchanger temperature. The frosting amount may be estimated according to a change in electric power consumed by the blower (the outdoor blower) 13 of the outdoor heat exchanger (the heat source side heat exchanger). Further, it is also possible to directly detect the frosting amount.
Second Embodiment
[0050] A second embodiment of the present invention is explained with reference to FIG. 3 . FIG. 3 is a flowchart showing operation for controlling defrosting operation in the second embodiment. Note that the configuration of an air conditioner is the same as the configuration shown in FIG. 1 . The second embodiment is explained with reference to FIG. 1 as well.
[0051] In FIG. 3 , steps S 0 , S 1 , and S 4 to S 7 are the same as the steps shown in FIG. 2 . Therefore, explanation of the steps is omitted.
[0052] The second embodiment describes an example in which steps S 2 and S 3 in FIG. 2 are made more specific. In step S 8 in FIG. 3 , the detection of a frosting amount in step S 2 in FIG. 2 is performed by calculating a power ratio of the outdoor blower 13 before and after frosting on the outdoor heat exchanger 5 and using the power ratio.
[0053] Power (power consumption) of the outdoor blower 13 can be calculated from the following expression by detecting an electric current flowing to a motor of the outdoor blower 13 . Note that a voltage and a power factor are fixed.
[0000] Power=voltage×current×power factor
[0054] Therefore, it is possible to calculate a power ratio “P 2 /P 1 ” by calculating electric power P 1 of the outdoor blower 13 before frosting on the outdoor heat exchanger 5 and electric power P 2 of the outdoor blower 13 after the frosting.
[0055] A relation between a power ratio and a frosting amount is calculated in advance by an experiment or the like. When the number of revolutions of the outdoor blower 13 is fixed, electric power (power consumption) before frosting is small because ventilation resistance of the outdoor heat exchanger 5 is small. However, when frosting proceeds, since the ventilation resistance gradually increases, the power consumption increases. Therefore, it is possible to estimate a frosting amount by calculating a power ratio of the outdoor blower 13 before and after frosting of the outdoor heat exchanger 5 .
[0056] Subsequently, in step S 9 , the air conditioner determines on the basis of the power ratio calculated in step S 8 whether the power ratio in the outdoor blower 13 is equal to or larger than a predetermined set value R 1 . The set value R 1 is a value of a power ratio corresponding to a case in which the ratio of the area of frosting (the frosting area) is, for example, approximately 20 to 30% with respect to the heat transfer area in the outdoor heat exchanger 5 .
[0057] When the power ratio is smaller than the set value R 1 in the determination in step S 9 (in the case of NO), the air conditioner returns to step S 1 and continues the heating operation. When the power ratio is equal to or larger than the set value R 1 (in the case of YES), the air conditioner shifts to step S 10 .
[0058] In step S 10 , the air conditioner determines on the basis of the power ratio calculated in step S 8 whether the power ratio in the outdoor blower 13 is equal to or larger than a predetermined set value R 2 . The set value R 2 is a value of a power ratio corresponding to a case in which the ratio of the area of frosting (the frosting area) is, for example, approximately 80% with respect to the heat transfer area in the outdoor heat exchanger 5 . Therefore, the set value R 2 is a value larger than the set value R 1 .
[0059] When the power ratio is equal to or smaller than the set value R 2 in the determination in step S 10 (in the case of YES), the air conditioner determines that the frosting amount is relatively small (the ratio of the frosting area is approximately 20 to 80%), shifts to step S 4 , and carries out the hot gas bypass defrosting operation.
[0060] When the power ratio is larger than the set value R 2 in the determination of step S 10 (in the case of NO), the air conditioner determines that the frosting amount is large (the ratio of the frosting area is higher than approximately 80%). In this case, the air conditioner shifts to step S 6 and carries out the reverse cycle defrosting operation.
[0061] If the defrosting operation in step S 4 or step S 6 ends (step S 5 or S 7 ), the air conditioner returns to the heating operation in step S 1 .
[0062] In this way, according to the second embodiment, the air conditioner estimates the frosting amount according to the power ratio of the outdoor blower before and after frosting of the outdoor heat exchanger 5 and selects and carries out the hot gas bypass defrosting operation when the frosting amount is small and selects and carries out the reverse cycle defrosting operation when the frosting amount is larger than the predetermined set value. Therefore, it is possible to reduce time for defrosting, which is a total of times required for defrosting operation and heating operation startup after the defrosting operation, and suppress a decrease in a total heating capacity during air conditioner operation.
[0063] Note that, in the second embodiment, the power ratio is calculated and the frosting amount is estimated. However, even if a current ratio is used instead of the power ratio, it is possible to estimate the frosting amount in the same manner. That is, if values of electric currents flowing to the motor of the outdoor blower 13 before and after frosting of the outdoor heat exchanger 5 are detected, a ratio (a current ratio) of the current values before and after the frosting is calculated, and a relation between the current ratio and the frosting amount is calculated in advance by an experiment or the like, it is also possible to estimate the frosting amount.
Third Embodiment
[0064] A third embodiment of the present invention is explained with reference to FIG. 4 . FIG. 4 is a flowchart showing operation for controlling defrosting operation in the third embodiment. Note that, in this embodiment as well, the configuration of an air conditioner is the same as the configuration shown in FIG. 1 . The third embodiment is explained with reference to FIG. 1 as well.
[0065] In FIG. 4 , in this embodiment as well, steps S 0 , S 1 , and S 4 to S 7 are the same as the steps shown in FIG. 2 . Therefore, explanation of the steps is omitted.
[0066] The third embodiment also describes an example in which steps S 2 and S 3 in FIG. 2 are made more specific. In step S 11 in FIG. 4 , the detection of a frosting amount in step S 2 in FIG. 2 is performed by detecting the temperature of the outdoor heat exchanger 5 with the heat exchanger temperature thermistor 15 and using the temperature.
[0067] That is, when frost is deposited on the outdoor heat exchanger 5 , since heat exchange efficiency is deteriorated, the number of revolutions of the compressor 3 increases. As a result, evaporation pressure in the outdoor heat exchanger 5 drops and the temperature of the outdoor heat exchanger 5 also drops according to the drop of the evaporation pressure. Therefore, if a relation between the temperature of the outdoor heat exchanger 5 and the frosting amount is calculated in advance by an experiment or the like, it is possible to estimate a frosting amount on the outdoor heat exchanger 5 by detecting the temperature of the outdoor heat exchanger 5 .
[0068] Subsequently, in step S 12 , the air conditioner determines on the basis of the temperature of the outdoor heat exchanger 5 detected by the heat exchanger temperature thermistor 15 in step S 11 whether the temperature of the outdoor heat exchanger 5 is equal to or smaller than a predetermined set value T 1 . The set value T 1 is a value of temperature corresponding to a case in which the ratio of the area of frosting (the frosting area) is, for example, approximately 20 to 30% with respect to the heat transfer area in the outdoor heat exchanger 5 .
[0069] When a value of the temperature is larger than the set value T 1 in the determination in step S 12 (in the case of NO), the air conditioner returns to step S 1 and continues the heating operation. When the value of the temperature is equal to or smaller than the set value T 1 (in the case of YES), the air conditioner shifts to step S 13 .
[0070] In step S 13 , the air conditioner determines on the basis of the temperature of the outdoor heat exchanger 5 detected in step S 11 whether the temperature of the outdoor heat exchanger 5 is equal to or larger than a predetermined set value T 2 . The set value T 2 is a value of temperature corresponding to a case in which the ratio of the area of frosting (the frosting area) is, for example, approximately 80% with respect to the heat transfer area in the outdoor heat exchanger 5 . Therefore, the set value T 2 is a value smaller than the set value T 1 .
[0071] When the value of the temperature is larger than the set value T 2 in the determination in step S 13 (in the case of YES), the air conditioner determines that the frosting amount is relatively small (the ratio of the frosting area is approximately 20 to 80%), shifts to step S 4 , and carries out the hot gas bypass defrosting operation.
[0072] When the value of the temperature is smaller than the set value T 2 in the determination in step S 13 (in the case of NO), the air conditioner determines that the frosting amount is large (the ratio of the frosting area is equal to or larger than approximately 80%). In this case, the air conditioner shifts to step S 6 and carries out the reverse cycle defrosting operation.
[0073] If the defrosting operation in step S 4 or step S 6 ends (step S 5 or S 7 ), the air conditioner returns to the heating operation in step S 1 again.
[0074] In this way, according to the third embodiment, the air conditioner estimates the frosting amount according to the temperature of the outdoor heat exchanger 5 detected by the heat exchanger temperature thermistor 15 and selects and carries out the hot gas bypass defrosting operation when the frosting amount is small and selects and carries out the reverse cycle defrosting operation when the frosting amount is larger than the predetermined set value. Therefore, as in the first and second embodiments, it is possible to reduce time for defrosting, which is a total of times required for defrosting operation and heating operation startup after the defrosting operation, and suppress a decrease in a total heating capacity during air conditioner operation.
[0075] Note that, in the third embodiment, the temperature (evaporation temperature) of the outdoor heat exchanger 5 is detected and the frosting amount is estimated. However, even if pressure (evaporation pressure) on a compressor suction side, that is, a lower pressure side from the outdoor expansion valve 6 to the suction side of the compressor 3 is detected instead of the temperature of the outdoor heat exchanger 5 , it is possible to estimate the frosting amount in the same manner. That is, if a pressure sensor is provided on the suction side of the compressor 3 to detect low-pressure side pressure and a relation between the low-pressure side pressure and the frosting amount is calculated in advance by an experiment or the like, it is also possible to estimate the frosting amount.
Fourth Embodiment
[0076] A fourth embodiment of the present invention is explained with reference to FIGS. 5 to 7 . In this embodiment as well, the configuration of an air conditioner is the same as the configuration shown in FIG. 1 . The fourth embodiment is explained with reference to FIG. 1 as well.
[0077] FIG. 5 is a flowchart showing operation for controlling defrosting operation in the fourth embodiment.
[0078] In FIG. 5 , in this embodiment as well, steps S 0 , S 1 , and S 4 to S 7 are the same as the steps shown in FIG. 2 . Therefore, explanation of the steps is omitted.
[0079] In the fourth embodiment, steps S 11 , S 12 , and S 13 shown in FIG. 5 are the same as steps S 11 , S 12 , and S 13 in the third embodiment shown in FIG. 4 . Further, steps S 8 , S 9 , and S 10 in the fourth embodiment are the same as steps S 8 , S 9 , and S 10 in the second embodiment shown in FIG. 3 .
[0080] The fourth embodiment also describes an example in which steps S 2 and S 3 in FIG. 2 are made more specific. That is, in step S 11 in FIG. 5 , the detection of a frosting amount in step S 2 in FIG. 2 is performed by detecting the temperature of the outdoor heat exchanger 5 in the outdoor heat exchanger 5 with the heat exchanger temperature thermistor 15 . Further, in step S 8 in FIG. 5 , a power ratio of the outdoor blower 13 before and after frosting on the outdoor heat exchanger 5 is calculated and the detection of a frosting amount is performed using the power ratio as well. In this way, in the fourth embodiment, the frost amount detection in step S 2 is performed using both of the temperature of the outdoor heat exchanger 5 and the power ratio of the outdoor air blower before and after frosting on the outdoor heat exchanger 5 .
[0081] In this embodiment, first, in step S 11 , as in the third embodiment, the air conditioner detects the temperature of the outdoor heat exchanger 5 with the heat exchanger temperature thermistor 15 . Further, in step S 8 , as in the second embodiment, the air conditioner calculates a power ratio of the outdoor blower 13 before and after frosting on the outdoor heat exchanger 5 .
[0082] Subsequently, in steps S 12 and S 13 , the air conditioner performs operation same as the operation in the third embodiment.
[0083] That is, in step S 12 , the air conditioner determines on the basis of the temperature of the outdoor heat exchanger 5 detected by the heat exchanger temperature thermistor 15 in step S 11 whether the temperature of the outdoor heat exchanger 5 is equal to or smaller than the predetermined set value T 1 . When a value of the temperature is larger than the set value T 1 (in the case of NO) in the determination in step S 12 , the air conditioner returns to step S 1 and continues the heating operation. When the value of the temperature is equal to or smaller than the set value T 1 (in the case of YES), the air conditioner shifts to step S 13 .
[0084] In step S 13 , the air conditioner determines on the basis of the temperature of the outdoor heat exchanger 5 detected in step S 11 whether the temperature of the outdoor heat exchanger 5 is equal to or larger than the predetermined set value T 2 . When the value of the temperature is smaller than the set value T 2 in the determination of step S 13 (in the case of NO), the air conditioner determines that the frosting amount is large. In this case, the air conditioner shifts to step S 6 and carries out the reverse cycle defrosting operation.
[0085] In this embodiment, when the value of the temperature is larger than the set value T 2 in the determination in step S 13 (in the case of YES), the air conditioner shifts to step S 9 .
[0086] In step S 9 , the air conditioner determines on the basis of the power ratio calculated in step S 8 whether the power ratio in the outdoor blower 13 is equal to or larger than the predetermined set value R 1 . When the power ratio is smaller than the set value R 1 in the determination in step S 9 (in the case of NO), in this embodiment, even when the temperature of the outdoor heat exchanger 5 is between the set values T 1 and T 2 , the air conditioner determines that the frosting amount has not reached a frosting amount in which the defrosting operation should be performed. The air conditioner returns to step S 1 and continues the heating operation.
[0087] When the power ratio is equal to or larger than the set value R 1 in step S 9 (in the case of YES), the air conditioner shifts to step S 10 .
[0088] In step S 10 , the air conditioner determines on the basis of the power ratio calculated in step S 8 whether the power ratio in the outdoor blower 13 is equal to or larger than the predetermined set value R 2 . When the power ratio in the determination is equal to or smaller than the set value R 2 in step S 9 (in the case of YES), the air conditioner determines that the frosting amount is relatively small, shifts to step S 4 , and carries out the hot gas bypass defrosting operation. When the power ratio is larger than the set value R 2 in the determination in step S 10 (in the case of NO), the air conditioner determines that the frosting amount is large. In this case, the air conditioner shifts to step S 6 and carries out the reverse cycle defrosting operation.
[0089] If the defrosting operation in step S 4 or step S 6 ends (step S 5 or S 7 ), the air conditioner returns to the heating operation in step S 1 again.
[0090] FIG. 6 is a graph for explaining a method of determining the set values T 1 and T 2 of the outdoor heat exchanger temperature with respect to outdoor air temperature. In FIG. 6 , the horizontal axis indicates the outdoor air temperature and the vertical axis indicates the temperature of the outdoor heat exchanger 5 . The outdoor air temperature can be detected by the outdoor air temperature thermistor 14 shown in FIG. 1 . The temperature of the outdoor heat exchanger 5 can be detected by the heat exchanger temperature thermistor 15 .
[0091] A portion of a range A indicated by hatching is a range for determining the set values T 1 and T 2 with respect to the outdoor air temperature. For example, when the outdoor air temperature is 2° C., as shown in FIG. 6 , an upper limit temperature of a portion where a broken line indicating 2° C. and the range A cross is determined as the set value T 1 . A lower limit temperature of the portion where the broken line indicating 2° C. and the range A cross is determined as the set value T 2 .
[0092] When the temperature of the outdoor heat exchanger 5 is higher than the range A, the defrosting operation is not performed and the heating operation is continued. When the temperature of the outdoor heat exchanger 5 is lower than the range A, the reverse cycle defrosting operation is carried out. When the temperature of the outdoor heat exchanger 5 is within the range A, that is, between the set values T 1 and T 2 , depending on determination results in steps S 9 and S 10 , it is highly likely that the hot gas bypass defrosting operation is performed. Note that, in the case of the third embodiment, the hot gas bypass defrosting operation is carried out if the temperature of the outdoor heat exchanger 5 is within the range A.
[0093] As shown in FIG. 6 , the set values T 1 and T 2 of the outdoor heat exchanger temperature for determining the frosting amount are changed according to an outdoor air temperature. When the outdoor air temperature is lower than 2° C., the outdoor heat exchanger temperature is a value lower than the set values T 1 and T 2 . When the outdoor air temperature is higher than 2° C., the outdoor heat exchanger temperature is a value higher than the set values T 1 and T 2 . The set values T 1 and T 2 are determined on the basis of FIG. 6 . The determination in steps S 12 and S 13 is carried out using the set values.
[0094] FIG. 7 is a diagram for explaining selection of a defrosting system based on a power ratio in the outdoor blower 13 before and after frosting and the temperature of outdoor heat exchanger 5 . The horizontal axis indicates a power ratio in the outdoor blower 13 before and after frosting and the vertical axis indicates the temperature of the outdoor heat exchanger 5 detected by the heat exchanger temperature thermistor 15 . When the operation of the flowchart indicating the operation for controlling the defrosting operation shown in FIG. 5 is executed, an appropriate defrosting system is selected as shown in FIG. 7 on the basis of the set values T 1 , T 2 , R 1 , and R 2 described above. The defrosting operation is carried out or the defrosting operation is not carried out and the heating operation is continued.
[0095] That is, when the power ratio and the outdoor heat exchanger temperature are present in a region B surrounded by the set values T 1 , T 2 , R 1 , and R 2 , the hot gas bypass defrosting operation is carried out. When the outdoor heat exchanger temperature is between the set values T 1 and T 2 and the power ratio is equal to or larger than the set value R 2 (a region C) and, when the outdoor heat exchanger temperature is equal to or smaller than the set value T 2 , the reverse cycle defrosting operation is carried out. Further, when the outdoor heat exchanger temperature is between the set values T 1 and T 2 and the power ratio is equal to or smaller than the set value R 1 (a region D) and when the outdoor heat exchanger temperature is equal to or larger than the set value T 1 , the defrosting operation is not performed and the heating operation is continued.
[0096] In this way, according to the fourth embodiment, the frosting amount is estimated according to the temperature of the outdoor heat exchanger 5 detected by the heat exchanger temperature thermistor 15 and the power ratio of the outdoor blower before and after frosting on the outdoor heat exchanger 5 . Therefore, it is possible to accurately estimate that frost is surely deposited on the outdoor heat exchanger 5 and accurately estimate the frosting amount. Therefore, it is possible to prevent erroneous detection of the frosting amount, avoid the defrosting operation when the frosting amount is extremely small, and accurately select according to the more accurately estimated frosting amount whether the hot gas bypass defrosting operation is performed or the reverse cycle defrosting operation is performed. Therefore, it is possible to reduce time for defrosting, which is a total of times required for the defrosting operation and the heating operation startup after the defrosting operation, and suppress a decrease in a total heating capacity during the air conditioner operation.
[0097] Note that the present invention is not limited to the embodiments explained above. Various modifications are included in the present invention. For example, steps S 11 and S 8 in FIG. 5 may be executed in the opposite order or may be simultaneously executed. The execution order of steps S 12 and S 13 and steps S 9 and S 10 may be changed to execute steps S 12 and S 13 after carrying out steps S 9 and S 10 .
[0098] The embodiments are explained in detail in order to clearly explain the present invention and are not always limited to embodiments including all the explained components. Further, a part of the components of a certain embodiment can be replaced with the components of another embodiment. The components of another embodiment can be added to the components of a certain embodiment. Other components can be added to, deleted from, and replaced with a part of the components of the embodiments.
[0099] Programs for realizing the functions and information such as the set values and the set times can be stored in recording devices such as a memory, a hard disk, and an SSD (Solid State Drive) or recording media such as an IC card, an SD card, and a DVD.
REFERENCE SIGNS LIST
[0000]
1 : outdoor machine
2 : indoor machine
3 : compressor
4 : four-way valve
5 : outdoor heat exchanger (heat source side heat exchanger)
5 a : gas header
5 b : liquid header
6 : outdoor expansion valve (expansion valve)
7 : outdoor machine side gas prevention valve
8 : outdoor machine side liquid prevention valve
9 : hot gas bypass circuit
10 : hot gas bypass on-off valve (on-off valve)
11 , 12 : refrigerant pipe
13 : outdoor blower
14 : outdoor air temperature thermistor
15 : heat exchanger temperature thermistor
16 : indoor heat exchanger (use side heat exchanger)
16 a : gas header
16 b : liquid header
17 : indoor expansion valve (expansion valve)
18 : indoor machine side gas prevention valve
19 : indoor machine side liquid prevention valve | A hot gas bypass circuit that connects a discharge side of the compressor and a portion between the heat source side heat exchanger and the expansion valve, an on-off valve that opens and closes a channel of the hot gas bypass circuit, and a control device performing control to select one of hot gas bypass defrosting and reverse cycle defrosting according to a frosting amount on the heat source side heat exchanger and perform defrosting. The control device controls to open the on-off valve of the hot gas bypass circuit such that a part of a refrigerant discharged from the compressor is supplied to the heat source side heat exchanger via the hot gas bypass circuit and, the control device switches switch the four-way valve such that the refrigerant discharged from the compressor is supplied to the heat source side heat exchanger after passing through the four-way valve. | 5 |
TECHNICAL FIELD
[0001] The present invention relates to an apparatus for printing employing flexographic printing technology. In particular, the present invention relates to such an apparatus for printing of a web of packaging material with printing ink, the apparatus comprising an ink pan or chamber and an anilox roll partly rotary within the ink chamber for picking up and transferring printing ink from the ink chamber to a printing cylinder which is rotary in transfer contact with the anilox roll, as well as a counter pressure cylinder which is rotary adjacent the printing cylinder and which, together with the printing cylinder, forms a nip through which the web of packaging material is intended to be led for transferring printing ink from the printing cylinder to the web, the ink pan or chamber extending axially along the anilox roll and displaying an upper axial doctor blade in contact with the circumferential surface of the anilox roll for scraping off excess ink, and a lower similarly axial doctor blade in contact with the circumferential surface of the anilox roll for preventing printing ink from running out from the ink chamber, the ink chamber having a first end wall at its one axial end and a second end wall at its other axial end.
BACKGROUND ART
[0002] In general, flexographic printing of a web of packaging material is carried into effect using a thin-running and often volatile printing ink which implies that the printing ink must be transferred from the ink pan or chamber to the packaging material web before it has had time to dry on route. For this transfer, use is therefore made of a hard roll (anilox roll) which displays on its circumferential surface engraved cells with the aid of which printing ink is taken up from the ink pan or chamber and transferred to the printing cylinder rotary in transfer contact with the anilox roll. In order to facilitate taking up of printing ink from the ink chamber, the anilox roll is rotary in direct contact with the printing ink in the ink chamber. The ink chamber is defined upwardly by an upper axial elongate doctor blade in contact with the circumferential surface of the anilox roll, and downwardly by a lower, similarly axially extending doctor blade in contact with the circumferential surface of the anilox roll. The upper doctor blade, which lightly abuts against the circumferential surface of the anilox roll, is intended to scrape off and recycle picked up excess ink before departure from the ink chamber. The lower doctor blade, which lightly abuts against the circumferential surface of the anilox roll, is intended to prevent printing ink from leaking out from the ink chamber.
[0003] The ink chamber is filled to a predetermined level with continuously circulating printing ink, via an inlet and an outlet to the ink chamber. The quality of the printing ink is continuously regulated in an external unit, in respect of viscosity and temperature and other properties so that a uniform printing result is obtained.
[0004] Both of the axial end walls of the ink chamber may, in a prior art apparatus, extend right up to sealing abutment against the circumferential surface of the anilox roll in order to ensure that as little printing ink as possible leaks out laterally from the ink chamber.
[0005] According to another prior art example, the end walls are disposed in spaced apart relationship from the surface of the anilox roll, in which event sealing against leakage of printing ink through the thus formed gaps between each respective end wall and the circumferential surface of the anilox roll is catered for by means of an observed relationship between the viscosity of the printing ink and the speed of rotation of the anilox roll during ongoing printing. According to this relationship, there is for each viscosity a speed of rotation above which the tendency of the printing ink to accompany the anilox roll is greater than the tendency of the printing ink to leak out from the ink chamber laterally through the thus formed gaps at the axial end wall. Thus, this prior art embodiment affords the advantage in relation to the previously described embodiment that it requires no frequently recurring operational stoppage for replacement of worn rubber seals. A further advantage is that it causes no wear, or very slight wear, to the anilox roll because of friction heat as described above.
[0006] One drawback inherent in this latter described embodiment is however that it not seldom occurs that residual printing ink on the circumferential surface of the anilox roll, after transfer of printing ink to the printing cylinder, dries and adheres to the anilox roll and as a result cannot be scraped off by the doctor blades, but accompanies the anilox roll into the ink pan or chamber when the anilox roll is rotated during operation. Such drying of printing ink is repeated turn after turn which the anilox roll rotates and leads to an increasing accumulation of dried printing ink which gradually grows in the radial direction and progressively lifts both the lower and the upper doctor blade, with consequentially increased losses of printing ink from the ink chamber.
[0007] A further drawback which is associated with both of the above described prior art embodiments is that the ink picking up engraved cells on the circumferential surface of the anilox roll, after transfer of the picked up printing ink to the printing cylinder are filled with air which passes beneath the lower doctor blade and accompanies the anilox roll into the ink chamber where it is released and accumulates along an axial stretch between the axial end walls of the ink chamber. According as the accumulated air volume inside the ink chamber increases, the risk also increases that air fills the whole or parts of the engraved cells on the roll surface and thereby prevents these cells from taking up printing ink.
[0008] There is thus still a need in the art for an improved apparatus for flexographic printing of a web of packaging material.
Objects of the Invention
[0009] One object of the present invention is thus to obviate the above-described drawbacks inherent in the prior art apparatuses for flexographic printing of a web of packaging material.
[0010] A further object of the present invention is to realise an apparatus of the type described by way of introduction without suffering from the problems and drawbacks of the type described above.
[0011] Further objects and advantages of the present invention will be apparent from the following description.
Brief Outline of the Invention
[0012] According to one aspect of the present invention, there will thus be realised an apparatus for printing of a web of packaging material with printing ink, the apparatus comprising an ink pan or chamber and an anilox roll rotary partly inside the ink chamber for taking up and transferring printing ink from the ink chamber to a rotary printing cylinder in transfer contact with the anilox roll, as well as a further counter pressure cylinder which is rotary adjacent the printing cylinder and which, together with the printing cylinder, forms a nip through which the web of packaging material is intended to be led for transferring printing ink from the printing cylinder to the web, the ink pan or chamber extending axially along the anilox roll and displaying an upper axial doctor blade in contact with the circumferential surface of the anilox roll for scraping off excess ink, and a lower, similarly axial doctor blade in contact with the circumferential surface of the anilox roll for preventing printing ink from running out from the ink chamber, the ink chamber displaying a first end wall at its one axial end and a second end wall at its other axial end. The apparatus according to the invention is characterised in that it includes at least one spray- or shower device provided with a nozzle, which has its nozzle directed to peripheral circumferential edge regions of the circumferential surface of the anilox roll for supplying a cleaning fluid to these regions for removing and thereby preventing printing ink from drying and adhering within such edge regions.
[0013] The spray- or shower device preferably has its nozzle directed to the peripheral edge regions of the anilox roll.
[0014] With the aid of this spray- or shower device, it is thus possible constantly during ongoing printing to keep the residual printing ink within these peripheral regions of the circumferential surface of the anilox roll in a liquid state and by such means avoid this printing ink from “fouling” on the circumferential surface of the anilox roll, even in that case when the pertinent printing ink is dissolved in a volatile solvent which readily becomes fugitive at a relatively low temperature. To this end, the spray- or shower device provided with the nozzle is connectable to a suitable source of cleaning fluid for the printing ink through a hose or a conduit.
[0015] In one particularly preferred embodiment of the apparatus according to the present invention, the first and/or second axial end wall of the ink chamber has a through-going outlet aperture for removing air from the ink chamber.
[0016] In one practical embodiment, each respective axial end wall is configurated as a unit module of two mutually spaced apart configurated end wall elements, the through-going outlet aperture being provided in the wall element located most proximal the centre of the ink chamber. By such means, printing ink which, where applicable, leaks out laterally from the ink chamber is collected and taken care of via the interjacent outlet and is thereby prevented from causing splashing and soiling.
[0017] Such a unit module of end wall elements is preferably manufactured from a rubber or plastic material.
[0018] According to yet a further embodiment of the present invention, the axial end walls of the ink chamber extend towards and terminate a short distance from the circumferential surface of the anilox roll rotary partly inside the ink chamber, for the formation of a gap between the anilox roll and each respective end wall. The thus formed gap has a gap width of approx. 0.5-1.5 mm when the apparatus is employed for printing a web of packaging material which is driven at a web speed of approx. 400-600 m/min.
[0019] Further, the edge of each respective end wall facing towards the anilox roll may display a geometric configuration which is adapted to the opposing convex circumferential surface of the anilox roll, the thus adapted geometric configuration preferably being such that the gap between the anilox roll and each respective end wall displays a constant width throughout the entire length of the gap.
[0020] In one embodiment of the apparatus according to the present invention, both axial end walls of the ink chamber are disposed in contact with the circumferential surface of the anilox roll.
[0021] According to still a further embodiment, both axial end walls of the ink chamber are disposed a short distance from the circumferential surface of the anilox roll, sealing of the thus formed gap between the ink chamber and the circumferential surface of the anilox roll being in this case catered for by means of the previously described relationship between the viscosity of the printing ink and the relevant speed of rotation of the anilox roll.
[0022] In yet a further embodiment of the apparatus according to the present invention, in particular in that case when the axial end walls of the ink chamber extend up to and are in abutment with the circumferential surface of the anilox roll, at least one of the two end walls is provided with an air bleeder hole in line with or substantially flush with the axial stretch of air accumulated inside the ink chamber which has accompanied the anilox roll and is released inside the ink chamber.
[0023] In that the chamber side wall is disposed a distance from the surface of the anilox roll, no sealing rubber projections are required on the end walls in frictional contact with the circumferential surface of the anilox roll, at the same time as these end walls are not worn or exposed to abrasion by the rotating anilox roll either. In other words, wear of both the end walls and the anilox roll can be avoided almost completely. Moreover, nor is any frictional heat generated which would raise the temperature of the printing ink and thereby occasion unevenness and poor quality in the printing result, or even coagulation of printing ink at the ends of the ink chamber, with similar consequential deterioration in printing result.
[0024] Practical examples of cleaning fluid to be used in connection with the apparatus according to the present invention can be either gaseous or liquid fluid. Preferred such liquid cleaning fluid are chosen from the group consisting of water, solvent for the actual print ink in use, and the actual print ink in use. The most preferred liquid cleaning fluid for use in the apparatus according to the invention is the actual print ink in use, since it already has the appropriate composition, temperature and viscosity and will therefore have only a negligible impact on the qualities of the print ink in use. As a consequence, the actual print ink in use is the far superior choice of cleaning fluid in connection with an apparatus according to the invention in which the axial end walls of the ink chamber extend towards and terminate a short distance from the circumferential surface of the anilox roll rotary partly inside the ink chamber, for the formation of a gap between the anilox roll and each respective end wall, as mentioned above. Still another advantage of using the actual print ink as said cleaning fluid is that it does not require any extra complicated equipment for application. To this end it will suffice to supplement the apparatus with only one extra tube or hose in fluid communication with the print ink present in the ink chamber of the apparatus and the at least one spray- or shower device.
[0025] Additional advantages and preferred embodiments of the apparatus according to the present invention have further been given the characterising features as set forth in the appended subclaims.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
[0026] The present invention will now be described in greater detail hereinbelow, with reference to the accompanying Drawings. In the accompanying Drawings:
[0027] FIG. 1 is a perspective view of an apparatus according to the present invention for flexographic printing;
[0028] FIG. 2 is a schematic side elevation of an anilox roll in combination with an ink pan or chamber;
[0029] FIG. 3 is a schematic sectional view of the ink chamber according to FIG. 2 ;
[0030] FIG. 4 schematically illustrates one example of an end wall module for the axial ends of the ink chamber; and
[0031] FIG. 5 schematically illustrates the apparatus according to the present invention on printing of a web of packaging material with printing ink.
DETAILED DESCRIPTION OF THE INVENTION
[0032] Referring to the Drawings, FIG. 1 thus shows one example of an apparatus according to the present invention. The apparatus has an anilox roll 1 , a printing cylinder in the form of an impression plate cylinder 2 (hereinafter designated impression cylinder) and an ink pan or chamber 3 , the ink chamber being disposed axially along the one side of the anilox roll 1 . The ink chamber 3 is defined by a first chamber wall 4 , an upper and a lower doctor blade 5 , 6 , part of the circumferential surface 7 of the anilox roll 1 , as well as by an end wall 8 at each respective axial end of the ink chamber 3 . The first chamber wall 4 may be designed as a curved, C-shaped or U-shaped wall or as a planar wall, depending upon the length of the doctor blades 5 , 6 employed and depending upon how the doctor blades are fixed at the first chamber wall. Suitably, the wall is designed as an integrated unit in which the doctor blades are secured.
[0033] In order to maintain uniform quality and uniform properties of the printing ink, the ink is circulated continuously through the ink chamber 3 by the intermediary of an inlet 9 and fills up the ink chamber to a predetermined level 10 , before being led out of the chamber by the intermediary of an outlet 11 . The viscosity, temperature and homogeneity of the printing ink are regulated in an external unit 12 (only illustrated schematically), including int. al. agitators and temperature control. It is important that printing ink be transferred to the impression cylinder 2 from the anilox roll 1 in a uniform quantity and with uniform quality, so that no differences occur in printing result between different regions of the printed web. In such instance, the continuous circulation of printing ink plays a decisive part, in that the ink in then continuously monitored and regulated in respect of important properties, regardless of whether the printing process is in operation or whether the printing unit for some reason is inoperative. It is also important that the anilox roll 1 be constantly kept wet and filled with printing ink and be uniformly coated with ink also in stationary downtime, so that the ink does not dry and occasion problems in later printing processes. Suitably, the printing ink is led into the ink chamber 3 by the intermediary of an inlet 9 in or close to the bottom of the ink chamber and out of the chamber by the intermediary of an outlet 11 on a level just above the maximum level 10 to which printing ink is intended to be filled in the chamber.
[0034] The end wall 8 is disposed such that the edge which faces towards the surface of the anilox roll 1 adheres to the configuration of the anilox roll but at a distance from the circumferential surface 7 of the anilox roll. Between the circumferential surface 7 of the anilox roll 1 and the edge of the end wall 8 there is thus a gap which may have a width of from approx. 0.5 mm to approx. 2 mm, preferably from approx. 0.5 mm to approx. 1.5 mm, most preferably from approx. 0.6 to approx. 1.0 mm.
[0035] When the rolls and cylinders of the apparatus, including the anilox roll 1 , are rotated at a certain minimum speed, the printing ink in the ink chamber forms a liquid film along this gap so that liquid no longer leaks out from the ink chamber 3 through the gap.
[0036] A most preferred gap width for a water-based printing ink which is often used for printing a web of packaging material for liquid foods and which has a viscosity of approx. 20 s is from approx. 0.6 to approx. 0.9 mm.
[0037] As shown in the figure, the apparatus according to the present invention has one or more (in the figure only one is shown) spray- or shower devices 20 provided with a nozzle, which via a hose or conduit 21 may be in flow communication with a suitable source of cleaning fluid for the relevant printing ink.
[0038] As mentioned above, operative cleaning fluid can be either gaseous or liquid type fluid. Preferred examples of such liquid type fluid can be chosen from the group consisting of water, solvent, and the actual print ink in use. For water-based print inks, the cleaning fluid is preferably water, and for solvent-based print inks the cleaning fluid is preferably the solvent for the actual print ink. The most preferred cleaning fluid or liquid is however the actual print ink in use as explained above.
[0039] Said spray- or shower device 20 is, in the illustrated embodiment, positioned adjacent the anilox roll 1 and has its nozzle directed towards the axial end of the anilox roll 1 in order to spray the cleaning fluid towards the axial end regions of the circumferential surface 7 of the anilox roll 1 and thereby prevent any possible residual printing ink at these regions of the circumferential surface 7 from drying and “fouling” on the anilox roll 1 , as was mentioned previously. While being preferred to dispose the spray device 20 at a position outside the ink chamber 3 , as shown, it may when necessary also be placed at other suitable positions in association with the anilox roll 1 , on condition however that it is always placed after the transfer by the anilox roll 1 of printing ink to the impression cylinder 2 .
[0040] According to the present invention, the spray- or shower device 20 may be disposed to continuously apply cleaning fluid during ongoing printing to the ends of the anilox roll 1 , but it is often sufficient that the device applies the cleaning fluid intermittently at frequencies which in all essentials are determined by the consistency and viscosity of the printing ink employed. With printing inks which contain a large proportion of pigment and, as a result, have a high viscosity, it is advantageous to apply the cleaning fluid with rapid pulsations, while it is often sufficient to use slow pulsations in connection with printing inks of slight viscosity (a low proportion of pigment in relation to the quantity of solvent).
[0041] The illustrated apparatus in FIG. 1 preferably also has an aperture provided in the one axial end wall 8 of the ink chamber 3 (schematically illustrated in FIGS. 3 and 4 ) for ventilation of the ink chamber 3 during operation. The ventilation aperture through which air which accompanies the rotating anilox roll 1 into the ink chamber 3 is released and accumulated in an axial stretch throughout the entire length of the ink chamber on a more or less predictable level within the chamber as has been previously explained. With a suitable geometric configuration and positioning of the ventilation aperture, this may thus be effectively utilized for frequently removing the thus accumulated air from the air chamber and thereby prevent or considerably counteract consequential tendencies to frothing inside the ink chamber and tendencies to deterioration in print quality related to such frothing.
[0042] FIG. 2 is a schematic end elevation of an apparatus with an anilox roll 1 and associated ink chamber 3 according to another embodiment of the present invention. On the one hand, FIG. 2 shows how the side chamber wall 8 may be designed so that its wall is disposed at one and the same distance from the surfaces of the doctor blades 5 and 6 as from the circumferential surface 7 of the anilox roll 1 . In the same manner as the gap to the circumferential surface 7 of the anilox roll 1 is sealed by the printing ink when the anilox roll 1 is rotated at a speed of rotation above a certain minimum speed of rotation, as was explained earlier, the gap between the anilox roll 1 and the doctor blades 5 , 6 is sealed in the same manner and for the same reasons.
[0043] In FIG. 2 , the ink chamber 3 has two end walls 8 , an inner 8 a and an outer end wall 8 b (shown in FIG. 3 ). FIG. 2 shows a cross section of the ink chamber 3 along a line taken between the inner 8 a and the outer end wall 8 b. The visible end wall is thus the inner end wall 8 a.
[0044] Outside the inner end wall 8 a, there is located an outlet 18 for excess ink which has been scraped off from the circumferential surface 7 of the anilox roll 1 after absorption of printing ink in the ink chamber 3 which is led off from the ink chamber by the intermediary of the outlet 18 . In connection with start-up of the apparatus, and in connection with operation of the apparatus being arrested for repair or maintenance or the like, the speed of rotation of the anilox roll is at least temporarily slower than the speed of rotation which is required to counteract the tendency of the picked up printing ink to leak out laterally from the ink chamber 3 , for which reason leakage of printing ink cannot be avoided during such occasions. By such an arrangement with an extra end wall (i.e. two end walls 8 a and 8 b, instead of merely one end wall), the ends of the anilox roll 1 may nevertheless be kept clean and the entire printing unit can be protected from ink spatter.
[0045] FIG. 3 is a cross sectional view of the one axial end of an ink chamber according to the same embodiment as in FIG. 2 , seen from the position of the anilox roll in front of the ink chamber, but with the anilox roll removed.
[0046] In this example, the ink chamber is defined by an elongate first chamber wall 4 , an upper doctor blade 5 and a lower doctor blade 6 , and thus has two end walls, an inner end wall 8 a and an outer end wall 8 b, at each respective axial end of the ink chamber.
[0047] Outside the inner end wall 8 a, there is disposed an outlet for excess ink 18 , through which printing ink is led off from the ink chamber by the intermediary of the outlet 18 . In connection with start-up of the apparatus and in connection with operation of the apparatus being arrested for repair or maintenance and the like, the speed of rotation of the anilox roll is at least temporarily slower than the speed of rotation which is required to counteract the tendency of the picked up printing ink to leak out laterally from the ink chamber 3 , for which reason leakage of printing ink cannot be avoided during such occasions. By such an arrangement with an extra end wall (i.e. two end walls 8 a and 8 b, instead of merely one end wall), the ends of the anilox roll 1 may nevertheless be kept clean and the entire printing unit be protected from ink spatter. One example of positioning of the outlet 18 for the circulating printing ink is also shown.
[0048] As was mentioned earlier, the one axial end wall 8 a of the ink chamber (the inner end wall) has an aperture 24 provided in the end wall 8 a for ventilation of the ink chamber during operation. The ventilation aperture 24 through which air which accompanies the rotating anilox roll 1 into the ink chamber is released and accumulated in an axial stretch throughout the entire length of the ink chamber on a more or less predeterminable level inside the ink chamber, as was previously explained. With a suitable geometric configuration and positioning of the ventilation aperture 24 , this may thus effectively be utilized for frequently removing the thus accumulated air from the ink chamber and thereby prevent or considerably counteract consequential tendencies to frothing inside the ink chamber and tendencies to deterioration in print quality related to such frothing.
[0049] FIG. 4 shows one embodiment of an axial end wall which, in the illustrated embodiment, has two end walls 8 a and 8 b which are mutually spaced apart and are designed in one continuous piece. The illustrated integral end wall is designed as a readily replaceable module of a suitable plastic or rubber material. The end wall module has an inner 8 a and an outer end wall 8 b with front edges whose configuration is adapted to follow the cylindrical circumferential surface of the anilox roll. In the lower region of the module, which is intended to be turned to face towards the bottom of the ink chamber, there is disposed an outlet 14 which, during operation, is disposed to lead off printing ink which may have leaked out from the ink chamber through the gap between the inner end wall 8 a and the circumferential surface of the anilox roll. Alternatively, each respective front edge ( 80 a, 80 b ) of the two side walls may be provided with a thinner projection of plastic or rubber material which is disposed a distance from the surface of the anilox roll (not shown in the figure). Such an end wall module is thus suitably manufactured from a plastic or rubber material, and includes an inner end wall and an outer end wall, the inner end wall having a thickness of between 2 and 5 mm and with a spacing of from 20 to 50, preferably from 20 to 40 mm between the two end walls.
[0050] FIG. 5 schematically illustrates a printing process employing the apparatus according to the present invention. In FIG. 5 , the same reference numerals as earlier have been employed for the same or equivalent parts. The anilox roll 1 is rotated in the direction of rotation of the arrow, partly within the ink chamber 3 positioned axially along the roll 1 for taking up printing ink in the cells engraved on the circumferential surface of the roll 1 . Picked up excess ink is scraped off from the roll 1 by an upper doctor blade (obscured in the figure) abutting against the circumferential surface, on exit from the ink chamber 3 . The printing ink thus remaining in the engraved cells accompanies the rotating anilox roll 1 and is transferred to an impression cylinder 2 rotating in transfer contact with the anilox roll 1 . The printing ink thus transferred to the impression cylinder 2 accompanies the rotating impression cylinder 2 for transfer to a web 26 of packaging material which is led through the nip between the impression cylinder 2 and a counter pressure cylinder 17 rotating adjacent the impression cylinder 2 . After drying/setting of the transferred printing ink on the surface of the web, the printed web is rolled up for further processing, such as lamination and mechanical processing in a per se known manner.
[0051] In order to maintain good print quality and reduce process-related quality disruptions, but also to minimise unnecessary waste and spillage of expensive printing ink because of uncontrolled leakage of printing ink, the apparatus according to the invention has a spray- or shower device 20 disposed adjacent the anilox roll in order, during ongoing operation, to continuously or intermittently spray cleaning fluid for the printing ink on particularly sensitive regions of the circumferential surface of the anilox roll 1 . Such a region is the peripheral edge regions of the anilox roll 1 where printing ink in certain cases (in particular printing ink with a high proportion of pigment in relation to solvent) shows a tendency to dry on the anilox roll, as has been previously explained. Such undesirable drying of the printing ink is effectively counteracted with the aid of the applied cleaning fluid which ensures that residual printing ink within these sensitive regions on the surface of the anilox roll is constantly kept in soluble form. | The disclosure relates to an apparatus for flexographic printing of a web of packaging material. The apparatus has an anilox roll which is rotary in an ink pan or chamber for picking up and transferring printing ink to an impression cylinder which is rotary adjacent the anilox roll and forms, together with a counter pressure cylinder rotary adjacent the impression cylinder, a nip through which the web is led for receiving printing ink from the impression cylinder. In order to prevent printing ink from drying and adhering to the anilox roll, the apparatus displays a spray- or shower device through which a cleaning fluid for the printing ink is applied on the circumferential surface of the anilox roll. | 1 |
BACKGROUND OF THE INVENTION
[0001] The invention relates to a hydraulic cylinder unit, specifically a hydraulic cylinder unit with a cylinder tube having an inner surface with a piston that is guided thereon and that has an outer surface, with a piston rod joined thereto whose rod surface is guided on a cylinder head that closes the rod-side cylinder space, with at least one rod seal arranged therein that seals the piston rod-side cylinder space from the area of the cylinder unit between the rod surface and the cylinder head by means of a rotationally symmetrical inner seal surface, and with at least one piston seal arranged in the piston that seals the piston-rod side cylinder space and the cylinder space formed by the cylinder floor and the piston between the cylinder space inner surface and the outer surface of the piston by means of a rotationally symmetrical outer seal surface.
[0002] Especially low-friction cylinder units are of interest for various purposes. Among these are cylinders for suspension and steering functions, or working cylinders subject to high demands in terms of sensitivity and positionability. The effect of increased friction is a poor ratio of effective force, that is working force of the cylinder, to theoretical pressure force. Among other things, this leads to the fact that the cylinder must be designed larger than theoretically necessary in order to provide adequate effective force.
[0003] In suspension cylinders, the frictional force acts like additional damping. However, the greater the basic damping of the cylinder itself, the lower the portion that can be effectively influenced in the control. However, it is precisely the option for influencing damping that is the basis for a modem, active suspension and damping system.
[0004] In addition to relatively high friction, the ratio of static friction to sliding friction is also of interest because major differences between the two values can lead to undesired oscillations or vibrations (so-called stick/slip effect).
[0005] Finally, unsatisfactory friction values and relatively wide variance of known hydraulic cylinder units in series are also disadvantageous.
[0006] The object of the invention is therefore to design a hydraulic cylinder unit such that it is particularly low in friction.
SUMMARY OF THE INVENTION
[0007] This object is inventively attained in a hydraulic cylinder unit in accordance with the invention in that the rod seal and/or piston seal (hereinafter referred to as seal) has, at least by region, on its inner and outer seal surfaces (hereinafter seal surfaces) a shape that deviates from the surface of a vertical circular cylinder while forming a converging gap with regard to the rod surface and the inner surface of the cylinder tube.
[0008] The inventively provided rotationally symmetrical rod seal thus is in contact along a circumferential closed line, hereinafter referred to as the inner equator, on its inner seal surface with the outer surface of the piston, and/or the likewise rotationally symmetrically embodied piston seal is thus in contact along a likewise circumferential closed line, hereinafter referred to as the outer equator, on its outer seal surface with the inner surface of the cylinder tube. The line can also form a certain width while creating a circumferential contacting surface. Thus, as the distance from the equator to the gaps converging in the direction of the equator decreases, the free cross-section of the gaps for the passage of the displaced hydraulic fluid preferably grows increasingly smaller. In this, the shape of the region that is adjacent to each gap and that deviates from the shape of the surface of a vertical circular cylinder can be embodied curved not only as a result of its rotational symmetry in the circumferential direction but also in the axial direction. However, a gap embodied in a wedge-shape without additional curvature is also possible.
[0009] The inventive principle thus utilizes the hydrodynamic effect of the hydraulic liquid in the converging gap in order to minimize the frictional forces between preferably the piston seal and the cylinder tube on the one hand and the rod seal and the piston rod on the other hand. Although the qualities of the running surface (roughness, material, surface treatment) are not the subject of the invention, it must be embodied such that, in combination with the running surface (inner surface of the cylinder tube or outer surface of the piston rod), with the seal it ensures optimum friction and wear behavior.
[0010] It has been found that the frictional force or damping properties of the hydraulic cylinder unit in accordance with the invention can be substantially reduced by using the piston seal and/or rod seal. Numerous possibilities and advantages result from this. Thus, the reduction in the size of the cylinder due to improved force utilization can lead to more numerous employment possibilities and to savings in costs. Furthermore, the improvement in the properties of suspension cylinders, due to reduced basic damping, leads to the fact that a greater portion is available for actively influencing system damping. In working cylinders, controllability and sensitivity can be markedly enhanced. In addition, new areas of application become available for the inventive cylinder units for cylinders that were previously not suitable due to inadequate effective force, frictional forces and thus interfering forces that were too high, or damping that was too high. Double-acting cylinders can also act as the hydraulic cylinder unit.
[0011] In one advantageous embodiment of the invention, the piston seal has two largely wedge-shaped gaps that deviate from the surface of a vertical circular cylinder, of which the one gap is open to the cylinder space and the other is open to the rod-side cylinder space.
[0012] In accordance with the invention, the gap for the rod seal is embodied asymmetrical with respect to its center plane and open to the piston rod-side cylinder space so that at least in the outward-moving direction of the piston rod the hydrodynamic friction-reducing floating effect results.
[0013] If in addition an additional seal is arranged between the rod seal and the area of the cylinder unit and between it and the rod seal a recess acting as a reservoir for the hydraulic fluid that is carried out is arranged in the cylinder head, the extra hydraulic fluid carried out as a lubricating film can be collected there and the hydrodynamic friction-reducing floating effect can also be produced in the inward-moving direction of the piston rod.
[0014] One exemplary embodiment of the invention is explained in greater detail in the following, with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 depicts a schematic section through a cylinder unit, in partial break-away;
[0016] FIG. 2 is detail II in accordance with FIG. 1 , using a larger scale;
[0017] FIG. 3 is detail III in accordance with FIG. 1 , using a larger scale;
[0018] FIG. 4 is FIG. 2 using a larger scale.
DETAILED DESCRIPTION OF THE INVENTION
[0019] The cylinder unit illustrated in FIG. 1 and labeled 5 overall has a cylinder tube 6 on whose inner surface 7 a piston 8 having an outer surface 9 is guided. On the piston, a piston rod, labeled 10 overall, is joined to a rod surface 11 that extends out of the cylinder unit 5 via a cylinder head labeled 12 overall that is driven out when hydraulic fluid that is under pressure acts upon the cylinder space 14 that is formed between the piston 8 and the cylinder floor 13 . If the cylinder unit 5 is embodied with double action, pressure can also act on the annular piston rod-side cylinder space 15 that is formed by the piston rod 10 , the cylinder head 12 , and the piston 8 , driving the piston rod 10 in.
[0020] A piston seal labeled 16 overall is provided on the piston 8 between the cylinder space 14 and the piston rod-side cylinder space 15 . Correspondingly, a rod seal labeled 17 overall is provided on the cylinder head 12 between the external area of the cylinder unit 5 and the piston rod-side cylinder space 15 .
[0021] FIG. 2 illustrates the piston seal 16 in greater detail. This piston 8 has three circumferential grooves 181 , 182 spaced at intervals from one another on the outer surface 9 of the piston. A guide ring 19 is inserted in each of the two external, outwardly open grooves 181 . Provided in the center groove 182 is the seal that is labeled 16 overall and that is arranged from two parts, specifically the piston seal 161 embodied as a sliding and sealing element and the pre-stress element 162 arranged thereunder, e.g. in the form of an elastomer ring that when installed assures that the sliding and sealing element 161 exerts a certain basic pressure against the cylinder's inner surface 7 .
[0022] The piston seal 161 has an outer seal surface 163 that is symmetrically embodied with respect to the center plane 164 ( FIG. 4 ) of the piston seal 161 , while forming with respect to the inner cylinder surface 7 of the cylinder tube 6 two converging gaps 165 ( FIG. 4 ), deviating from the surface of a vertical circular cylinder. The highest point and at the same time the longest circumferential, closed line of contact, the outer equator 166 , between the seal outer surface 163 and the inner surface 7 of the cylinder tube 6 is located in the region of the center plane. 164 . Thus, as the distance from the outer equator 166 to the two gaps 165 that converge in the direction of this outer equator 166 decreases, the free cross-section of the gaps for the passage of the displaced hydraulic fluid grows increasingly smaller. In the exemplary embodiment depicted, the region that is adjacent to the gap 165 and that deviates from the shape of the surface of a vertical circular cylinder is embodied in a wedge-shape with curvature in the axial direction. The wedge-shaped gap 165 between the outer seal surface 163 and the inner cylinder surface 7 of the cylinder tube 6 results in a hydrodynamic effect such that the piston seal 161 lifts from the hydraulic fluid carried into the wedge-shaped gap 165 over the highest point, the outer equator 166 , that is, the seal outer surface 163 , which is overall ball-shaped, lifts from the inner cylinder surface 7 of the cylinder tube 6 . This substantially reduces the mechanical frictional forces of the seal. FIG. 4 depicts this part of the piston 8 from FIG. 2 in greater detail.
[0023] The rod seal, labeled 17 overall, that is inserted in the cylinder head 12 , is illustrated in greater detail in FIG. 3 . In interiorly situated circumferential grooves that are spaced at intervals from one another, a wiping element 20 is provided in the outermost groove and a rod guide 21 is provided in the groove next closest to the piston rod-side cylinder space 15 . The rod seal 17 is likewise provided in two parts, with a seal 171 embodied as a sliding and sealing element and with a pre-stress element 172 located thereunder that corresponds to the element 162 already discussed in accordance with FIG. 2 .
[0024] Deviating from the piston seal 161 , the inner seal surface 173 of the rod seal 171 is embodied asymmetrical with respect to the center plane and has either only one wedge-shaped gap or two gaps with different gap angles and/or length. In the former case the gap is preferably open to the piston rod-side cylinder space 15 .
[0025] An additional seal labeled 22 overall is arranged between the rod seal 171 and the outer area of the cylinder unit. Arranged between the latter and the rod seal 171 is a recess 23 in the cylinder head that acts as a reservoir for the hydraulic fluid, in which recess is collected hydraulic fluid that is carried out as a lubricating film under the rod seal 171 during the outward stroke of the piston rod. During the subsequent inward stroke of the piston, this quantity of oil can be carried with its piston rod using the return ability of the rod seal back into the rod-side cylinder space 15 .
[0026] The asymmetrical shape of the seal inner wall 173 is provided in order to promote the return using the rod seal 171 , this shape ensuring the return of the quantity of hydraulic fluid previously carried out.
[0027] The piston seal and the rod seal may be comprised of a polyurethane or a dimensionally stable material, such as polytetrafluoroethylene, polyamide, polyethylene or polyoxymethylene. These polymers may be admixed with a filler, such as subdivided (e.g., particulate or powdered) bronze or graphite, before being fabricated into the seals. | A hydraulic cylinder unit is provided with a rod seal and/or piston seal which has a surface that deviates from the vertical circular cylindrical surface of the piston head throughhole through which the piston rod passes or the vertical circular cylindrical surface of the cylinder interior while forming respective converging gaps with regard to the rod surface and the interior surface of the cylinder, respectively. | 5 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] The present application is a continuation-in-part of, and claims benefit from, U.S. patent application Ser. No. 10/228,044, filed Aug. 27, 2002, and incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to logic adapted to execution on an electronic digital device for a self-modifying copier. More particularly, it relates to a self-modifying copier used to nondisruptively load code and data into a runtime area of an active digital electronic device.
BACKGROUND OF THE INVENTION
[0003] The field of computing technology advances at almost a lightening pace. Equipment rarely has more than a five year life. In most instances, the life is only two to three years. In some instances, it is possible to replace various pieces of the equipment. In other instances, all that is required is a modification to existing code.
[0004] “Smart” devices operating under control of a digital processor today include not just traditional computer systems, but also include, for example, telephones; personal digital assistants; routers, switches, and other networking devices; media presentation, recording, and distribution systems; storage systems, databases, and data warehouses; kiosks; security monitoring equipment, devices supporting web services; space shuttles, and tractors. It is easy to imagine situations in which any of these kinds of equipment might benefit from being able to update information, including running code, on the fly nondisruptively; i.e., without interruption to active operation. We will refer to such a device operating under the control of a processor as a “system.”
[0005] It is desirable to provide an apparatus and method that enables running code on such systems to be upgraded to add functionality or fix bugs without any system down time. The device would run or operate in real time and continue to process requests. A process that updates a system without requiring it to shut down is often referred to as a nondisruptive code load (NDCL).
[0006] A variety of approaches to NDCL have been implemented. Christeson et al. (U.S. Pat. No. 5,579,522) teach a computer system having two update modes, normal and recovery, selectable from outside the computer's enclosure using a hardware jumper. In a normal update mode, an operating system is transferred to and caused to execute in volatile random access memory. The system's BIOS and flash memory may be used in this initialization. An update program is then executed within the operating system, providing a user with update selections to save, verify or update nonvolatile memory areas, including the system BIOS or flash memory. A recovery update mode causes a special recovery BIOS to be executed in the event that the normal BIOS has been corrupted, thereby overwriting the normal BIOS of a computer system. The normal mode of Christeson is a variety of NDCL that Gabel (U.S. Pat. No. 5,930,504) characterizes as teaching that procedures for updating a logical area within a system may reside within that same logical area; in order to avoid change or corruption during an update process if they were to remain in the affected logical area, however, those procedures are protected by copying them to a safe system memory area from which they execute the update. The recovery mode of Christeson is clearly disruptive, requiring a reboot of the system after a manual change in a hardware jumper setting. In the context of a telecommunications switching system, Nilsson et al. (U.S. Pat. No. 5,410,703) teach maintaining an old software version effectively in parallel with a new version, gradually switching traffic over to the new version. Ishii et al. (U.S. Pat. No. 5,835,761) discuss performance improvements during NDCL that can be achieved by first copying the new code version into a shadow area of fast memory.
[0007] The parameters and variables required to keep the system operational must be preserved through a nondisruptive code load. The patent of O'Brien et al. (U.S. Pat. No. 6,141,771) teaches copying a trusted machine state to a second portion of memory, reinitializing some portion of memory that does not include the trusted machine state, and then restoring the trusted machine state to either the original memory area or to a new memory area. O'Brien et al. also allude to an alternative method of preserving a trusted machine state, one that avoids initializing the portion of memory that contains that state; no specific structure or process for reinitializing the system is described, however, for this alternative method, which is not the focus of their invention.
SUMMARY OF THE INVENTION
[0008] The central concept of the present invention is an executable self-modifying copier, resident in runtime memory. Runtime memory is an area of a digital device from which a processor reads instructions. The word “memory” is being used generically here to include a medium to which instructions can be written and then later written over, such as random access memory or disk storage. Runtime memory might be volatile random access memory, or it could be nonvolatile firmware so that its contents will not be erased when the system is shut down and restarted. The invention applies equally to either alternative. Henceforth without loss of generality this document will describe a single area of runtime memory, while in fact a given system may have a plurality of areas of runtime memory that exploit the benefits of the invention.
[0009] The runtime memory has some structure or format that the executing code requires to function properly. For example, the executing code might access within memory certain parameters or variables about the state of the system. For example, within a digital camera, a typical state variable is an aperture setting. The logic requires these variables to be found in portions of runtime memory whose locations are usually known and constant. Another example of a required format within runtime memory is the start of the code that executes when the system is initialized (i.e., rebooted). The structure of runtime memory, therefore, typically consists of a plurality of segments. Both the old version and the new version of what occupies that memory, namely the old runtime version before the update and the new runtime version afterwards, will be some combination taken from code modules, data modules, and modules that combine both code and data. The data might consist of system parameters, but in general it can be virtually anything that can be represented digitally, such as statistical data, transactional data, images, or music.
[0010] In one embodiment of the invention, the new version is first loaded into a shadow area of memory. It will often be the case that the memory in the shadow area will have faster and more robust performance than some external medium, such as slow disk, containing the new code version. Thus, the preliminary shadowing operation will both shorten the process of upgrading and reduce the risk of errors. We will refer to the area from which the new version is transferred as the source area, which might be shadow memory or any other medium.
[0011] If the arrangement of the segments in the runtime area is unchanging through every upgrade, then the process of copying the new version is fairly straightforward, consisting essentially of copier instructions in the runtime memory superposing segments of the new version into corresponding segments containing the old version. In other words, the copier could be static, and would typically itself occupy a code segment. The copying process in this case is not entirely trivial, however, because consideration must be given to currently executing processes, system interrupts occurring while the transfer is occurring, and so forth.
[0012] If, on the other hand, the structure of the runtime area must be changed with the new version, then the upgrade process can be significantly more complicated if it is done in place, that is, by directly overwriting the runtime area. Such a structural modification might include, for example, one or more of the following: a change in the starting address of a segment; a change in the ending address of a segment; the addition of a new code or data segment; and the deletion of an existing code or data segment. The structural modification could obviously leave some segments intact, although the content (i.e., code or data) of such segments might change with the upgrade.
[0013] In general, a static copier within the runtime area would not contain logic to anticipate how the segments might be rearranged in the next upgrade iteration, nor, indeed, all succeeding ones. Consequently, there is a puzzle regarding how the processor can execute code in the runtime area that effects the structural change, when the nature of the desired change is embodied only in the new version, residing in the typically nonexecutable source area.
[0014] The solution employed by the present invention is for a runtime area copier module to consist of two parts: a bootstrapper and a dynamic copier part. The content of the bootstrapper will typically, but not necessarily, be static through upgrades, while the dynamic copier part has the opportunity to change from one runtime version to the next. Two essential functions of the bootstrapper are to copy the new version of the dynamic copier part into runtime memory and to cause the new dynamic copier part to begin execution. In one embodiment of the invention, the bootstrapper will have fixed start and ending addresses in the runtime area, while the dynamic part (which will be replaced and typically overwritten during the NDCL) will have a fixed start address. In some embodiments, the entire copier will reside within a runtime memory segment having fixed starting and ending addresses, with enough space available for the dynamic part of the copier to expand within the segment over a number of anticipated upgrade cycles. Instructions within the new dynamic part of the copier, once loaded into runtime memory and executed, will produce the intended runtime area structural change and load in the remainder of the new version of code and data.
[0015] The content of the bootstrapper can remain static in either of two ways. One alternative is for instructions in the static copier part of runtime memory to be overwritten with identical instructions from the source region as the copier executes. This approach has an advantage of simplicity, in that the entire runtime version is overwritten. The second alternative is for the copier to only overwrite its dynamic part, which will be faster, although usually only slightly faster, than a complete overwrite. Performance of the copier can be improved by the utilization of a processor instruction cache, when available. The processor instruction cache can also facilitate changes to the bootstrapper part of the copier.
[0016] In some embodiments of the invention, state information about the system is stored in a trusted system state segment that is left untouched during upgrades of the executable code. The trusted system segment will have fixed start and end addresses. In some embodiments, the copying process involves decompression, decryption, or other similar operations being applied to some or all of the information being copied.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is a conceptual block diagram illustrating several elements of an embodiment of the present invention.
[0018] FIG. 2 is a diagram of an exemplary structuring of memory in the runtime area and a shadow (source) area.
[0019] FIG. 3 is a flowchart illustrating an embodiment of the runtime area upgrade process.
[0020] FIG. 4 is a conceptual block diagram illustrating a processor having an instruction cache and a data cache.
[0021] FIG. 5 is a flowchart illustrating an embodiment of the runtime area upgrade process utilizing a processor instruction cache.
DETAILED DESCRIPTION OF THE INVENTION
[0022] The present invention provides an apparatus and method for installing executable code or data in a manner that is non-disruptive to the system, so that the system is able to continue operating without the need to sacrifice any system down time. FIG. 1 is a conceptual block diagram showing one embodiment of the invention. The system 105 is an electronic digital device that contains a processor 108 and a runtime area 110 . The processor 108 can be a microcontroller on an integrated circuit board, a central processor of a supercomputer, or anything in between. The system 105 could be, for example, a computer, a digital camera, a portable media player, or a mobile phone. The runtime area 110 is an area of memory from within which the processor 108 can execute instructions represented in digital form (i.e., software code). The runtime area 110 is represented on a medium that is both readable and writable. The arrow labeled 190 indicates that the processor 108 has access to data and code for execution, both located in this area. This medium will be referred to as memory, although it need not be conventional volatile memory. The runtime area 110 contains at least two modules, one of which is a copier 120 . The other module could be an old code module 160 , a old data module 170 , or some combination of code and data. More typically, in addition to the copier 120 , the runtime area 110 will contain at least an old code module 160 , an old data module 170 , and a fixed content module 115 , whose content remains the same through all upgrades. The runtime area 110 might, in fact, contain a plurality of some or all of these module types. A particular example of a fixed content module 115 is a trusted system state 116 , which contains system state information and other parameters that are located in fixed, well-known locations, to ensure reliability of processing and continuity through upgrades of the system 105 .
[0023] The upgrade process includes copying a new version 101 of runtime area content (hereinafter, “new version”) from a source area 111 into the runtime area 110 , replacing portions of the old version 100 , but not any fixed content modules 115 . It is well-known in the art that other steps and other components will typically be involved for a code upgrade to be done nondisruptively. The scope of the invention encompasses any such ancillary steps and components when used in combination with core concepts of the present invention.
[0024] The source area 111 could be located internally within the system 105 , or it might be external. The large outer rectangle in the FIG. 1 suggests an internal source area 111 , while a dashed line 106 suggests the alternative of an external source area 111 .
[0025] The new version 101 might have a collection of modules that are in correspondence with the original modules. For example, every old code module could have a corresponding new code module, and conversely. This need not be the case, however. FIG. 1 , for example, shows that the source area 111 has a new second code module 181 . The figure is also suggestive of some other kinds of restructuring of the content of the runtime area 110 that an upgrade might accomplish. For example, the new data module 171 has a different size from the old data module 170 (namely, larger), while the new code module 161 is smaller than its counterpart old code module 160 . The modules in the source area 111 are also arranged differently from those in the runtime area 110 , suggesting that the same might be true after the new modules have been installed into the runtime area 110 . In general, the upgrade process can result in a restructuring of the content within runtime area 110 that can qualitatively be simple or complex. Additions and deletions of modules, rearrangements of locations, and changes in module sizes are among the possible restructuring possibilities.
[0026] The invention accomplishes the upgrade, including any concomitant runtime area 110 restructuring, using a self-modifying copier 120 . At the start of the upgrade process, there are two versions of the copier 120 , an old copier module 130 within the runtime area 110 , and a new copier module 131 , within the source area 111 .
[0027] In the embodiment of the invention illustrated in FIG. 1 , the old copier module 130 includes two parts, an old bootstrapper 140 and an old copier dynamic part 150 . The new copier module 131 includes a new copier dynamic part 151 . (Each “part” is actually code, so, for example, “new copier dynamic code” is an alternative term for that part.) The old bootstrapper 140 causes the new copier dynamic part 151 to be copied into the runtime area 110 , and thereafter causes the processor 108 to execute the new copier dynamic part 151 . The adaptation of logic within the old bootstrapper 140 to copying the new copier module 131 , at least the new copier dynamic part 151 but possibly also, as discussed below, the new bootstrapper 141 , is indicated by the arrow labeled 195 in FIG. 1 .
[0028] The new copier dynamic part 151 contains logic for loading the new runtime content version 101 into the runtime area 110 , including any restructuring required within the runtime area 110 to accommodate the various modules of the new version 101 . For convenience, we will exclude the new version of the copier 120 from the term new runtime content version 101 . Logic in the modules in the runtime area 110 can consequently be ignorant about how the runtime area 110 might be reconfigured during an upgrade. In effect, the old copier module 130 knows how to kick off the upgrade process and the new copier module 131 , specifically the new copier dynamic part 151 , takes over from there. In FIG. 1 , logic in the new copier dynamic part 151 to copy and arrange the various modules of the new runtime content version 101 is suggested by arrows labeled 196 . The copying process might also accomplish one or more incidental tasks on portions of the new runtime content version 101 , including decompression, decoding, decryption, or even code assembly or compilation.
[0029] The new copier module 131 might also include a new bootstrapper 141 . The fact that a new bootstrapper 141 is optional is suggested in FIG. 1 by its enclosure within a dashed line. If it exists at all, the new bootstrapper 141 is typically identical to the old bootstrapper 140 . While overwriting the old bootstrapper 140 with an identical version of itself might seem redundant, in some situations there might be good motivation to do so stemming from hardware or software considerations. It is also conceivable that the designers of the system 105 might want to leave open the possibility of improving or fixing bugs within the old bootstrapper 140 , in which case the new bootstrapper 141 could have some differences from the old bootstrapper 140 .
[0030] Referring now to FIG. 2 , we see a simple embodiment of the concepts that were illustrated in FIG. 1 in which the runtime area 110 and the source area 111 each consist of a respective block of memory. Here, the source area 111 is actually a shadow area into which the new runtime content version 101 has been staged (i.e., preloaded) to reduce the time required for the upgrade process. The runtime area 110 includes a runtime area copier section 210 , a runtime area code section 220 , a runtime area data section 230 . The source area 111 includes corresponding sections, specifically a source area copier section 211 , a source area code section 221 , a source area data section 231 . As their names suggest, these sections contain a copier, code, and data, respectively. The runtime area 110 contains an additional section, a fixed content section 200 . The fixed content section 200 , which can contain any kind of digital content such as code or data, remains untouched during the upgrade process. In the embodiment of FIG. 2 , the fixed content section 200 contains a trusted system state 116 .
[0031] In the embodiment illustrated by FIG. 2 , the starting and ending memory addresses within the runtime area 110 are fixed and the sections are contiguous. Thus, for example, the runtime area code section 220 extends up to the start of the runtime area data section 230 . The old code module 160 , however, does not fully occupy the runtime area code section 220 . A code expansion area 260 remains vacant, providing limited room for the code module in the runtime area 110 to grow from one upgrade iteration to the next. Similarly, the fixed content section 200 includes a fixed content section expansion area 240 , the runtime area copier section 210 includes a copier expansion area 250 , and the runtime area data section 230 includes a data expansion area 270 . A runtime area 110 structure including segments with fixed starting and ending addresses, while not essential to the invention, is often convenient so that system 105 logic can anticipate where to find particular information regardless of upgrades.
[0032] In the exemplary embodiment, the old copier module 130 is divided into an old bootstrapper 140 and an old copier dynamic part 150 . The old bootstrapper 140 has static start and end addresses, contained in memory extending up to the start of the old copier dynamic part 150 . Because, in this embodiment of the invention, the bootstrapper remains unchanged through the upgrade, the copier expansion area 250 is exclusively dedicated to potential expansion of the copier dynamic part.
[0033] A few things are worthy of notice in the source area 111 . The sizes of the new copier dynamic part 151 , the new code module 161 , and the new data module 171 differ from their respective counterparts in the old runtime content version 100 . On the other hand, the new bootstrapper 141 is identical in size to the old bootstrapper 140 because it is identical in content. Each content module in the source area 111 would be copied into the runtime area 110 , beginning at the start address of the corresponding memory section there. In this configuration, the old copier module 130 would entirely overwrite itself with the new copier module 131 during the upgrade process.
[0034] Even in the relatively simple embodiment shown in FIG. 2 , the new copier dynamic part 151 might have several tasks effecting the restructuring of the runtime area 110 . As a minimum, the logic of the new copier dynamic part 151 must be aware of the format of the new version 101 , such as the starting and ending addresses of the new data module 171 within the source area 111 , so that the segments of the runtime area 110 can be appropriately populated. Another possibility is that logic executing on the processor 108 might rely upon knowledge of the ending addresses of the portions of the memory sections actually in use (or equivalently the starting addresses of the expansion areas). This information might be stored by the new copier dynamic part 151 during NDCL at previously specified locations within the trusted system state 116 .
[0035] FIG. 3 is a flowchart illustrating an embodiment of the invention in which at the start 300 of the process, the new runtime content version 101 is staged 310 into a source area 111 that is a shadow area containing fast memory. In other embodiments, the source area 111 might be external to the system 105 , or might consist of a read-only medium, such as a compact disk. The processor 108 (or, more precisely, code executing on the processor) initiates 320 execution of the old copier module 130 , specifically the old bootstrapper 140 . Whether the next step, in which the old bootstrapper 140 overwrites 330 itself with a new bootstrapper 141 from the source area 111 is included depends upon embodiment, as previously discussed. In the next step 340 , the copier 120 copies the new copier dynamic part 151 into the runtime area 110 as a replacement for the old copier dynamic part 150 . Some responsibility for this task must fall on the old bootstrapper 140 , although the new copier dynamic part 151 might also participate in copying itself after it has begun executing 350 .
[0036] In step 360 , which is an optional step that has been included in this particular embodiment, the copier 120 decompresses some or all of the modules of the new runtime content version 101 . Note that this step might be done at alternative locations in the flowchart. For example, the new copier module 131 might be decompressed by the old bootstrapper 140 between steps 320 and 330 . Decompression might be done all at once, or it might be done in smaller bits; for example, code might be decompressed on the fly, one instruction at a time. In fact, steps that are presented for convenience of illustration as sequential in the flowchart might actually occur together in a single step; for example, steps 360 and 370 might be carried out in combination or in parallel. In certain embodiments, some modules within the new runtime content version 101 will need decompression but not others. Analogously to decompression 360 , steps (not shown) might be added to the process for decoding or decrypting various modules of the new runtime content version 101 , with similar configuration flexibility. Of course, such secondary processes as decompression, decoding, and decryption might not be required at all in some embodiments. In step 370 , the new copier dynamic part 151 , now resident itself within the runtime area 110 , copies the remainder of the new runtime content version 101 modules from the source area 111 to the runtime area 110 , reconfiguring the runtime area 110 appropriately.
[0037] The discussion so far has not addressed details regarding treatment of cache 400 that might be available to the processor 108 . A processor 108 might have instruction cache 410 , data cache 420 , or, as illustrated by FIG. 4 , both. Physically, the cache 400 might be housed within the processor 108 itself, but could be separate. Within the conceptual framework illustrated by FIG. 1 , the cache 400 will be within the system 105 but outside both the runtime area 110 and the source area 111 . Either cache 400 type might be implemented in one or more separate units, so when we refer to “the data cache,” we mean as many individual units of data cache as are involved within the particular context.
[0038] Despite some perils for the unwary described below, the availability of instruction cache 410 offers advantages in terms of processor 108 performance and a safe area where a small piece of code such as the old bootstrapper 140 can execute. This approach allows the old bootstrapper 140 to conveniently overwrite and even modify itself during the upgrade.
[0039] FIG. 5 is a flowchart illustrating the interplay between the instruction cache 410 , the data cache 420 , and the runtime area 110 during copying of the new bootstrapper 141 and the new copier dynamic part 151 . FIG. 5 in effect adds cache-specific implementation details to FIG. 3 , which also pertains to configurations in which cache is either not present or has been disabled.
[0040] The availability, types, and implementation of cache 400 tend to be specific to a family of processors 108 , or even to a single processor 108 model. FIG. 5 assumes that the processor 108 has both instruction cache 410 and data cache 420 enabled, but variants of FIG. 5 for which either type is not present are straightforward and within the scope of the invention.
[0041] The process starts 500 with the new version being staged 510 into a source area 111 , which in this embodiment is a shadow area within fast memory to improve performance. In step 515 , the old bootstrapper 140 is placed within instruction cache 410 . This can be done manually by loading and locking the instruction cache 410 , or automatically if the system 105 provides a command to cause the processor 108 to do so according to algorithms of the processor 108 . The old bootstrapper 140 within the instruction cache 410 will typically be an instruction loop adapted to copying the new bootstrapper 141 and the new copier dynamic part 151 from the source area 111 into the runtime area 110 . Execution of the old bootstrapper 140 is initiated in step 520 . In addition to better processor 108 performance, having the old bootstrapper 140 within the instruction cache 410 in effect allows the bootstrapper to be conveniently modified as it overwrites 530 the runtime area 110 copy of itself. Next, the old copier dynamic part 150 is replaced 540 by the new copier dynamic part 151 by being partly or wholly overwritten.
[0042] Because the copier 120 is self-modifying code, the distinction between “data” and “instructions” is obscured. Because processors 108 are often configured under the assumption that they will not be overwriting their own instruction set, many processors 108 will behave as if the new version 101 being copied from the source area 111 is data, not instructions. Unless the data cache 420 has been disabled (which may be preferable), the processor 108 might copy at least some portion of the new version 101 into its data cache 420 for faster availability of the “data”. Code in the data cache 420 is not in the runtime area 110 , where it is needed for completion of the upgrade. Flushing 545 the data cache 420 fixes this problem, returning the instructions contained therein to the memory of the runtime area 110 .
[0043] Because the instruction cache 410 still contains the old bootstrapper 140 , a command is issued to invalidate 547 the contents of the instruction cache 410 , which forces the processor 108 to fetch its instructions from runtime area 110 memory, hence refreshing itself and initiating execution of the new copier dynamic part 151 . The system 105 typically provides specific assembly level instructions for operations such as loading and invalidating the instruction cache 410 and for disabling and flushing the data cache 420 . As in FIG. 3 the step 560 of decompressing some or all of the information being transferred from the source area 111 to the runtime area 110 is optional. Other similar operations, such as decryption, decoding, compression, encryption, or encoding can also be done optionally. Finally, the new copier dynamic part 151 completes the copying and rearrangement of the runtime area 110 , while keeping the fixed content section 200 intact.
[0044] The present invention is not limited to all the above details, as modifications and variations may be made without departing from the intent or scope of the invention. For example, the functionality of the tracking camera could be split between two cameras, one dedicated to viewing presets and the other to tracking movement of a presenter, without departing from the central concept of integrating preset sensing zones with tracking away from those zones. As another example, other forms of devices might be used to configure a controller. Consequently, the invention should be limited only by the following claims and equivalent constructions. | A method and apparatus for achieving a non-disruptive code load in a digital electronic device utilizes a copier that modifies itself as it executes. A fixed data section might be left unmodified to preserve a trusted system state. The copier has two parts, a bootstrapper and a dynamic part. As a minimum, the bootstrapper copies the new dynamic part into the runtime area and initiates execution of the new dynamic part. Through the dynamic part, the desired new runtime area configuration for data and code modules is achieved. The bootstrapper is typically static through upgrades, but instruction cache associated with the processor can make self-modification of even the bootstrapper more convenient. | 6 |
[0001] The present application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/338,990, filed Dic. 10, 2001, which application is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to the construction of small water-repellent microphones, and more particularly an improved method for the construction of a small water-resistant microphone, which method reduces the difficulty associated with handling small parts, and provides improved acoustic performance. Such small water-repellent microphone is well suited for use as the microphone of an Implantable Cochlear Stimulation (ICS) system, wherein the microphone is generally worn on the user's head, and is subject to moisture generally encountered in such use (e.g., perspiration, rain, fog, etc.)
[0003] Cochlear stimulation systems are known in the art. Such systems are used to help the profoundly deaf (those whose middle and/or outer ear is dysfunctional, but whose auditory nerve remains intact) to hear. The sensation of hearing is achieved by directly exciting the auditory nerve with controlled impulses of electrical current, which impulses are generated as a function of transduced acoustic energy. The acoustic energy is picked up by a microphone carried externally (not implanted) by the person using the device and converted to electrical signals. The electrical signals, in turn, are processed and conditioned by a signal receiver and processor, also referred to as a Wearable Processor (WP), in an appropriate manner, e.g., converted to a sequence of pulses of varying width and/or amplitude. The sequence of pulses, or command words that define such sequence of pulses, is carried by an external cable running from the WP to an external headpiece positioned on the side of the user's head. Generally, a magnet in the headpiece holds the headpiece in place. Such magnet also aligns the headpiece with a corresponding magnet in the implantable parts of the ICS system. Such implantable part receives the command words or pulse sequence, and converts them to appropriate stimulation current pulses that are applied to the auditory nerve through an electrode array implanted in the cochlea, as is known in the art.
[0004] While known ICS systems have succeeded in providing the sensation of hearing to the profoundly deaf, they unfortunately also have the disadvantage of appearing unsightly due to the external cable running from the WP to the headpiece positioned on the side of the user's head. The WP is typically worn or carried by the user on a belt or in a pocket. While the WP is not too large, it is likewise not extremely small, and hence also represents an inconvenience for the user. The cable which connects the WP with the headpiece is often a source of irritation and self-consciousness for the user.
[0005] The above-described aesthetic considerations, and inconvenience of an external wire, are addressed by U.S. Pat. No. 5,824,022, issued Oct. 20, 1998, for “Cochlear stimulation system employing Behind-The-Ear (BTE) Speech Processor With Remote Control.” The '022 patent teaches a small single external device that performs the functions of both the WP and the headpiece. The external device is positioned behind the ear to minimize its visibility, and requires no cabling to additional components. The '022 patent is incorporated herein by reference.
[0006] While the BTE device taught by the '022 patent resolves the issues of aesthetics and inconvenience, the resulting device, and known BTE hearing aids, disadvantageously include a microphone which is exposed to perspiration and rain, resulting in frequent failures. Therefore, there is a need for a microphone assembly that provides resistance to moisture, while maintaining a good frequency response. Further, due to the small size of known microphones used with BTE devices, the assembly of water-repellent microphone assemblies may be awkward and time consuming. Thus there is a further need for a construction method for small water-repellent microphones.
SUMMARY OF THE INVENTION
[0007] The present invention addresses the above and other needs by an improved method for constructing a water-repellent microphone providing easy assembly and good acoustic performance. In one embodiment, a water-repellent membrane and a washer are pre-assembled. The surface of the washer opposite the membrane is covered by an adhesive, and the adhesive is covered by a removable liner. The method of assembly comprises removing the liner, and pressing the membrane and washer over the sound port of the microphone. The washer provides spacing between the microphone and the membrane and increases the membrane area through which sound passes. In a second embodiment, the washer is provided as a separate element with adhesives and liners on both sides. A first liner is removed and the washer is attached to the membrane or the microphone, and then the second liner is removed and the assembly is completed.
[0008] In accordance with one aspect of the invention, there is provided a water repellent membrane and washer assembly. The membrane and washer are provided attached to one another. An adhesive and liner reside on the side of the washer opposite the membrane. The water-repellent microphone may then be assembled by removing the liner, and pressing the membrane and washer against the surface of the microphone which includes the sound port. The requirement to apply an adhesive, or to assemble the water-repellent microphone in a fixture is thus eliminated. Further, the requirement to manually manipulate small parts is minimized.
[0009] It is an additional feature of the present invention to provide a separate membrane and washer. The washer includes adhesives and liners on both side. The washer may either be attached to the microphone first, or to the membrane first. As in the first embodiment, there is not need to handle a separate adhesive, or to assemble the water-repellent microphone in a fixture.
[0010] It is a further feature of the invention to provide a water repellent membrane and a washer, wherein the washer resides between the membrane and the soundport of the microphone. The acoustic performance of the water-repellent microphone is limited by the area of the membrane through which sound passes. If the membrane is attached directly to the microphone, the membrane area is limited by the size of the microphone sound port. The addition of a washer between the membrane and the microphone increases the area sound may pass through to the size of the passage through the washer, thus providing good acoustic performance,
[0011] It is an additional feature of the invention to provide a water-repellent seal between the membrane, washer, and microphone. The water-repellent microphone is assembled using an adhesive between the membrane and the washer, and between the washer and the microphone. Such adhesive provides a 360 degree seal to effectively repel the water from entering the microphone.
[0012] It is a another feature of the present invention to provide a method of pre-assembly of a membrane and microphone. In known applications, a microphone sub-assembly is constructed by inserting a membrane, washer, and microphone into a boot (or housing). Great care must be taken during assembly to properly position the members. By pre-assembling the membrane, washer, and microphone, a single member may be inserted into the boot, thus eliminating the need to position the individual members.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The above and other aspects, features and advantages of the present invention will be more apparent from the following more particular description thereof, presented in conjunction with the following drawings wherein:
[0014] FIG. 1 shows a Behind-The-Ear (BTE) device residing upon the ear of a user;
[0015] FIG. 2 shows a partial cross-section of the BTE device;
[0016] FIG. 3 depicts a cross-section of a microphone subassembly suitable for use with the BTE device;
[0017] FIG. 4 shows a water-repellent microphone suitable for use within the microphone subassembly;
[0018] FIG. 5 depicts a cross-sectional view of a second microphone subassembly suitable for use with the BTE device;
[0019] FIG. 6 shows a second water-repellent microphone suitable for use within the second microphone subassembly;
[0020] FIG. 7 depicts a BTE device including an In-The-Ear (ITE) microphone, residing upon the ear of a user;
[0021] FIG. 8 shows additional details of an earhook attachable ITE microphone;
[0022] FIG. 9 shows a plan view of a water-repellent membrane and washer;
[0023] FIG. 9A shows a cross-sectional view of a first membrane and washer assembly taken along line 9 A- 9 A of FIG. 9 , wherein a first adhesive resides upon a first side of the washer, and a second adhesive resides upon a second side of the washer, and wherein the washer is water-repellent attached to the membrane by the second adhesive;
[0024] FIG. 9B depicts the membrane and washer of FIG. 9A , wherein the membrane and washer are not attached;
[0025] FIG. 9C shows the membrane and washer assembly of FIG. 9A with a first release liner residing upon the first adhesive;
[0026] FIG. 9D shows the membrane and washer assembly of FIG. 9B with the first release liner residing upon the first adhesive and a second release liner resides upon the second adhesive;
[0027] FIG. 10A shows a cross-sectional view of a second membrane and washer assembly taken along line 9 A- 9 A of FIG. 9 , wherein the first adhesive resides upon the first side of the first washer, and the second adhesive resides upon the second side of the first washer, and wherein a third adhesive resides upon a third side of the second washer and a fourth adhesive resides upon a fourth side of the second washer, and wherein the first washer is water-repellent attached to the membrane by the second adhesive, and the second washer is water-repellent attached to the membrane by the third adhesive.
[0028] FIG. 10B depicts the membrane and washers of FIG. 10A , wherein the membrane and washers are not attached;
[0029] FIG. 10C shows the membrane and washer assembly of FIG. 10A , with the addition of the first release liner over the first adhesive, and a fourth release liner over the fourth adhesive; and
[0030] FIG. 10D shows the membrane and washer on FIG. 10B , with the first release liner residing upon the first adhesive, the second release liner resides upon the second adhesive, a third release liner resides upon the third adhesive, and the fourth release liner residing upon the fourth adhesive.
[0031] Corresponding reference characters indicate corresponding components throughout the several views of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0032] The following description is of the best mode presently contemplated for carrying out the invention. This description is not to be taken in a limiting sense, but is made merely for the purpose of describing the general principles of the invention. The scope of the invention should be determined with reference to the claims.
[0033] The water-repellent microphone of the present invention provides a simple and effective method for sealing the a sound port of a microphone against water, thus providing improved performance and reliability. It will be apparent to those skilled in the art that the present invention has application to microphones used for various purposes. While the exercise of the method to Implantable Cochlear Stimulation (ICS) systems will be described in detail in the following description, the exercise of the present invention to other applications is intended to come within the scope of the present invention.
[0034] A Behind-The-Ear (BTE) hearing device 10 is shown carried and resting on an ear 12 of a user in FIG. 1 . The BTE device 10 may either be a standard hearing aid, or the external electronics for an Implantable Cochlear Stimulation (ICS) system. In either case, a microphone is required to receive acoustic energy (i.e., sound waves) and convert the acoustic energy into an electrical signal for further processing. In order to receive the acoustic energy, the microphone must be open to at least some extent to the environment.
[0035] As can be seen in FIG. 1 , the BTE device 10 forms an arch that starts behind the ear 12 and reaches over the ear 12 . The BTE device 10 ends near the top of the arch, and an earhook 14 continues the arch a short distance. In typical BTE hearing devices, the microphone resides in the BTE device 10 near the highest point of the arch, behind a microphone port 16 . While the microphone port 16 is advantageously positioned to receive sound in a natural manner (i.e., from the direction the patient is looking), the position also exposes the microphone to various moisture sources. Such moisture sources include rain, splashed water, perspiration, etc. Such moisture may not only degrade a microphone's performance, but in some instances it may render the hearing device inoperable.
[0036] A cross-section of a portion of a BTE device 10 is shown in FIG. 2 . A microphone subassembly 20 is positioned directly behind the microphone port 16 (see FIG. 2 ). A BTE device case 18 includes a water deflector 24 residing above the microphone port 16 . The water deflector 24 advantageously deflects large volumes of water attempting to enter the microphone port 16 . The microphone subassembly has an assembly front 26 which resides against the microphone port 16 , and an assembly rear 28 opposite the assembly front 26 .
[0037] A cross-section of a first microphone subassembly 20 a is shown in FIG. 3 . The microphone subassembly 20 a , is comprised of components assembled inside a first boot (or housing) 22 a . The exterior of the boot 22 a is shaped to cooperate with the BTE device case 18 to retain the microphone subassembly 20 a in the BTE device case 18 . The interior of the boot 22 a defines a microphone cavity, wherein a water-repellent microphone 30 a resides. A boot port 32 provides an opening to the water-repellent microphone 3 a . The boot port 32 extends from the assembly front 26 (see FIG. 2 ) to the microphone cavity. The microphone cavity extends from the cavity front end abutting the boot port 32 to the cavity rear end coinciding with the assembly rear 28 . When the microphone subassembly 20 a is mounted in the BTE case 18 , the boot port 32 is aligned with the microphone port 16 to provide an acoustic path for acoustic energy outside the BTE device 10 to enter the boot port 32 . A step 31 is defined at a front end of the microphone cavity. The step 31 provides a surface for the water-repellent microphone 30 a to seat against.
[0038] The water-repellent microphone 30 a comprises a microphone 34 , first washer 36 a , and water-repellent membrane 38 , as shown in FIG. 4 . The membrane 38 is water-repellent attached to the washer 36 a , and the washer 36 a is water-repellent attached to the microphone 34 , wherein the microphone port 40 is surrounded by the washer 36 a . When inserted into the boot 22 a (see FIG. 3 ), the membrane 38 resides against the step 31 , thus providing a large membrane 38 surface for effective transmission of sound.
[0039] A cross-section of a second microphone subassembly 20 b is shown in FIG. 5 . The second microphone subassembly 20 b is nearly identical to the first microphone subassembly 20 a , except for the absence of a step, and an additional washer added to water-repellent microphone 30 b . As shown in FIG. 6 , the second water-repellent microphone 30 b comprises the microphone 34 , the first washer 36 a , membrane 38 , and additionally, a second washer 36 b . The second washer 36 b is water-repellent attached to the membrane 38 , the membrane 38 is water-repellent attached to the washer 36 a , and the washer 36 a is water-repellent attached to the microphone 34 , wherein the microphone port 40 is surrounded by the washer 36 a . As is apparent by comparing FIGS. 4 and 6 , the additional of the second washer 36 b to the second water-repellent microphone 30 b is the only difference between the first water-repellent microphone 30 a , and the second water-repellent microphone 30 b . When the second water-repellent microphone 30 a is inserted in to the boot 22 b , the second washer 36 b resides against the front end of the microphone cavity, thus providing a large membrane 38 surface for effective transmission of sound.
[0040] Those skilled in the art will recognize that boots, microphone cavities, and sound ports may be made in a variety of shapes. Such other shapes, or combinations of shapes, are intended to come within the scope of the present invention.
[0041] An example of another type of microphone assembly that may be used with a BTE ICS system is disclosed in applicants' co-pending and co-owned U.S. patent application, Ser. No. 09/733,736, filed Dec. 8, 2000, entitled “Water-Resistant Microphone Subassembly”, which application is incorporated herein by reference.
[0042] As an alternative to a BTE ICS system with a microphone residing in the BTE device, an In-The-Ear (ITE) microphone may be utilized with the BTE device. An ITE microphone earhook 40 and BTE device 10 are shown residing on the ear 12 of a user in FIG. 7 . The ITE microphone earhook 40 comprises a second earhook 14 b , a third microphone subassembly 20 c , and a stalk 44 . The microphone subassembly 20 c is attached by the stalk 44 to the earhook 14 b . The microphone subassembly 20 c preferably resides behind the tragus and directed towards the concha of the ear, with a second boot port 32 a facing downward and somewhat rearward. Some users may vary location of the microphone subassembly 20 c , and these variations are intended to come within the scope of the present invention.
[0043] A more detailed view of the ITE microphone earhook 40 is shown in FIG. 8 . The microphone subassembly 20 c comprises the water-repellent microphone 30 a , a third boot (or housing) 22 c , and defines a sound boot port 32 a . The microphone 30 a (see FIG. 4 ) resides inside the boot 22 c . Alternatively, the ITE microphone earhook 40 may also utilize a water-repellent microphone 30 b as described in FIG. 6 above. Those skilled in the art will recognize that various other embodiments of an ITE microphone may be exercised. In each variation, similar environmental conditions motivate the use of a water-repellent microphone, and all of these variations utilizing a water-repellent microphone constructed as described herein are intended to come within the scope of the present invention.
[0044] A plan view of a membrane and washer assembly 46 is shown in FIG. 9 . A cross-sectional view of a first embodiment of the membrane and washer assembly 46 taken along line 9 A- 9 A of FIG. 9 is shown in FIG. 9A . A first membrane and washer assembly 46 a comprises the following elements: the membrane 38 , the first washer 36 a , a first adhesive 50 a on a first side of the washer 36 a opposite the membrane 38 , and a second adhesive 50 b on a second side of the washer 36 a adjacent to the membrane 38 . The membrane is preferably made from Versapor 10000R . The washer is preferably made from polyester. The adhesive 50 a is preferably acrylic (3M VHB), whereas the adhesive 50 b is preferably silicone-based or acrylic (3M VHB). The membrane and washer have about the same outside diameter, preferably between about 0.090 and 0.125 inches. The inside diameter of the washer is preferably between about 0.068 and 0.072 inches, wherein the washer defines a substantially cylindrical passage that passes through the center of the washer. The membrane 38 is preferably between about 0.005 and 0.010 inches thick, and the combined width of the combination of the washer 36 a and the adhesives 50 a , 50 b is preferably between 0.008 and 0.010 inches thick. The water-repellent microphone 30 a (see FIG. 4 ) in constructed by pressing the adhesive 50 a against the end of the microphone 32 which includes the sound port 40 (see FIG. 6 ), wherein the washer 36 a is substantially centered on the sound port 40 and encloses the soundport 40 .
[0045] In another embodiment, the membrane and washer 46 b as shown in FIG. 9B , are provided as a separate membrane 38 and washer 36 a , wherein the adhesives 50 a and 50 b reside on the washer 36 a . The construction of a water-repellent microphone using the membrane and washer 46 b comprises pressing the adhesive 50 a against the microphone, and pressing the adhesive 50 b against the membrane, in any order, thereby constructing the water-repellent microphone 30 a.
[0046] In yet another embodiment, a membrane and washer assembly 46 c is provided with a release liner 52 a residing over the adhesive 50 a , as shown in FIG. 9C . In all aspects other than the addition of the release liner 52 a , the membrane and washer assembly 46 c is identical to the membrane and washer assembly 46 a . The construction of the water-repellent microphone 30 a using the membrane and washer assembly 46 c includes a further step of removing the release liner before pressing the membrane and washer assembly 46 c against the microphone 32 .
[0047] In another embodiment of the present invention, a membrane and washer 46 d includes release liner 52 a over the adhesive 50 a , and release liner 52 b over adhesive 50 b , as shown in FIG. 9D . In all aspects other than the addition of the release liners 52 a and 52 b , the membrane and washer assembly 46 d is identical to the membrane and washer assembly 46 b . The construction of the water-repellent microphone 30 a using the membrane and washer assembly 46 d includes a further step of removing the release liner 52 a before pressing the membrane and washer assembly 46 c against the microphone 32 , and removing the release liner 52 b before pressing the membrane 38 against the adhesive 50 b.
[0048] A cross-sectional view of a membrane and washer assembly 46 e is shown in FIG. 1A . The membrane and washer assembly 46 e includes the first washer 36 a , the membrane 38 , and a second washer 36 b . The washers 36 a and 36 b are water-repellent attached to the membrane 38 by the adhesive 50 b and an adhesive 50 c , respectively. The adhesive 50 a resides on a first side of the washer 36 a , which first side faces away from the membrane 38 , and a fourth adhesive 50 d resides on a fourth side of the second washer 36 b , which fourth side faces away from the membrane 38 . The membrane and washer assembly 46 e may be attached to a microphone 32 by pressing the membrane and washer assembly 46 e against the microphone 32 ., thus constructing the water-repellent microphone 30 b (see FIG. 6 ).
[0049] A membrane and washer 46 f is shown in FIG. 10B comprising the first washer 36 a , the membrane 38 , and a second washer 36 b , wherein the washer 36 a includes the adhesive 50 a on the first side, and the adhesive 50 b on the second side, and the washer 36 b includes a third adhesive 50 c on a third side, and the fourth adhesive 50 d on the fourth side. The water-repellent microphone 30 b is constructed by pressing the first adhesive 50 a against the microphone 32 , pressing the membrane 38 against the second adhesive 50 b , and pressing the third adhesive 50 c against the membrane 38 .
[0050] A membrane and washer assembly 46 g shown in FIG. 10C comprises the membrane and washer assembly 46 e with the further addition of the first release liner 52 a over the adhesive 50 a , and a fourth release liner 52 d over the adhesive 50 d . The water-repellent microphone 30 b is constructed by removing the release liner 52 a and pressing the adhesive 50 a against the microphone 32 .
[0051] An additional membrane and washer 46 h is shown in FIG. 10D . The membrane and washer 46 h comprises the membrane and washer assembly 46 f with the further addition of the first release liner 52 a over the adhesive 50 a , the second release liner 52 b over the adhesive 50 b , a third release liner 52 c over the adhesive 50 c , and the fourth release liner 52 d over the adhesive 50 d . The water-repellent microphone 30 b is constructed by removing the release liner 52 a and pressing the adhesive 50 a against the microphone 32 , removing the second release liner 52 b and pressing the membrane against the adhesive 50 b , and removing the third release liner 52 c and pressing adhesive 50 c against the membrane.
[0052] In an alternative embodiment, the washer is attached to the membrane by methods other than adhesives. For example, the washer may be attached to the membrane by thermobonding or by ultrasonic bonding. Those skilled in the art will recognize these, and other boding techniques, which are intended to come within the scope of the present invention.
[0053] Those skilled in the art will recognize variations to the membrane and washers described above. In particular, the order of construction of the water-repellent microphones 30 a and 30 b may freely vary from the order the steps were recited in above. Further, the inclusion of a fourth release liner and a fourth adhesive are optional in the embodiments in which they are included.
[0054] While the invention herein disclosed has been described by means of specific embodiments and applications thereof, numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope of the invention set forth in the claims. | A water-repellent microphone and an improved method for constructing such a water-repellent microphone provides easy assembly and good acoustic performance. In one embodiment, a water-repellent membrane and a washer are pre-assembled. The surface of the washer opposite the membrane is covered by an adhesive, and the adhesive is covered by a removable liner. The method of assembly comprises removing the liner, and pressing the membrane and washer over the sound port of the microphone. The washer provides spacing between the microphone and the membrane and increases the membrane area through which sound passes, thus providing good acoustic performance. In a second embodiment, the washer is provided as a separate element with adhesives and liners on both sides. A first liner is removed and the washer is attached to the membrane or the microphone, and then the second liner is removed and the assembly is completed. | 7 |
[0001] This application claims priority under 35 U.S.C. 119 to Korean Patent Application No. 10-2006-0137272 (filed on Dec. 29, 2006), which is hereby incorporated by reference in its entirety.
BACKGROUND
[0002] A metal-oxide-semiconductor (MOS) transistor (MOSFET) may be used primarily as a switching device in an integrated circuit. The MOS transistor may lend several benefits in terms of ease of electrical control, high-integration and enhanced switching characteristics.
[0003] A MOS transistor may include a gate electrode for turning on/off a channel region in a semiconductor substrate may be formed on and/or over a gate insulation layer. The MOS transistor may also include a source region and a drain region, which are impurity diffusion regions formed in the semiconductor substrate on both sides of the gate electrode.
[0004] In obtaining a highly integrated MOS transistor, its switching characteristics may become deteriorated due to a single channel effect and narrow width effect. Accordingly, achieving further integration may become limited. Also, the source region and the drain region used as input/output terminals of a signal may be formed as a diffusion region by implanting impurities into the semiconductor substrate. Even still, the MOS transistor may have an adverse impact on switching characteristics such as junction breakdown, leakage current, and increases in area due to lateral diffusion of the impurities, etc. Therefore, there is a need for a switching device having a different structure.
SUMMARY
[0005] Embodiments relate to a switching device that can include at least one of the following: a switching electrode formed over a semiconductor substrate; a first terminal electrode formed over the semiconductor substrate spaced apart from the switching electrode; and a second terminal electrode extending laterally over the semiconductor substrate including the switching electrode and the first terminal electrode. In accordance with embodiments, the second terminal has a first end that is fixedly supported and a second end that is not fixedly supported.
[0006] Embodiments relate to a switching device that can include a switching electrode formed over a semiconductor substrate; a first terminal electrode formed over the semiconductor substrate spaced apart from the switching electrode; and a second terminal electrode extending laterally over the semiconductor substrate including the switching electrode and the first terminal electrode. In accordance with embodiments, the second terminal can have a first end that is fixedly supported and a second end that is not fixedly supported.
[0007] Embodiments relate to a method of manufacturing a switching device that can include at least one of the following steps: forming a first metal layer over a semiconductor substrate; forming a second metal layer formed spaced apart laterally from the first metal layer over the semiconductor substrate; forming an elastic layer spaced apart vertically from and extending over the first metal layer and the second metal layer. In accordance with embodiments, the elastic layer can include a first end fixedly positioned and a second end not fixedly positioned.
DRAWINGS
[0008] Example FIGS. 1 and 2 illustrate a switching device, in accordance with embodiments.
[0009] Example FIGS. 3 and 4 illustrate a method of fabricating a switching device, in accordance with embodiments.
DESCRIPTION
[0010] As illustrated in example FIG. 1 , a switching device in accordance with embodiments can include switching electrode 12 and first terminal electrode 14 spaced at a predetermined interval formed on and/or over semiconductor substrate 10 . Switching electrode 12 and first terminal electrode 14 can be formed of a metal layer and connectable to wiring, respectively.
[0011] Second terminal electrode 18 can be positioned spaced at a predetermined interval vertically above first terminal electrode 14 and switching electrode 12 . One end of second terminal electrode 18 can extend over switching electrode 12 and terminal electrode 14 . On the other hand, a second end of second terminal electrode 18 can be fixedly positioned on and/or over support layer 16 a formed on and/or over substrate 10 .
[0012] As illustrated in example FIG. 2 , second terminal electrode 18 can be composed of an elastic material such that it is free to be bent downwardly towards semiconductor substrate 10 . In the switching device in accordance with embodiments, since second terminal electrode 18 can perform the switching operation by way of elasticity, second terminal electrode 18 can be formed of a thin metal film having elasticity.
[0013] In two opposed electric conductors, attractive force or repulsive force operates by way of charged electrical charges. The electric conductor can be positioned spaced at a predetermined interval and easily bent by way of attractive forces when charges having opposite polarity are accumulated. The attractive force can be maintained up to the time before the charges are discharged. The switching device in accordance with embodiments can apply voltage so that different charges can be accumulated in switching electrode 12 and second terminal electrode 18 using such a principle.
[0014] The attractive force can be generated between switching electrode 12 and second terminal electrode 18 using an electric field. When the attractive force is generated between switching electrode 12 and second terminal electrode 18 , second terminal electrode 18 composed of an elastic material can be easily bent downwardly toward switching electrode 12 . Since a first end of second terminal electrode 18 is supported by support layer 16 a and the second end thereof is spaced above first terminal electrode 14 , the second end can directly contact first terminal electrode 14 . Thereby, first terminal electrode 14 and second terminal electrode 18 can be electrically conducted when connected.
[0015] Accordingly, the switching device in accordance with embodiments can obtain high integration and thinness by reducing the size of first terminal electrode 14 and switching electrode 12 . Also, since first terminal electrode 14 and second terminal electrode 18 can be physically contacted to perform switching, the switching device in accordance with embodiments can have enhanced switching characteristics, as compared to a switching device (e.g., a MOS transistor) by way of channel formation.
[0016] As illustrated in example FIG. 3 , a method of manufacturing a switching device in accordance with embodiments can include forming switching electrode 12 and first terminal electrode 14 on and/or over semiconductor substrate 10 . Switching electrode 12 and first terminal electrode 14 can be formed of a conductive layer. Furthermore, it is preferable that switching electrode 12 and first terminal electrode 14 are composed of a metal material to obtain a fast response speed. Switching electrode 12 and first terminal electrode 14 can be formed by applying a patterning or a damascene process by means of a photolithographic process.
[0017] As illustrated in example FIG. 4 , support layer 16 can then be formed on and/or over semiconductor substrate 10 including switching electrode 12 and first terminal electrode 14 . Support layer 16 can be composed of a silicon insulation material and have a low dielectric constant in order that it can prevent loss of signal charges due to parasitic capacitance and signal delay.
[0018] A conductive film can then be formed and patterned on and/or over support layer 16 to form second terminal electrode 18 . Second terminal electrode 18 can extend laterally over switching electrode 12 and first terminal electrode 14 . An isotropic etching process may then be conducted on support layer 16 .
[0019] The support layer 16 between first terminal electrode 14 and second terminal electrode 18 and also between switching electrode 12 and second terminal electrode 18 can then be removed by an etching process. Thereby, support layer 16 a supporting second terminal electrode 18 is formed on and/or over semiconductor substrate 10 adjacent switching electrode 12 . Moreover, space can be formed between second terminal electrode 18 and first terminal electrode 14 and also between second terminal electrode 18 and switching electrode 12 .
[0020] The switching device in accordance with embodiments can include a second terminal electrode spaced vertically above the switching electrode and which is also made of an elastic material to enable bending of the second terminal electrode due to the attractive forces between the second terminal electrode and the switching electrode. Through such a construction, the second terminal electrode and the first terminal electrode are physically contacted, thereby making it possible to perform turn-on.
[0021] Unlike the MOS transistor, the switching device in accordance with embodiments neither uses an impurity diffusion region nor performs switching action through a channel region. Accordingly, it can achieve high integration and thinness. Moreover, the switching function can be performed by way of the physical contact of the first terminal electrode and the second terminal electrode, thereby making it possible to improve turn on-off characteristics.
[0022] Although embodiments have been described herein, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More particularly, various variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. In addition to variations and modifications in the component parts and/or arrangements, alternative uses will also be apparent to those skilled in the art. | A switching device having a construction that facilitates physical contact between the second terminal electrode and the first terminal electrode, thereby enabling the performance of turn-on. Embodiments do not require an impurity diffusion region nor performs switching action through the channel region so that can become highly integrated and thinness. Also, switching can be performed by way of the physical contact of the first terminal electrode and the second terminal electrode, thereby making it possible to improve turn on-off characteristics. | 7 |
This is a division of application Ser. No. 632,215 filed Apr. 15, 1996, now U.S. Pat. No. 5,740,972.
BACKGROUND OF THE INVENTION
The present invention relates to papermaking and refining of lignocellulosic and other natural and synthetic fibrous materials in the manufacture of paper, paperboard, and fiberboard products. In particular, the invention relates to replacable refiner fillings used in the process of refining chip or pulp.
In nearly all production refining equipment in use today including beaters, jordans, conical refiners, multi-disc, and disc refiners, the refining working surfaces of the refiner fillings are comprised of closely spaced bars and grooves which work against each other through relative rotation while the fibrous material passes between them. The clearance between the opposed bar and groove working surfaces determines the power applied to the refiner, as well as the extent of refining of the fibrous material.
In each kind of refiner equipment, it is often desirable to make bars as narrow and as closely spaced from each other as possible in order to achieve maximum bar edge length for the refiner with resultant distribution of the refiner power over a greater number of bar contact or bar crossing points. This relative intensity, or specific edge load as it is called, is widely recognized as an important quality parameter for most paper and board products.
While the bars of any refiner type can be of any practical width and spacing, the actual width and spacing are limited by the materials and methods used to make them, or by the cost to make them, or both. In a typical disc refiner, the replacable working surfaces, or refiner plates as they are most commonly called, may be made by casting or machining. In some instances they may be made by fabricating wherein appropriately spaced bars are affixed by welding onto a base.
In the case of cast refiner plates, the width of the bar and the width of the groove are limited to no less than about 1/8". At normal groove depths of 1/4" or so, cast bars narrower than this are prone to breakage due to internal flaws, and the need to have a draft angle of 3 deg. or so for the casting process, causes the groove volume (which provides for passage of fibrous material) to be greatly diminished at closer bar spacing than about 1/8".
In the case of machined refiner plates, the limiting factor is cost. The cost is more or less proportional to the number of grooves which must be milled to the required depth in a solid steel blank.
In the case of fabricated plates, cost is also a constraint because bars are individually welded.
Another important feature of replacement refiner plates is their useful life. During operation, the bars become worn down, until at some point, the depth of the groove between bars is so shallow that the refiner can no longer adequately transport fibrous material through the refiner plates. There are several causes of wear including abrasive nature of the fibrous materials and other particles in the medium, and the clashing of the refiner plates in the event of sudden interruption of the flow of process material.
The precise nature of the wearing of refiner plates is not fully understood. Hardness of the bar material has been shown to be an important factor. It has also been demonstrated that the rate of wear is very closely related to the corrosion resistance of the bar material.
In general, a compromise must be reached between the hardness, corrosion resistance, and toughness of the material that is chosen for a cast or machined refiner plate. Toughness is a required property because occasional tramp metal contamination occurs in the process medium. If the plates were to shatter when a piece of metal passed through the refiner, it would cause severe and costly operational problems for the paper or board mill.
There are several potential wear advantages to fabricated or machined refiner plates, however a serious limitation results from the necessity of producing refiner discs in a complete circle configuration. A full circle replacement plate for a 34" or larger refiner will weigh several hundred pounds thus requiring lifting aids for installation into, and removal from, a refiner. Cast refiner plates can be, and usually are produced in segments, with each segment being 30, 45, or 60 degrees and with 12, 8, or 6 segments respectively being required to make up a complete replacement working surface for a single disc of a disc refiner. Each segment will weigh less than 35 pounds, and will usually be individually bolted into the place on the disc, such that an entire set of plates can be replaced by a person without the need for special lifting devices. For this and other reasons, most replacement disc refiner plates are castings, usually of special cast iron or stainless steel alloys.
As a practical matter, one of the reasons machined or fabricated plates are not produced as segments has to do with an operational requirement for non-parallel edge crossing of the refiner bars for processing fibrous material. If a stator plate and a rotor plate, whose working surfaces act against each other, contain bars whose leading edges pass each other in parallel or nearly parallel condition, there is a known tendency for excessive cutting of the fibrous material being processed. Thus it is often a process requirement that a refiner plate does not have any precisely radial bars, but rather that it have bars with at least a slight offset or oblique from a radial orientation, typically between 3 and 20 degrees.
Refiner disc plate segments have precisely radial side edges such that it is a somewhat costly complication to produce a disc working surface pattern having no precisely radial bar or groove at the segmental dividing lines. Therefore, the segment joint must cut across the pattern of bars and grooves at a shallow angle. This requirement is difficult and costly to accomplish in the case of machined and fabricated plates and which, even in the case of cast plates, leaves narrowly tapered bars likely to be very much weakened at their extremities.
In sum, the utility of disc refiner plates is limited by the operational requirement for bars oriented obliquely to radial, by consequent manufacturing limitations, and by the rate of working surface wear through corrosion and abrasion.
SUMMARY OF THE INVENTION
The present invention provides improvements in replaceable refiner fillings and has as a primary objective the manufacture of refiner fillings with working surfaces using relatively narrow, closely spaced bars on the working surface of the plate. This is accomplished by using relatively thin blades of any suitable material, separated by shallower spacer bars having a thickness which determines the width of the grooves, and subsequently fusing or bonding the assembled blades and spacers into a solid piece by methods appropriate for the blade and spacer materials being used.
In another primary aspect of the invention, blade and spacer components are selected from metallic materials having different corrosion resistance. Cathodic protection for the refiner blade elements is achieved by using a metallic material for the spacer which is less noble, according to the Electromotive-Force Series of Metals, than the material used for the blade. In this way, the spacer, which is not subject to appreciable abrasion, will pit and corrode harmlessly, while the blade or bar wear is greatly reduced. This feature of galvanic, or cathodic, protection is also applied to cast or machined refiner plates by inserting or attaching sacrificial metal elements.
In a further primary objective of the invention, improved segmental replacement disc refiner plates are produced with segments having both non-circular edges (i.e., side edges) which are not precisely radial. Instead, the side edges are oblique to the precisely radial line by an angle between about 3 and 20 degrees such that the refiner plate segmental dividing line is parallel to the adjacent refiner blade.
OBJECTS OF THE INVENTION
It is an object of the invention to provide improved refiner plates for use in papermaking refiners.
It is an object of the invention to provide improved refiner plates in which bars and spacers are assembled in proper order and are fused or bonded together.
It is a further object of the invention to provide improved refiner plates in which bars and spacers are selected for corrosion resistance.
It is a further object of the invention to provide improved refiner plates in which bars and spacers are selected from the Electromotive-Force Series of Metals with the spacers being a metal less noble than the metal selected for the bars.
It is a further object of the invention to provide improved refiner disc plate segments of a circle having side edges oblique to the radius of the circle and with at least a portion of the bars parallel to an oblique side edge.
It is a further object of the invention to provide improved refiner disc plate segments having side edges oblique to a radius of the disc with the bar pattern parallel to an oblique side edge and with the bar pattern repeating as necessary to have all bars on the working surface of the disc plate within a given range of obliquity to the radius.
Other and further objects of the invention will occur to one skilled in the art with an understanding of the following detailed description of the invention or upon employment of the invention in practice.
DESCRIPTION OF THE DRAWING
A preferred embodiment of the invention has been chosen for purposes of illustrating the construction and operation of the invention and is shown in the accompanying drawing in which:
FIG. 1 is a plan view of the working surface of a refiner disc plate showing an arrangement of bars according to the invention.
FIG. 2 is a section view taken along FIG. 2--2 of FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawing, a preferred embodiment of a refiner disc 10 according to the invention comprises a supporting plate 12 to which blades 14 and spacers 16 are affixed and wherein the blades and spacers define the disc working surface and intervening grooves 18.
The blades may be fabricated of any suitable durable material including metals such as aluminum, bronze, nickel alloy, and ceramic or composite materials capable of bonding to spacers. Similarly, the spacers are any suitable material that can be strongly bonded to the supporting plate. Materials for blades are selected for hardness and corrosion resistance.
In a preferred embodiment of the invention, the blades are fabricated of stainless steel, and the spacers of plain carbon steel, and the backing plate of either plain carbon steel or stainless steel. The entire assembly of blades, spacers and backing plate are bonded to comprise a refiner disc by a process of copper brazing or high temperature diffusion welding.
During use, the topmost surface of the stainless steel blade is constantly exposed to abrasive removal of a protective oxide layer. The exposed surface is much more resistant to abrasive/corrosive wear because of the cathodic protection provided by the immediately adjacent and less noble carbon steel spacer.
As shown in FIG. 1, a preferred embodiment of the invention, the refiner disc 10 is defined by outer 20 and inner 22 concentric segments and side edges 24, 26 offset or oblique to the radius R of the outer circle.
Each segment may have a value for θ of 30, 45, or 60 degrees so that 12, 8, or 6 segments, respectively comprise a refiner disc.
The extent of offset of the side edges is indicated by the angle which is preferably between 3 and 20 degrees off the radial. Beginning at the right side edge 24 in FIG. 1, the segement bars 14 are positioned parallel to the right side edge and extend from the outer periphery 20 inwardly toward the inner periphery 22 of the segment. As shown in FIG. 1, the bars terminate short of the inner periphery thereby defining with the inner periphery a feeding zone 28 for pulp entry to the refiner blades and grooves. Feeder bars 30 aid in directing pulp flow into the refeiner grooves. Bores 32 accommodate fasteners (not shown) for securing the segments in place.
It will be apparent from FIG. 1 that blade obliqueness to the segment radial R increases with distance normal to right side edge 24. For example, the blade 14' nearest the right side edge has an oblique angle equal to ∝, while bar 14" has a greater oblique angle, ∝. It is desirable with refiner plates to avoid shallow crossing angles (i.e., high degree of obliquity to radial) of stator and rotor blades and therefore desirable to maintain blade obliqueness in a range of 3 to 20 degrees. Hence, the blade pattern is begun anew at that location in the refiner segment where increasing obliqueness (as the case with blade 14") approaches 20 degrees. So, at this location the bar pattern is reset beginning with a low angle ∝, say 3 degrees, and continuing until the bar pattern reaches the left side edge of the segment 26.
Blade pattern repetition may be unnecessary in the case of narrower disc segments as in a refiner disc with 12 segments of 30 degrees each.
It will be seen that the disc refiner segment with non-radial side edges permits the blade of spacer immediately adjacent to one edge to be parallel to the edge while not being precisely radial in its orientation. Therefore, the bars on opposing rotor and stator plates never cross radially and thereby avoid refiner process disadvantages induced by radial crossing of bars. At the same time, the refiner plates according to the invention have the advantages of reduced cost and increased durability with having short blades bordering on one edge only of the disc segment.
Various changes may be made to the structure embodying the principles of the invention. The principles of the invention, while described in preferred embodiment of refiner disc segments, are also applicable to other configurations of refiner fillings. For example, the invention also has application to working surfaces of refiners in conical configurations.
The foregoing embodiments are set forth in an illustrative and not in a limiting sense. The scope of the invention is defined by the claims appended hereto. | Replacable refiner plates used for papermaking and refining of lignocellulosic and other natural and synthetic fibrous materials in the manufacture of paper, paperboard, and fiberboard products. The refiner plates include blade patterns and use corrosion resistant materials. | 1 |
This application is a §371 national stage of PCT International Application No. PCT/US2003/039207, filed Dec. 8, 2003, and claims the benefit of U.S. Provisional Application No. 60/431,897, filed Dec. 9, 2002, the contents of which are hereby incorporated by reference.
The invention disclosed herein was made with United States government support under grant numbers TLN 10-122 and DO 0788 from the Department of the Army, Army Research Office 1132; Scientific Services Program. Accordingly, the United States government has certain rights in this invention.
Throughout this application, various publications are referenced by author and date. Full citations for these publications may be found at the end of the specification immediately preceding the claims. The disclosures of these references in their entireties are hereby incorporated by reference into this application to describe more fully the art to which this invention pertains.
BACKGROUND OF THE INVENTION
Irreversible inhibitors of acetylcholinesterase (AChE) are used extensively as insecticides and have also been used as chemical weapons. World-wide stockpiles of these agents for use in chemical warfare are estimated to exceed 200,000 tons (Lejeune et al, 1998). The extreme toxicity of these compounds and their global proliferation has made the development of protective agents and antidotes an important research priority.
AChE inhibitors are derivatives of phosphoric, pyrophosphoric and phosphonic acids. These agents react to form a phosphoester with the serine residue that resides in the active site of the AChE enzyme. This phosphoester form of the enzyme is inactive, although the active enzyme can be regenerated through hydrolysis of the phosphoester.
The toxicity of the organophosphorus agents arises from the stability of the phosphoester intermediate that is formed with the enzyme. As its name implies, AChE functions to cleave the ester linkage of acetylcholine, forming acetic acid and choline. To do this, the enzyme transiently forms an ester with the carboxyl moiety of acetylcholine, releasing choline. The resulting carboxylate ester of the enzyme is inactive. However, this ester undergoes rapid hydrolysis, measured in milliseconds, to regenerate the original, active form of the enzyme. In contrast, the rates of hydrolysis for the phosphate esters of AChE are measured in hours. The reversible inhibitors of AChE that are used clinically generate a carbamylated enzyme and have rates of hydrolysis measured in minutes. Thus, the time required for regeneration of the active enzyme via hydrolysis of the ester linkage of the inactive, acetylated enzyme defines the difference between the enzyme's normal function, reversible inhibition, and irreversible inhibition.
One strategy for developing antidotes to irreversible AChE inhibitors has been the synthesis of highly nucleophilic small molecules capable of efficiently cleaving phosphate esters. Hydroxylamine is one such compound that was demonstrated to significantly increase the rate of hydrolysis of phosphorylated AChE. However, efficient hydrolysis was only achieved at toxic concentrations of hydroxylamine.
To date, this approach has yielded only one compound that has shown clinical efficacy, 2-pyridine aldoxime methylchloride (2-PAM). The oxygen atom of this molecule is part of an oxime functional group. The oxime moiety is a hydroxylamine-like nucleophile formed from the reaction of hydroxylamine with aldehydes or ketones. The effectiveness of this compound is limited by its inability to cross the blood-brain barrier. However, effectiveness is further impaired by an inability to regenerate the enzyme once “aging” has occurred. This latter impediment means that treatment is only effective if administered within a few minutes to a few hours of toxin exposure, depending on the toxin.
Organophosphorus agents, particularly some of the more recent additions to chemical weapons arsenals, have the propensity to become truly irreversible inhibitors through the aging process. This molecular process occurs when, having first reacted with AChE to inactivate the enzyme, a phosphoester bond undergoes cleavage, resulting in an anionic ester which is extremely resistant to hydrolysis. The phosphorylated enzyme which has aged in this way is completely refractory to regeneration by currently available antidotal agents, including 2-PAM. It is this aging process that makes the phosphorus-derived chemical warfare agents, such as sarin, soman, VX and tabun, extremely lethal.
In addition to efforts to produce antidotes, research has focused on protecting against exposure to organophosphorus agents, thereby preventing or moderating their toxic effects. One important strategy has been the use of recombinant enzymes for the biocatalytic degradation of organophosphorus agents. This methodology is being utilized in the development of protective clothing as well as agents for surface or aerial decontamination. In these methodologies, microbial enzymes, such as cholinesterases or organophosphorus hydrolases, are attached to a solid support in a manner that retains some portion of their catalytic activity. Such biocatalytic materials include silicone polymers (Gill 2000) and polyurethane foams (LeJeune 1996, 1999; Cheng 1996).
Peripheral blocking methods, i.e., methods that rely on agents that would intercept nerve agents in the circulatory system before they partition into the central nervous system or muscle, are currently the only choice for protection against organophosphorus agents. The standard technology in use today for protection against nerve agents is based upon the recombinant enzyme, butyrylcholinesterase (BuChE). BuChE rapidly reacts with nerve agents to form an intermediate phosphoester with a serine in the active site much as occurs when these agents react with AChE. Compounding the slow rate of hydrolysis of this intermediate is the inactivation of the enzyme through the process of molecular aging discussed above. Thus, BuChE is essentially an autocatalytic stoichoeometric blocker rather than a true hydrolytic enzyme. Butyrylcholinesterase mutants demonstrate enzymatic turnover, but low turnover, combined with high immunogenicity, an inability to cross the blood-brain barrier and a high equivalent weight ratio (almost 500:1 for butyrylcholinesterase to nerve gas). These factors make it difficult to maintain in vivo enzyme levels sufficient to protect against a lethal dose of a toxin such as a nerve agent.
To date, the above-mentioned shortcomings have not been overcome.
SUMMARY OF THE INVENTION
This invention provides a method for determining whether a peptide forms a phosphorus based ester with an organophosphorus agent. This invention also provides a method for determining whether, among a plurality of peptides, there exists a peptide that forms a phosphorus-based ester with an organophosphorus agent. This invention further provides a method for identifying and characterizing a peptide, among a plurality of peptides, that forms a phosphorus-based ester with an organophosphorus agent. This invention further provides a peptide which forms a phosphorus-based ester with an organophosphorus agent, which peptide comprises a nucleophilic functional group. This invention also provides a peptide library, wherein each peptide therein comprises a nucleophilic functional group. This invention further provides a composition of matter comprising a peptide and a pharmaceutical or a nonpharmaceutical carrier. This invention also provides an article of manufacture comprising a peptide affixed to a solid substrate.
This invention, further provides a method for reducing the likelihood, of injury due to exposure to an organophosphorus-containing agent in a subject exposed to or at risk of exposure to such agent, comprising administering to the subject an effective amount of a peptide of the instant invention.
This invention also provides a method for decontaminating an area exposed to an organophosphorus-containing agent comprising introducing to the area an effective amount of a peptide of the instant invention. This invention further provides a kit for decontaminating an area exposed to an organophosphorus-containing agent comprising the instant peptides and instructions for use.
Finally, this invention provides a method for determining the presence of an organophosphorus-containing agent in an area.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 : A sarin analog tethered to a fluorescent label was synthesized as shown to provide a low toxicity version of soman that would retain its chemical reactivity and report its reaction with a peptide molecule displayed on a library bead.
FIG. 2 : Structure of the fluorescently labeled sarin analog (1) and additional analogs with the following properties, hydrophobicity (2), water-solubility (3) and UV-activity (4).
FIG. 3A : Analog (2) was synthesized by fluoration of 1-(isopropylhydroxyphosphinyl)-10-undecene with DAST.
FIG. 3B : Synthesis of analog (3). The olefin (5) was oxidatively converted to aldehyde (6) with OSO 4 and NaIO 4 . Reductive amination of (6) with dimethyl amine and sodium borohydride afford the amine (7). Quaternazation of the tertiary amine (7) with iodomethane in DMF gave (8) which was treated with DAST to afford the analog (3).
FIG. 3C : Synthesis of analog (4). Treatment of phenylphosphonic dichloride with excess isopropanol in the presence of triethylamine afforded the diisopropyl phenylphosphonate which was subjected to basic hydrolysis with NaOH to generate the monoester (isopropyl phenylphosphonic acid). The nerve gas analog (4) was generated by treatment with DAST in a manner similar to analog (1).
DETAILED DESCRIPTION OF THE INVENTION
Definitions
In this invention, “administering” can be effected or performed using any of the various methods and delivery systems known to those skilled in the art. The administering can be performed, for example, intravenously, orally, via implant, transmucosally, transdermally, intramuscularly, and subcutaneously. In a preferred embodiment, the peptide is administered intramuscularly.
Determining an “effective amount” of the instant peptide for decontamination purposes can be done based on in vitro data. Determining an effective amount of the instant peptide for administering to a subject can be done based on animal data using routine computational methods. In one embodiment, the effective amount contains between about 10 mg and 1000 mg of the instant peptide. In another embodiment, the effective amount contains between about 50 mg and about 500 mg of the peptide. In a further embodiment, the effective amount contains between about 100 mg and about 250 mg of the peptide, and preferably about 200 mg thereof.
“Pharmaceutical carriers” are well known in the art and include, but are not limited to, 0.01-0.1 molar phosphate buffer, 0.8% saline solution, propylene glycol, polyethylene glycol, vegetable oils and injectable organic esters such as ethyl oleate. Aqueous carriers include water, alcoholic/aqueous solutions, emulsions or suspensions, including saline and buffered media. Parenteral vehicles include sodium chloride solution, Ringer's dextrose, dextrose and sodium chloride, lactated Ringer's or fixed oils. Intravenous vehicles include fluid and nutrient replenishers, electrolyte replenishers such as those based on Ringer's dextrose, and the like. Preservatives and other additives may also be present, such as, for example, antimicrobials, antioxidants, chelating agents, inert gases and the like.
“Nonpharmaceutical carriers” include, without limitation, foams and aerosols. For example, a polyurethane foam can be synthesized to incorporate a peptide of the instant invention using methods standard in the art of polymer synthesis. In one example, a hydrophilic polyurethane prepolymer is reacted with water containing the peptide and a surfactant, forming a foam. Such prepolymers are known in the art and comprise a urethane capped with multiple isocyanate functionalities. As one of skill in the art would be aware, various surfactants can be used in order to alter the porosity, density and surface properties of the foam.
The term “organophosphorus agent” is synonymous with “organophosphorus-based agent”, and is used herein to refer to a chemical compound comprising carbon, hydrogen, phosphorous and oxygen. Organophosphorus agents include, without limitation, phosphorus-based esters. A number of commercially important insecticides, as well as chemical warfare agents, contain a phosphorus-based -ester moiety which either is inherently toxic to humans or is readily converted into a toxic moiety. Examples of such agents include, without limitation, malathion, parathion, paraoxon, schradan, dichlorfenthion, soman, sarin, VX, GB and tabun.
The term “phophorus-based ester” is used herein to refer to any ester of phosphorous. Examples of such esters include, without limitation, a phosphate ester, a phosphonate ester and a phosphinate ester.
The term “peptide” is used herein to refer to a polymer of amino acid residues. In one embodiment, a peptide has 15 or fewer amino acid residues. Amino acid residues include, without limitation, any of the 20 naturally occurring amino acids or modifications thereof, as well as natural or synthetic derivatives thereof. A peptide can also comprise one or more modified amino acid residues. Modifications include, without limitation, the conjugation to, an amino acid residue of a non-protein moiety (e.g. an oxime or a cyclodextran). Other modifications include the addition of a chemical tag useful for identification or purification. Examples of chemical tags include, without limitation, a biotin molecule a radioisotope and a fluorescent molecule.
As used herein, a “solid substrate” and a “solid support” are synonymous, and shall mean any water- and/or lipid-insoluble support to which a peptide can be affixed. Examples of solid supports include, without limitation, alumina pellets, trityl agarose and glass/silica beads, and polymers such as nylons, acrylates, and silicas.
“Subject” shall mean any animal, such as a primate, mouse, rat, guinea pig or rabbit. In the preferred embodiment, the subject is a human
Embodiments of the Invention
This invention provides a method for determining whether a peptide forms a phosphorus-based ester with an organophosphorus agent comprising the steps of contacting the peptide with the agent under conditions permitting the formation of a phosphorus-based ester and determining whether a phosphorus-based ester has formed.
This invention also provides a method for determining whether, among a plurality of peptides, there exists a peptide that forms a phosphorus-based ester with an organophosphorus agent. This method comprises the steps of contacting the plurality of peptides with the agent under conditions permitting formation of a phosphorus-based ester and determining whether a phosphorus-based ester has, formed.
This invention further provides a method for identifying and characterizing a peptide among a plurality of peptides that forms a phosphorus-based ester with an organophosphorus agent. This method comprises the steps of contacting the agent with the plurality of peptides under conditions permitting the formation of a phosphorus-based ester, identifying the peptide or peptides that form such an ester with the agent and determining the amino acid sequence of the peptide so identified.
In an embodiment of any of these methods, the organophosphorus agent which reacts with a peptide is selected from the group consisting of malathion, parathion, paraoxon, schradan, dicholorfenthion, soman, sarin, VX, GB and tabun, or an analog thereof.
In any of these three methods, the phosphorus-based ester can be any ester of phosphorus including, for example, a phosphate ester, a phosphonate ester or a phosphinate ester.
In one embodiment of the instant methods, the peptides are bound to a solid support such as a bead, a microtiterplate, a glass chip or a silicone chip. In another embodiment, the agent is labeled with a detectable marker. In a preferred embodiment, the detectable marker is a radioisotope, a fluorescent molecule, biotin or an enzyme. In one example, the agent is a nerve agent and the detectable marker is rhodamine. In another example, the agent has the structure set forth as analog (1) in FIG. 2 , which is a rhodamine-conjugated analog of the nerve agent soman.
In another embodiment of the instant methods, the peptides are not bound to a solid support. Instead, the agent or peptide is labeled with a moiety that provides a basis for affinity purification. Such moieties are well-known in the art and include, for example, biotin and glutathione. Such purification can comprise a step of removing unreacted peptide and agent prior to affinity purification. This step may be accomplished in a number of ways using techniques that are well-known in the art, such as chemical separation based on solubility, size exclusion chromatography and gel electrophoresis.
This invention also provides a peptide which forms a phosphorus-based ester with an organophosphorus agent, which peptide comprises a nucleophilic functional group. In one embodiment of this invention, the nucleophilic functional group comprises a thiol or a hydroxyl group. In a preferred embodiment, the peptide is between six and 15 amino acids in length or has a molecular weight of less than 1500 daltons. In one embodiment, the peptide is six amino acids in length.
In the preferred embodiment of this invention, the agent with which the peptide reacts is an organophosphorus insecticide or chemical warfare agent.
This invention also provides a peptide library, wherein each peptide therein comprises a nucleophilic functional group. In one embodiment, each peptide in the library comprises a thiol or hydroxyl-containing amino acid residue, and the position at which such thiol or hydroxyl-containing amino acid residue occurs is the same for each peptide in the library. In another embodiment, each peptide is of a fixed length. In a further embodiment, the length of each peptide is between six and 15 amino acid residues and/or the molecular weight of each peptide is less than 1500 daltons. In a further embodiment, each peptide has a length of six amino acid residues. In still another embodiment, the first, second, third, fourth, fifth, or sixth amino acid residue in each hexapeptide is a serine.
This invention also provides a composition of matter comprising one of the instant peptides and a pharmaceutical carrier. This invention further provides a composition of matter comprising one of the instant peptides and a nonpharmaceutical carrier. In one embodiment, the nonpharmaceutical carrier is a foam or aerosol.
Foam formulations and mechanisms for their dispersal are well-known in the art and are particularly useful for surface decontamination. Foam formulations specifically designed for blast suppression are also known in the art and would be particularly useful in combination with the peptides of the instant invention in containing an explosive device that has been designed to disseminate a nerve agent.
This invention also provides an article of manufacture comprising one of the instant peptides affixed to a solid substrate. In one embodiment, the solid substrate is a polymer. In another embodiment, the solid substrate is a fabric or fiber. In yet another embodiment, the solid substrate is a filtration component, such as one used in a gas mask.
In the preferred embodiment, the peptides of the instant invention are incorporated into polymers using art-recognized techniques. Many different types of polymers are known in the art. The choice of polymer would depend, for example, upon whether the peptide is to be incorporated into protective clothing, a device such as a gas mask or a pellet or sheet for surface decontamination.
This invention provides a method for reducing the likelihood of injury due to exposure to an organophosphorus agent in a subject exposed to or at risk of exposure to such an agent. This method comprises administering to the subject an effective amount of a peptide of the instant invention.
This invention also provides a method for decontaminating an area exposed to an organophosphorus agent comprising introducing to the area an effective amount of a peptide of the instant invention.
This invention further provides a kit for decontaminating an area exposed to an organophosphorus agent comprising a peptide of the instant invention and instructions for use.
Finally, this invention provides a method for determining the presence of an organophosphorus agent in an area. This method comprises the steps of contacting a peptide of the instant invention with a sample taken from the area and determining whether a phosphorus-based ester is formed with the peptide. In this method, the formation of such an ester is indicative of the presence of an organophosphorus agent in the area.
This invention is illustrated in the Experimental Details section which follows. This section is set forth to aid in an understanding of the invention but is not intended to, and should not be construed to, limit in any way the invention as set forth in the claims which follow thereafter.
Experimental Details
Synopsis
The present invention provides methods and reagents for protection against poisoning by organophosphorus-based insecticides and nerve agents. In a novel approach to producing such reagents, this invention utilizes combinatorial chemistry and high-throughput screening to generate catalytic peptides for the inactivation of organophosphorus-based toxins. The peptides provided by the instant invention are selected based on their ability to autocatalytically bind and thereby inactivate substrate phosphoesters and offer several advantages over current enzyme-based approaches. These include decreased immunogenicity, and more favorable equivalent weight ratios.
Methods
Design of the Peptide Library
A combinatorial approach based on “split and pool” synthesis was used to generate a diverse population of peptides. Hexapeptide libraries were designed with five random positions and one fixed serine, giving 3.2 million unique peptides per library. Separate libraries were generated that contained a serine at each position, [x 1 , x 2 . . . x 6 ] in the peptide. Thus, a total of six libraries is produced, each having serine fixed in a different position of the hexapeptide.
Synthesis of the Peptide Libraries
Tental Gel™ was used as the solid phase support and sequences of active peptides were determined using mass spectrometry (MS). Peptide library synthesis was accomplished by a “split and pool” methodology using standard Fmoc peptide chemistry. For example, the first library, in which serine occupies the first position, x 1 , was synthesized as follows: (i) the beads were reacted with Fmoc-protected serine using benzotriazol-1-yloxytris (dimethylamino) phosphonium hexafluorophosphate (BQP) and hydroxybenzotriazole (HoBt) as coupling agents, (ii) amino groups were blocked with acetic anhydride, and (iii) the Fmoc protecting group was removed using 20% piperidine in DMF. The next five amino acids in the peptide were placed randomly using the “split and pool” method. This is accomplished by separating the entire population of beads into twenty groups of equal size. Each of the twenty amino acids is reacted with an individual group using BOP and HoBt as coupling agents. After the coupling reaction, the beads are combined so that they can be washed, blocked, and finally deprotected together. This split and pool synthesis is performed five times in order to add five random amino acids to each peptide.
Library Screening
Libraries were exposed to a fluorescently labeled nerve gas analog for 1 hr followed by 1 minute washes at room temperature in PBS containing 10% Tween 20, 10% DMF, followed by DMF containing 10% Tween 20. Butylcholinesterase coupled to native beads was used as a positive control. Library peptides which remained fully protected and thus unreactive were used as a negative control. Wash conditions were optimized to exclude noncovalent interactions between the fluorescent label and the beads utilizing either peptides in which the reactive groups were blocked by pre-incubation with either acetic anhydride or a single “non-specific” peptide not likely not to be configured for reaction.
Following incubation with analog (1) and extensive washing, beads displaying relatively high levels of fluorescence were selected and their peptides sequenced using LCMS. Peptides corresponding to those identified in the screen were synthesized using Tental Gel™ as the solid phase and standard Fmoc chemistry, then purified using high-pressure liquid chromatography (HPLC).
Synthesis of Fluorescent Sarin Analogs
Fluorescent-labeled sarin analogs were synthesized as shown in FIG. 1 . Briefly, 10-undecen-1-ol (1) was converted to an iodinated compound (3) through a tosylate intermediate (2). Reaction of (3) with excess tri-isopropylphosphite under reflux conditions afforded the di-isopropoxy phosphonate (4), which was converted to the isopropoxyhydroxy phosophonate (5) by refluxing with NaOH in methanol. The olefin (5) was oxidatively cleaved with ruthenium trichloride and sodium periodate to yield the terminal carboxylic acid (6). Treatment of (6) with excess diethylaminosulfur trifluoride (DAST), followed by N-hydroxysuccinimide (NHS), afforded the N-succinyl fluorophosphonate intermediate (8) Without further purification compound (8) was reacted with amine-functionalized rhodamine (NH 2 -rhodamine) to generate the rhodamine-labeled sarin analog (9). The structures of the compounds 2-8 and 9 (analog 1) were determined by NMR and MS. Experimental details are set forth below.
Compound (2) [1-((p-toluenesulfonyl)oxy)-10-undecene]: A solution of (1) (5 g, 0.029 mol) in pyridine (50 ml) was reacted with p-toluenesulfonyl chloride (8.2 g, 0.044 mol) at room temperature for 4 h. The reaction mixture was evaporated and the residue was dissolved in ethyl acetate. The acetate solution was washed with 1N HCl (2×30 ml) and concentrated under reduced pressure. The product (2) was purified by chromatography (SiO 2 , ethyl acetate/hexane 1/20). Colorless oil, yield 8.9 g, 94%, 1 H NMR (CDCl 3 , 300 MHz): 7.7(d, 2H), 7.32(d, 2H), 5.8(m, 1H), 5.0(m, 2H), 4.0(t, 2H), 2.4(s, 3H), 2.0(m, 2H), 1.7(m, 2H), 1.5-1.2(m, 12H); MS: found 324.18, cald. 324.18 for C 18 H 28 O 3 S.
Compound (3) [1-iodo-10-undecene]: A solution of (2) (8.0 g, 0.025 mol) in acetone (80 ml) was treated with NaI (7.0 g, 0.05 mol). The reaction mixture was refluxed for 2 h and concentrated. The residue was dissolved in ethyl acetate (50 ml) and washed with H 2 O (20 ml). The product (3) was purified by chromatography (SiO 2 , ethyl acetate/hexane 1/20). 5.5 g oil, 79%. 1 H NMR (CDCl 3 , 300 MHz): 5.8 (m, 1H), 5.0(m, 2H), 3.2(t, 2H), 2.0(m, 2H), 1.8 (m, 2H), 1.50-1.20(m, 12H). MS: found 280.07, cald. 280.07 for C 11 H 21 I.
Compound (4) [1-(di-isopropoxy) phosphinyl)-10-undecene]: A mixture of triisopropyl phosphite (10 ml, excess) and compound (3) (5.0 g) was refluxed for 15 h. Excess of triisopropyl phosphite was removed by distillation under reduced pressure. The product was purified by chromatography (SiO 2 , ethyl acetate/hexane 1/4). Oil, 5.4 g, 93%. 1 H NMR (CDCl 3 , 300 MHz) 5.70 (m, 1H), 4.9 (m, 2H), 4.80 (m, 2H, CHOP), 2.0-1.0 (m, 30H). MS: found 318.380, cald. 318.380 for C 17 H 35 O 3 P.
Compound (5) [1-(isopropylhydroxyphosphinyl)-10-undecene]: A solution of compound (4) (5.0 g, 0.016 mol) in methanol (80 ml) and aqueous NaOH (5.0 g in 15 ml H 2 O) was refluxed for 5 h. The solvents were removed by concentration under reduced pressure. The residue was dissolved in H 2 O (30 ml) and extracted with ethyl ether. The aqueous solution was acidified with 6 N HCl to pH=2, and extracted with ethyl acetate. The organic phase was evaporated to give pure compound (5) as clear oil. 3.9 g, 89%. 1 H NMR (CDCl 3 , 300 MHz) 5.70 (m, 1H), 4.9 (m, 2H), 4.80(m, 1H, CHOP), 2.0-1.0 (m, 24H)
Compound (6) [10-(iso-propylhydroxyphosphinyl) decanoic acid]: To compound (5) (−1.0 g, 3.6 mmol) dissolved in CCl 4 —CH 3 CN—H 2 O (1:1:1.5) (35 ml) was added NaIO 4 (3.1 g, 4 eq.) and ruthenium trichloride hydrate (20 mg). The reaction mixture was stirred for 2 h at room temperature and then partitioned between CH 2 Cl 2 (40 ml) and 1N HCl (20 ml). The organic layer was concentrated under reduced pressure and the resulting residue was purified by chromatography to give semisolid product (SiO 2 , ethyl acetate/methanol 1/2). 0.7 g, 70%. 1 H NMR (CDCl 3 ) 4.70 (m, 1H, CHOP), 2.3 (t. 2H), 2.0-1.0 (m, 24H). High resolution MS: found 295.166, cald. 295.166 for C 13 H 28 O 5 P.
Compound (9) [Rhodamine-labeled sarin analog (1)]: A solution of (6) (100 mg, 0.34 mmol), in CH 2 Cl 2 (3 ml) was treated at −78° C. with diethylaminosulfur trifluoride (DAST, 0.1 mL, 0.5 mmol), and the reaction mixture was stirred for 10 min. The resulting difluoride (7) was treated in situ with, N-hydroxysuucinimide (0.4 mmol) in DMF (0.2 ml) and stirred for another 5 minutes at room temperature. The reaction mixture was partitioned between ethyl acetate (15 ml) and water (10 ml), and the organic layer was washed with brine (5 ml), dried with Na 2 SO 4 and concentrated under reduced pressure to afford the N-hydroxysuccinimide (8). Without further purification, this compound was treated with amine-functionalized rhodamine derivative (1.0 eq) in DMF (2 ml) and stirred for 20 minutes. The solvents were evaporated under reduced pressure. The remaining residue was washed sequentially with diethyl ether and ethyl acetate to afford (9) as a red film. 150 mg, 49%, 1 H NMR (CDCl 3 , 300 MHz) 7.0-8.0 (m, 9H), 4.90 (m, 1H, CHOP), 2.5-1.0 (m, 46H). High resolution MS: found 793.4105, cald. 793.4400 for C 43 FH 59 N 4 O 7 P.
Synthesis of Additional Sarin Analogs
Synthesis of analog (2): Analog (2) was synthesized by fluoration of compound (5) ( FIG. 1 ), 1-(isopropylhydroxyphosphinyl)-10-undecene, with DAST in a similar manner to that of analog (1) shown in FIG. 1 and described above. The synthetic scheme of analog (2) is summarized in FIG. 3A .
Synthesis of analog (3): Analog (3) was synthesized by the route outlined in Scheme 2, FIG. 3B . The olefin (5) was oxidatively converted to an aldehyde (6) with OsO 4 and NaIO 4 . Reductive amination of (6) with dimethyl amine and sodium borohydride afforded the amine (7). Quaternazation of the tertiary amine (7) with iodomethane in DMF gave (8) which was treated with DAST to afford the analog (3).
Experimental details for analog (3): Compound (5) (0.74 g) in a solution of THF (10 ml) H 2 O (6 ml) was added to 2% OsO 4 in H 2 O (2 ml) and NaIO 4 (2.0 g, 4 eq.). The mixture was stirred at room temperature for 18 h, quenched with saturated Na 2 SO 3 (10 ml) and partitioned with ethyl acetate. Evaporation of the solvents afforded the aldehyde (6) [oil, 0.5 g. 70% by NMR]. The aldehyde (0.45 g) (6) in ethanol (50 ml) was added to dimethylamine (1.3 eq). To this solution was added NaBH 4 (1.1 eq). The reaction mixture was stirred for 4 h and the treated with 1 N HCl at 0° C. After removal of the solvents, the residue was dissolved in water and washed with ethyl ether. The aqueous layer was concentrated under reduced pressure to afford compound (7) [0.32 g, 63% by NMR]. The amine (7) (0.3 g) in DMF (10 ml) was treated with MeI (1 ml, excess) overnight. The solvent was removed under reduced pressure to give compound (8) which was converted to analog (3) in a similar manner as analog (1) [semisolid, 85% by NMR].
Synthesis of analog (4): Analog (4) was synthesized by the route outlined in scheme 3, FIG. 3C . Treatment of phenylphosphonic dichloride with excess isopropanol in the presence of triethylamine afforded the diisopropyl phenylphosphonate which was subjected to basic hydrolysis with NaOH to generate the monoester (isopropyl Phenylphosphonic acid). The nerve gas analog (4) was generated by treatment with DAST in a manner similar to analog (1).
Solution-phase Reaction of Peptides with Sarin Analogs
1 mmol of purified peptide was incubated with one of the nerve agent analogs (1.2 mmol) in PBS at room temperature for 2-3 hr. The formation of reaction product was monitored by HPLC (C 18 analytic column, gradient eluting with 100% H 2 O—−70% MeCN for 1 h) and confirmed by mass spectrophotometry.
Results and Discussion
In order to obtain catalytic peptides with the desired reactivity, libraries consisting of peptides containing a nucleophilic moiety were conceived which would react with the phosphonate moiety of organophosphorus-based agents to form a peptide phosphoester.
Initial work was done using hexapeptide libraries consisting of a serine at a fixed position [x 1 , x 2 , . . . x 6 ] and any amino acid at each of the remaining five positions. In one example, the hydroxyl moiety of serine serves as the nucleophile which reacts with the phosphonate of the agent to form a peptide-phosphoester, effectively blocking the ability of the agent to react with cellular proteins and thus neutralizing it.
Each of the six hexapeptide libraries consists of at least 3.2 million peptides comprised of a random amino acid at each of five positions and a serine at a fixed position (given by probability 20 5 =3.2×10 6 ). For example, Library 1 consists of at least 3.2 million peptides, each having a serine in position one (x 1 ) and any amino acid in each of the remaining five positions. In practice, each peptide was represented by approximately 6 copies in the library. Initially, three libraries were synthesized containing a fixed serine at either x 1 , x 2 , or x 3 , respectively.
In order to identify peptides with the desired reactivity, labeled analogs of the nerve gas sarin were synthesized. Labeled butylcholinesterase (BuChE) coupled to the same solid support as the library (in this case Tental Gel™) was used as a positive control to identify peptides with suitable reaction kinetics.
Although radiolabeled analogs are preferable because they minimize interference due to steric hinderance, such analogs of nerve agents present unacceptable hazards. Therefore, fluorescent sarin analogs were generated using each of rhodamine, fluorescein, cascade blue, dansyl cadaerine and disperse red as labels. Preliminary experiments using native beads as negative controls demonstrated that rhodamine-conjugated sarin analog (1) produced the optimal signal to noise ratio.
Library screening was performed with analog (1) and fluorescent beads were selected. Initially, beads demonstrating the highest fluorescence intensity were manually selected under the microscope. However, this technique could easily be optimized for selection using high-throughput methods such as flow cytometry (for libraries coupled to beads), plate readers (for libraries adsorbed onto microtiter plates) or microarray scanners (for libraries on microchips).
23 of the manually selected fluorescent beads were chosen for sequencing and a further subset of ten of the resulting peptides was chosen for resynthesis and further study. These ten peptides had the following sequence: YKDNSY (SEQ ID NO:1), YKDISY (SEQ ID NO:2), DNFKSY (SEQ ID NO:3), ANKYSY (SEQ ID NO:4), YYCDSY (SEQ ID NO:5), YHYYSY (SEQ ID NO:6), ANYYSY (SEQ ID NO:7), YEYQSY (SEQ ID NO:8), LIFASY (SEQ ID NO:9), YKEFSY (SEQ ID NO:10), and CAYCSY (SEQ ID NO:11)
Purified peptides identified in the initial screen were further tested for reactivity against sarin analog (2), which lacked the fluorescent tag. Using HPLC to monitor the reaction, one peptide was found to react with analog (2), demonstrated by the loss of its characteristic peak and the emergence of three new chromatographic peaks. YKDNSY disappeared at retention time 17 min, and the 3 new peaks appeared at 23, 25 and 29 min. 1 H NMR analysis demonstrated that the peaks at 4.9 ppm (H for Me 2 CHP(O)F) shifted to 4.5 ppm (H for Me 2 CHP(O)O), indicating formation of a phosphoester with the sarin analog. Diastereomers likely account for two of the products.
REFERENCES
Cheng, T. C. et al., Cloning and expression of a gene encoding a bacterial enzyme for decontamination of organophosphorus nerve agents and nucleotide sequence of the enzyme. Appl. Env. Microbiol. 62, 1636-1641 (1996)
Doctor, B. P., Richard K., et al., Immobilized enzymes: Nerve agent detoxifiers. Proceedings of the ERDEC Scientific Conference on Chemical and Biological Defense Research, Aberdeen Proving Ground, MD, United States , Nov. 17-20, 1998, p. 559-566 (1999).
Gill, I., and Ballesteros, A., Degradation of organophosphorous nerve agents by enzyme-polymer nanocomposites: efficient biocatalytic materials for personal protection and large-scale detoxification. Biotech. Bioeng. 70(4), 400-410 (2000).
LeJeune, K. E., Wild, J. R., Russell, A. J., Nerve agents degraded by enzymic foams. Nature 395(6697), 27-28 (1998).
Lejeune, K. E., Dravis, B. C., Yang, F., Retro, A. D., Doctor, B. P., Russell, A. J., Fighting nerve agent chemical weapons with enzyme technology. Ann. N.Y. Acad. Sci. 864, 153-170 (1998).
Lejeune, K. E. and Russell, A. J., Biocatalytic nerve agent detoxification in fire fighting foams. Biotechnol. Bioeng. 62(6), 659-665 (1999). | This invention provides methods and peptides for the inactivation of organophosphorus-based insecticides and chemical warfare agents. The instant methods include peptide screening methods, peptides and peptide libraries, related compositions of matter, articles of manufacture, and methods for prophylaxis, treatment, decontamination and detection. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation of international patent application PCT/EP2004/014605 filed on Dec. 22, 2004 and published in German language as WO 2005/064273 A1, which international patent application claims priority from German patent application DE 103 61 870.8 filed on Dec. 29, 2003.
BACKGROUND OF THE INVENTION
The invention relates to a laser scanner and a method for optically scanning and measuring an environment. More particularly, the invention relates to laser scanners used to scan and measure a variety of interior and exterior spaces. For instance, these may be manufacturing buildings in which specific facilities are planned. In this case, the laser scanner is placed on a stand into the space to be measured, and the measuring head is slowly rotated about a vertical axis, while a rotor—arranged in the measuring head—with a light transmitter rotates at a significantly higher rotational speed about a horizontal axis. In this way, the fast rotation results in a light fan being generated in a vertical plane, said light fan being slowly rotated through e.g. 360°, so that finally the entire environment has been scanned. The emitted light beams are reflected from the points in the environment, and the reflected light beam is received by the measuring head again. In this case, both the distance of the respectively measured point in the environment and the reflectivity of said point are determined, so that finally a faithful imaging with a solid angle of ideally 360° arises.
In another application of such scanners, elongated cavities, such as tunnels, are measured. In this case, the light transmitter rotates about a horizontal axis and it is moved along the tunnel to be measured. In this way, it is possible to monitor the state of tunnels, to determine the clearance at any point in the tunnel, etc.
Laser scanners of the abovementioned type are usually specified for a specific distance range. This means that objects can be detected and measured at greater or lesser distance depending on the class of the components used. Typically, the intensity of the reflected light beam depends on the distance of the measurement point and its reflectivity. The intensity of the reflected light beam results in a certain gray-scale value provided by the receiver.
In applications of laser scanners for a large distance range, where objects situated at a large distance are still to be reliably identified and measured, and in applications with a large gray-scale value range, where measurement points having a relatively poor reflectivity are to be reliably differentiated, the receiver's dynamic range limits are soon encountered. It must be taken into account that the intensity of the reflected light beam decreases more than proportionally with the distance. Thus, the quantity of light that is reflected from an object at a distance of 50 m amounts to only approximately 4×10 −6 of the quantity of light that is reflected from an object at a distance of 0.1 m. The range of different gray-scale values is an additional factor. According to the current prior art there are no receivers available which cover such a wide dynamic range.
DE 22 16 765 C3 discloses a method and a device for distance measurement. This involves determining first of all the distance to a specific measurement point and optionally also the reflectivity of the measurement point. The distance is determined from a propagation time measurement between an emitted light pulse and the light pulse reflected from the measurement point. Errors can occur if the propagation time measurement is ended and the received signal, i.e. a signal pulse generated from the reflected light pulse, reaches a specific trigger level but this signal pulse has an undefined maximum amplitude. In order to preclude this error, a regulation is performed which brings about an adjustment in such a way that the signal pulse is raised from a lower initial value until it has reached a defined level. The regulation works by adjusting either the transmission power or the reception gain prior to the generation of the signal pulse. The reflectivity is determined by detecting the amplitude of the signal pulse before being raised to the defined level and comparing it with a predetermined transmission power. In this case, furthermore, from the measured distance, a weighting is additionally carried out in order to calculate out the dependence of the amplitude of the reflected light pulse on the distance of the measurement point.
The known device and the known method are thus limited for measurements at a single measurement point, because the measurement point has to be intrinsically optimized in each case by adjusting the transmission power and/or the reception gain. This precludes scanning 2D or 3D measurements of an environment.
Furthermore, the reflectivity of the measurement point can be determined only when the absolute transmission power in the system that has not yet been adjusted is known. The inclusion of the distance finally determined and the weighting of the reflection value with this distance lead, finally, to an absolute value of the reflectivity at the location of the measurement point, but not to the gray-scale value received at the location of the measuring apparatus. This is because said gray-scale value is independent of distance. Specifically, in the case where an environment is represented in the manner of a photograph, each point has, for an observer, a gray-scale value that says nothing about how far away the point is from the observer. Therefore, image recordings of an environment cannot be produced by means of the known procedure.
SUMMARY OF THE INVENTION
In view of the above, it is an object of the invention to provide a laser scanner and method that allow measurements over a wide distance range and a wide gray-scale value range.
According to one aspect of the invention, this object is achieved by a laser scanner for optically scanning and measuring an environment, comprising a light transmitter for emitting a transmitter light beam to a measurement point in the environment, and a receiver for receiving a reflected light beam reflected from said measurement point, said receiver being configured to provide a grey-scale value representative of the measurement point, wherein the reflected light beam has an intensity, wherein the light transmitter has a predetermined transmission power which is adjustable as a function of the intensity, and wherein the receiver is configured to provide the gray-scale value as a function of the adjusted transmission power.
According to another aspect, this object is achieved by a method of optically scanning and measuring an environment, comprising the steps of: emitting a transmission light beam from a light transmitter to a measurement point in the environment, the light transmitter having a adjustable transmission power, receiving a reflected light beam reflected from said measurement point, the reflected light beam having an intensity, and determining a grey-scale value representative of the measurement point, wherein the transmission power of the light transmitter is adjusted as a function of the intensity, and wherein the gray-scale value is determined as a function of the adjusted transmission power.
The new scanner and method allow for a generally reduced transmission power and a high-quality reproduction of the environment of the laser scanner in a half tone representation. For varying distances and/or varying reflectivity of the measurement points, imaging errors are avoided by the transmission power being increased or reduced. Since the transmission power is taken into account in the formation of the gray-scale value, the measurement error systematically generated by the adjustment of the transmission power is precisely “calculated out” again, so that an unaltered faithful image of the environment is generated as a halftone representation.
For measurement points that are further away and/or weakly reflective, the transmission power is increased in order that the reflected signal still has a sufficient magnitude so as not to overtax the dynamic range of the receiver. Conversely, the transmission power can also be reduced in the case of very close and/or strongly reflective measurement points. This contrivance therefore makes possible, in a relatively simple manner, a reliable measurement even with large distance and/or gray-scale value ranges, without an excessive outlay having to be implemented for the receiver or actually overtaxing the possibilities of commercially available receivers. Furthermore, by limiting the transmission power, a lower energy consumption is made possible and persons in the vicinity of the scanner are reliably protected against injury, in particular eye injury.
In a preferred refinement of the invention, the transmission power is adjustable in such a way that the intensity of the reflected light beam is kept at least approximately constant.
This measure has the advantage that even receivers having a very small dynamic range and therefore having very low costs can be used.
In a exemplary embodiment of the invention, an adjustable power supply unit is assigned to the light source, the receiver being connected to the power supply unit via a first characteristic curve stage.
This measure has the advantage that, using simple circuitry means, it becomes possible to set the transmission power for a varying intensity of the reflected measurement beam, in which case the characteristic curve of the characteristic curve stage can be assigned in a manner dependent on the physical conditions such that the function of the intensity or the power of the emitted light beam against the intensity of the reflected measurement beam becomes substantially linear, if not even at least approximately constant.
In another embodiment, the receiver includes an adjustable amplifier, the control input of which is connected to the power supply unit via a second characteristic curve stage.
This allows a practical implementation with simple circuitry. The second characteristic curve stage makes possible a complete compensation of the adjustment of the transmission power as a function of the intensity of the reflected light beam.
Further advantages will be understood from the following description and the accompanying drawing. It goes without saying that the features mentioned above and those yet to be explained below can be used not only in the combination respectively specified, but also in other combinations or on their own, without departing from the scope of the present invention.
BRIEF DESCRIPTION OF THE FIGURES
An exemplary embodiment of the invention is illustrated in the drawing and is explained in more detail in the description below. In the figures:
FIG. 1 shows an extremely schematic perspective illustration of a use of a device according to the invention in practice;
FIG. 2 shows a schematic block diagram of an exemplary embodiment of a device according to the invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
In FIG. 1 , reference numeral 10 designates a laser scanner for the optical scanning and measurement of an environment of the laser scanner 10 . In an exemplary embodiment illustrated in FIG. 1 , an image of the environment with a solid angle of ideally 360° is intended to be generated from a static point.
For this purpose, the laser scanner 10 contains a measuring head 12 situated on a spatially fixed stand 14 . In this case, the measuring head 12 is rotatable as a whole relatively slowly about a vertical axis 16 , as indicated by an arrow 18 .
The measuring head 12 contains, for its part, a rotor 20 , which is rotatable significantly faster, that is to say at a significantly higher rotation speed, about a horizontal axis 22 , as indicated by an arrow 24 .
The rotor 20 emits a light beam 26 . In FIG. 1 , the beam emitted by the rotor 20 is designated by Ls, while a beam reflected from an object 30 in the environment is indicated by Lr.
In the situation illustrated in FIG. 1 , an object 30 is situated at a distance d from the measuring head 12 , on which object a measurement point 32 is currently being illuminated by the light beam 26 . Let the measurement point 32 have a gray-scale value GW.
FIG. 2 shows a circuit arrangement 40 arranged within the measuring head 12 .
The circuit arrangement 40 contains a light source 42 that rotates with the rotor 20 , for example a laser diode, which emits the light beam Ls with the transmission power Ps. The light source 42 is fed with a supply voltage U V by an adjustable power supply unit 44 . The transmission power Ps of the light source 42 can be set in this way.
The power supply unit 44 has connected to it, for the purpose of influencing the transmission power Ps, on the one hand a modulation oscillator 46 with a modulation voltage U Mod and on the other hand a first characteristic curve stage 48 with an output regulation voltage U R , the function of which will be explained below.
On the input side, the circuit arrangement 40 contains a receiver indicated by 50 , which receives the reflected light beam Lr with the intensity Ir. The receiver 50 is preferably situated in direct proximity to the light source 42 , because the emitted beam Ls is likewise in direct proximity to the reflected beam Lr or may even coincide with the latter. In the last-mentioned case, a semitransparent mirror or the like may be used for separating the beams Ls and Lr. These problems are known to the person skilled in the art of laser scanners and therefore need not be explained any further here.
The receiver 50 supplies at its output a signal which corresponds to an apparent gray-scale value GWs. On the output side, the receiver 50 is connected to an adjustable amplifier 52 . The amplifier 52 has an output terminal 54 , at which a signal corresponding to a genuine gray-scale value GWe can be tapped off.
The gain factor of the adjustable amplifier 52 is controlled by means of a second characteristic curve stage 56 , which is connected on the input side e.g. to the output of the first characteristic curve stage 48 . In this case, it is important that a signal reproducing the transmission power Ps is applied to the second characteristic curve stage 56 on the input side. In the exemplary embodiment this may be the output signal of the first characteristic curve stage 48 , but need not be said signal.
The circuit arrangement 40 operates as follows: By means of the modulation oscillator 46 , the amplitude of the emitted beam Ls, that is to say the transmission power Ps, is modulated with the modulation voltage U Mod in a manner known per se. This modulation signal then also appears in the reflected beam Lr and is evaluated as distance signal by means of the receiver 50 (not illustrated).
The output signal of the receiver 50 is a measure of the intensity Ir of the reflected light beam Lr. This signal is fed to the first characteristic curve stage 48 , which has a degressive profile. The degressive profile takes account of the change in the intensity I r depending on the distance d and on the gray-scale value GW. At the output of the first characteristic curve stage 48 , therefore, a regulation voltage U R is present which is all the higher, the smaller the intensity Ir becomes on account of a larger distance d or a larger gray-scale value GW. The regulation voltage U R influences the power supply unit 44 , so that the supply voltage U V increases in inverse dependence on the intensity Ir, to be precise preferably more than proportionally or exponentially. As a result, the transmission power Ps also increases, with the consequence that the intensity I r of the reflected beam Lr decreases to a much lesser extent as the distance d or gray-scale value GW increases than would be case without the regulation described. In the extreme case, it remains at least approximately constant. For this purpose, a desired value predefinition may additionally be added to the circuit 42 , 44 , 48 , 50 described (not illustrated).
This measure has no influence on the evaluation of the distance d, because the distance d is obtained by the modulation, that is to say by the phase shift between the modulation voltage U Mod and the modulated component of the reflected beam Lr.
The adjustment of the transmission power Ps in a manner dependent on the intensity Ir of the reflected light beam Lr leads to a systematic corruption of the gray-scale value signal, because the latter is directly dependent on the intensity I r of the reflected beam Lr. This is the reason while the output signal of the receiver 50 was referred to as an “apparent” gray-scale value GWs.
In order to correct these systematic corruptions again, a correction signal is formed from the output signal U R of the first characteristic curve stage 48 or some other signal which reproduces the transmission power Ps, by means of the second characteristic curve stage 56 , which correction signal adjusts the adjustable amplifier 52 in order to bring abut the correction mentioned. The “genuine” gray-scale value GWe thus appears at the output terminal 54 of said amplifier.
In this case, the characteristic curve of the second characteristic curve stage 56 is likewise degressive, because owing to the adjustment of the transmission power Ps for large distances d and high gray-scale values GW, the measured intensity I r is greater than it would be if the transmission power Ps was not adjusted in a manner dependent on the transmission power Ps. | A laser scanner for optically scanning and measuring an environment comprises a light transmitter having a predetermined transmission power for emitting a light beam. The emitted light beam is reflected at a measurement point in the environment. The reflected light beam is received with a certain intensity by a receiver. The transmission power is adjustable as a function of the intensity of the reflected light beam. Furthermore, a gray-scale value of the measurement point is determined as a function of the transmission power adjusted. | 6 |
TECHNICAL FIELD
The present invention relates to paclitaxel analogues and derivatives for use in applications in place of paclitaxel.
BACKGROUND ART
Paclitaxel (taxol), as it is already well-known, is a diterpenoid extracted from plants of the Taxus genus having anticancerogenic activity on different forms of human tumours. Its clinical use still involves some drawbacks due to the poor water solubility, which makes its administration complex, as well as to the onset of serious side-effects. Moreover, paclitaxel induces resistance quickly. Due to these reasons, research has been conducted for some years in attempts at synthesizing novel paclitaxel analogues which cause less adverse effects compared with the parent molecule.
SUMMARY OF THE INVENTION
The present invention relates to novel derivatives taxane skeleton endowed with a marked anti-tumoral activity. The novel derivatives have the general structure 1: ##STR1## wherein R 1 , and R 2 are hydrogen atoms, or R 1 is an hydrogen atom and R2 is an hydroxyl or an acetyloxy group, having izos carbonatoms or OR 1 and R 2 together form a cyclic carbonate group of formula: ##STR2## R 3 , which can be α- o β-oriented, is an hydrogen atom or an alkylsilyl group having 1 to 12 carbon atoms in the alkyl moiety which can be straight chain or branched. R 3 is preferably triethylsilyl (TES); R 4 is hydrogen, or the residue ##STR3## or an isoserine residue of formula A: ##STR4## wherein R 1 ' is a straight or branched alkyl or alkenyl group, containing one to five carbon atoms, or an aryl residue; R 2 ' is a straight or branched alkyl or alkenyl group, containing one to five carbon atoms, or an aryl residue, or a tert-butoxy group.
DETAILED DESCRIPTION OF THE INVENTION
The novel derivatives of general formula (1) are prepared by semisynthesis, starting from the natural syntons 10-deacetylbaccatine III (2) and 10-deacetyl14β-hydroxybaccatine III(3). For this purpose, they are selectively oxidized in position 10 and then esterified in position 13 with a suitable acylating agent which allows to introduce the group R 4 . ##STR5##
When taxanes of natural or synthetic origin already containing the desired isoserine chain in position 13, the molecules of structure 1 can be obtained from said taxanes by selective oxidation in position 10. As it will be described hereinafter, the selective oxidation in position 10 of 2, 3 and of the taxanes already containing the isoserine chain in position 13, can be obtained by treatment with copper (II) salts. 10-Deacetylbaccatine III (2) and its 14β-hydroxy (3) analogous can be recovered from suitably selected vegetable material (see. Indena U.S. Pat. No. 5,264,591). However, and it is one of the objects of the present invention, it is possible to synthesize taxane syntons containing an oxygenated function in position 14, which are therefore useful for the preparation of compounds of structure 1, containing an oxygenated function in position 14, starting from 10-deacetylbaccatine III (2). In fact, it has surprisingly been found that, after protecting the hydroxyl in position 7 of compound 2 as a silyl ether, the oxidation to ketone of the carbon in 13 and the introduction of a β-oriented alcohol function on the carbon in 14 take place by treatment with manganese dioxide. After protection of the hydroxyls in 10 and 14, for example as acetates, by treatment with hydrides, the 13-keto function is reduced to 13α-hydroxy.
The process, which is schematized below, leads to the formation of synthon 4, useful for the preparation of compounds with structure 1. ##STR6##
From synthon 4, after removing the protective groups with known methods described in literature, for example using hydrochloric acid to remove the silyl group and a base to remove the acetate groups, 10deacetyl-14β-hydroxybaccatine III (3) is obtained. Therefore, as mentioned, in order to prepare compounds of formula 1, 10-deacetylbaccatine III (2), 10deacetyl-14β-hydroxybaccatine III (3), natural or semisynthetic, or other taxanes having an hydroxyl function at 10 and already containing in position 13 the isoserine chain represented by the group R 4 must be available.
It has surprisingly been found that all these synthons, by treatment with copper (II) salts, preferably copper acetate, undergo a selective oxidation in position 10, without need for the protection of the other hydroxyl functions. For example, 10-deacetylbaccatine III (2), 10-deacetyl-14β-hydroxybaccatine III (3) and the natural taxane 10deacetyl-cephalomannine give the respective 10-keto derivatives 5-7 in yields from 75 to 85%. The oxidation generally requires protracted times (100-140 hours) and an excess of oxidizer and it is carried out at room temperature and in alcoholic solvent. ##STR7##
When, preparing the compound of formula 1 with, the presence of a cyclic carbonate group between the positions 1 and 14, synthon 3 is previously treated with phosgene in pyridine and the resulting carbonate is then oxidized in position 10 with copper (II) acetate, to give carbonate synton 8.
By treatment with bases, diketones 5-8 undergo an inversion in position 7, i.e. the hydroxyl in position 7 becomes α-oriented. Syntons 5, 6 and 8 or optionally their epimers in position 7, are therefore used for the preparation of taxanes of structure 1, after protection of the alcoholic functions present. The alcohol function in 13, contrary to the other hydroxyalcohol functions, is poorly reactive to silylation and therefore does not undergo derivatization.
For the esterification in position 13, the suitably activated isoserine chains are used, according to what reported in literature for the semisynthesis of paclitaxel and of its analogues (see. for example Eur. Pat. Appl. 400971, 1992; Fr. Dem. 86, 10400; E. Didier et al., Tetrahedron letters 35, 2349, 1994; E. Didier et al.; ibid 35, 3063, 1994). Preferably, isoserin chains are used in the activated forms of oxazolidinecarboxylic acids 9 a and 9 b. ##STR8##
In formulae 9a and 9b, R 1 'and R 2 'have the meaning described above. The esterification of the oxazolidinecarboxylic acids with the taxane syntons and the subsequent elimination of the protective groups are carried out as described in literature for the synthesis of paclitaxel and the analogues thereof.
Among the compounds of formula 1, compounds 10, 11 and 12 turned out to be particularly active. Compound 10 is 13- (2R,3S)-3-ter-butoxycarbonylamino-2-hydroxy3-isobutyl-propanoyl!-10-deacetyl-10-dehydro-baccatine III. Therefore, referring to general formula 1, compound 10 has: R 1 -R 2 =H, OR 3 -β-OH, R 1 '-iso-But, R 2 '=t-BuO. Compound 11 is 13= (2R,3S)-3-ter-butoxycarbonylamino-2-hydroxy-3-isobutyl-propanoyl!-10-dehydro-10-deacetyl-14β-hydroxy-baccatine III 1,14-carbonate. Therefore 11, referring to general formula 1, has R 1 , R 2 =--CO--O, OR 3 =β-OH, R 1 '=iso-But, R 2 '=t-BuO.
Compound 12 is 13- (2R,3S)-3-caproylamino-2-hydroxy-3-isobutyl-propanoyl!-10-dehydro-10-deacetyl 14β-hydroxy-baccatine III 1,14-carbonate. Therefore 12, referring to general formula 1, has R 1 , R 2 =--CO--O, OR 3 --B-OH, R 1 '=iso-But, R 2 '=C 5 H 1 . ##STR9##
The cytotoxicity data of the compounds 10 and 11 compared with those of paclitaxel are reported in Table 1.
TABLE 1______________________________________IC.sub.50 s of compounds 10, 11and paclitaxel on 6 humantumour cell lines. Exposition IC.sub.50 (nM)Cell line time (h) Paclitaxel 10 11______________________________________L1210 (murine 48 7.0 ± 3.0 0.6 ± 0.1 2.0 ± 0.1leukemia)A121 (human ovarian) 72 3.7 ± 0.3 0.8 ± 0.3 1.6 ± 0.2A549 (human NSCLC) 72 5.4 ± 0.5 1.9 ± 0.3 2.1 ± 0.3HT-29 (human colon) 72 6.0 ± 0.6 0.4 ± 0.1 0.6 ± 0.4MCF7 (human breast) 72 4.3 ± 0.1 1.2 ± 0.2 0.8 ± 0.2MCF7-ADR (resistant) 72 395 ± 8.7 13 ± 2.2 28 ± 6.2______________________________________ Standard conditions: basal medium RPMI 1640 + 20 mM HEPES + 2 mM LGlutamine.
Compounds of formula 1 show surprising advantages compared with paclitaxel on cell lines resistant to other anti-tumoral substances, such as adriamycin or cis-platinum. The differences between paclitaxel and these products are even more evident in in vivo models, such as athymic nude mouse with human tumor implant. Moreover, it has been found that the compounds of the invention in which R' 2 is an alkyl or alkenyl group are surprisingly devoid of cardiotoxic activity, contrary to taxol and the known derivatives thereof, and therefore they can advantageously be used in the treatment of tumors in cardiopathic patients who cannot be treated with taxol and its known derivatives. The products object of the invention can be incorporated in suitable pharmaceutical formulations for the administration of the products both parenterally and orally. For the intravenous administration, mixtures of Chremoform L and ethanol, polysorbates or liposomial preparations prepared with natural or synthetic phosphatidylcholine or mixtures of natural phospholipids in the presence of cholesterol are mainly used.
THE EXAMPLES FOLLOWING EXAMPLES FURTHER ILLUSTRATE THE INVENTION.
Example 1
Preparation of 10-deacetyl-10dehydrobaccatine III (5). 10 g of 10-deacetylbaccatine III (2), (isolated as described by G. Chauviere et al., C. R. Acad. Sci. Ser. II 293. 591. 1981) are suspended in 350 ml of methanol and mixed with 65 g of Cu(OAc) 2 . The suspension is stirred at room temperature for 120 h. The salts are filtered off and the solution is chromatographed on 100 g of silica gel eluting with a hexane/ethyl acetate 6:4 mixture. Upon crystallization from ligroin, 9.5 g of (5) are obtained, M+a m/z 542.
Example 2
Preparation of 10-deacetyl-10-dehydro-14βhydroxybaccatine III 1,14-carbonate (8). 10 g of 10-deacetyl-143-hydroxybaccatine III (3), isolated as described by G. Appendino et al., J. Chem. Soc. Perkin Trans I, 2925. 1992, are dissolved in 50 ml of anhydrous pyridine and treated for one hour with 1.5 eq. of 5% phosgene in toluene at -10° C. The reaction mixture is poured onto ice and the aqueous suspension is extracted with ethyl acetate, washing thoroughly the organic phase with diluted HC1. After drying over Na 2 SO 4 the organic phase is concentrated to dryness. 9 g of 1,14-carbonate are obtained, which are suspended in 350 ml of methanol and treated with 50 g of Cu(OAc) 2 under stirring at room temperature for 120 h. The suspension is filtered and the solution is evaporated to dryness. The residue is chromatographed on 100 g of silica gel eluting with a hexane/ethyl acetate 1:1 mixture. 8 g of (8) are obtained, M +a m/z 584.
Example 3
Preparation of 13- (2R,3S)-3-ter-butoxycarbonylamino-2-hydroxy-3-isobutyl-propanoyl!10deacetyl-10-dehydrobaccatine III (10)
A solution of 300 mg (1.84 mmol) of 7-0triethylsilyl-10-deacetyl-10-dehydrobaccatine, III, obtained from compound (5) (Example 1) by silylatio in position 7 according to the method described by J. Denis et al., J. Am. Chem. Soc Vol.100 page 5917, 1988 in 60 ml of toluene is mixed with 500 mg of (4S, 5R)-N-(ter-butoxycarbonyl)-2.2-dimethyl-4-isobutyl-5-oxazolidineecar boxylic acid, 240 mg of dicyclohexylcarbodiimide (1.2 eq.) and 24 mg of N,N-dimethylaminopyridine (0.2 eq). The reaction mixture is kept at 80° C. for 2 hours, then is filtered and washed with water; the organic phase is concentrated to dryness. The residue is treated with methanol containing 0.1% of H 2 SO 4 at 10° C. The methanol solution is diluted with water and the product is extracted with ethyl acetate; the organic phase is concentrated to dryness and the residue is chromatographed on silica gel eluting with acetone/hexane 4:6. 350 mg of (10) are obtained. M +a m/z 785.
Example 4
Preparation of 13- (2R,3S)-3-tertbutoxycarbonyl-amino-2-hydroxy-3-isobutyl-propanoyl!10deacetyl-10-dehydro-143-hydroxybaccatine III 1,14carbonate (11).
0.5 g of 7-o-triethylsilyl-10-deacetyl-10-dehydro-14β-hydroxybaccatine III 1,14-carbonate, obtained from compound (8) (Example 2) by silylation in position 7 according to what reported by J. Denis et al., J. Am. Soc. 100. 5917. 1988. are dissolved in 60 ml of toluene. The solution is mixed with 800 mg of (4S,5R)N-(tert-butoxycarbonyl)-2.2-dimethyl-4-isobutyl-5- oxazolidinee-carboxylic acid, 400 mg of cyclohexylcarbodiimide and 40 mg of N,N-dimethylaminopyridine. The reaction mixture is kept at 80°0 C. for two hours, then is filtered and washed with water and the organic phase is concentrated to dryness. The residue is treated with methanol containing 0.1% of H 2 SO 4 at 10° C. The methanol solution is diluted with water and the product is extracted with ethyl acetate; the organic phase is concentrated to dryness and the residue is chromatographed on silica gel, eluting with acetone/hexane 4:6. 580 mg of (11) are obtained, M + a m/z 827.
Example 5
Preparation of 10-deacetyl-10-dehydro-14β-hydroxybaccatine III (6).
10 g of 10-deacetyl-14β-hydroxybaccatine III (3) are suspended in 350 ml of methanol and mixed with 65 g of Cu(OAc) 2 . The suspension is kept under stirring at room temperature for 120 h. The salts are filtered off, the solution is evaporated to dryness and the residue is chromatographed on 100 g of silica gel eluting with a hexane/ethyl acetate 6:4 mixture. Upon crystallization from ligroin, 9.3 g of (6) are obtained, M + a m/z 558.
Example 6
Preparation of 10-deacetyl-10-dehydrocephalomannine (7).
0.4 g of 10-deacetylcephalomannine (J. L. Laughlin et al., J. Nat. Prod. 44. 312. 1981) are dissolved in 5 ml of MeOH and mixed with 600 mg of Cu(OAc) 2 . The reaction mixture is left under stirring for 54 hours at room temperature. After eliminazione of the salts for filtration, the solution The salts are filtered off, the solution is evaporated to dryness and chromatographed on silica gel (10 g) using a hexane-acetate d'ethyl 1:1 mixture as eluent. 220 mg of (7) are obtained, M + a m/z 829.
Example 7
Preparation of 7-triethylsilyl-14βhydroxybaccatine III (4)
500 mg of 7-triethylsilyl-10-deacetylbaccatine III, prepared according to the method by J. Denis et al., J. Am. Chem. Soc. Vol. 100 page 5917, 1988 are dissolved in 15 ml of a ethyl acetate-methylene chloride 9:1 mixture. The solution is mixed with 10 g of MnO 2 leaving the suspension at room temperature under stirring for 24 hours. After filtration, the solution is evaporated to dryness and the residue is chromatographed on silica gel (20 g) eluting with a hexane-ethyl acetate 8:2 mixture. 310 mg of 7triethylsilyl-10-deacetyl-13-dehydro-14βhydroxybaccatine III are obtained (M + a m/z 672).
300 mg of this product are dissolved in 2 ml of pyridine. The solution is mixed with 910 mg of Ac 2 O. After 16 hours the reaction mixture is poured onto ice and then extracted with ethyl acetate. The organic phase is washed with diluted HCl and then with water to neutrality. After evaporation of the solvent, the residue is crystallized from ether (220 mg, M + a m/z 756). The solid is dissolved in 10 ml of anhydrous THF; the solution is added with 160 μl of sodium bis(2methoxy-ethoxy)aluminum hydride (65% solution). After about 10 minutes, 10 ml of a NH 4 Cl saturated solution are added, extracting then with ethyl acetate. The organic phase is evaporated to dryness. The residue is purified on silica gel (15 g) eluting with a hexaneethyl acetate 7:3 mixture. 80 mg of (4) are obtained, M + a 716.
Example 8
Preparation of (4S,5R)-N-caproyl-2-(2.4dimethoxyphenyl)-4-isobutyl-5-oxazolidinee carboxylic acid methyl ester.
5 g of N-caproyl-β-isobutyl-isoserine methyl ester are dissolved in 200 ml of a mixture of anhydrous THF and benzene and the solution is treated with 2 equivalents of 2.4-dimethoxy benzaldehyde dimethyl acetal in the presence of 120 mg of pyridinium ptoluenesulfonate. The solution is refluxed for 1 hour. The solvent is distilled and the residue is chromatographed on silica gel eluting the main compound with a ethyl acetate/hexane 8:2 mixture. After removing under vacuum the solvent from the fraction containing the desidered isomer, the residue is crystallized from hexane/isopropyl ether. 2.5 g of a compound having m.p. 98° C. are obtained.
Example 9
Preparation of (4S,5R)-N-caproyl-2-(2.4dimethoxyphenyl)-4-isobutyl-5 oxazolidine carboxylic acid
2 g of the compound of Example 8 are suspended in 50 ml of a mixture of methanol aqueous (8:2) containing 5 g of K 2 CO 3 . The reaction mixture is left under stirring until complete dissolution of the isoserine derivative. The reaction mixture is carefully acidified to pH 5. with stirring, in the presence of ethyl acetate. The aqueous phase is discarded, whereas the organic one is dried over sodium sulfate and concentrated to dryness at low temperature under vacuum. The residue is dissolved in a toluene/methylene chloride mixture and it is ready for the reaction with the selected taxanes.
Example 10
Preparation of 13- (2R,3S)-3-caproylamino2-hydroxy-3-isobutyl-propanoyl!-10-dehydro-10-deacetyl 14β-hydroxy-baccatine III 1,14-carbonate (12) 5 g of 1,14-carbonate-7-TES-10-dehydro-baccatine III are dissolved in 100 ml of a mixture of toluene and methylene chloride in a 8.2 ratio, together with 6 g of (4S,5R)-N-caproyl-2-(2.4-dimethoxyphenyl)-4-isobutyl-5oxazolidine carboxylic acid. The reaction mixture is added with 500 mg of 4-dimethylaminopyridine and 2.5 g of 1.3-dicyclohexylcarbodiimide, then heated for 2 hours under mild reflux until the reagents disappear. The compounds insoluble in the medium are filtered off and the solution is concentrated to dryness. The residue is taken up with 50 ml of methanol/HCl (0.01%) and the reaction mixture is left at room temperature for 1 hour. The solution is alkalinized to pH 5 and concentrated to dryness in the vacuum. The residue is chromatographed on a silica gel column eluting with a methylene chloride/methanol 98:2 mixture. Upon crystallization from ethyl acetate, 1.2 g of compound (12) are obtained.
Example 11
Solution of compound (10) for parenteral administration
______________________________________Compound 10 2 mgCremophor EL 175 mgAbsolute alcohol q.s. to 0.4 ml.______________________________________
Example 12
Solution of compound (11) for parenteral administration
______________________________________Compound 11 2 mgCremophor EL 175 mgAbsolute alcohol q.s. to 0.4 ml.______________________________________
Example 13
Tablets containing compound (10)
______________________________________Compound 10 10 mgCross-linked sodium carboxymethyl cellulose 15 mgLactose (spray dried) 41.5 mgMicrocrystalline cellulose 40 mgColloidal silicon dioxide 0.5 mgMagnesium stearate 1 mg.______________________________________
Example 14
Tablets containing compound (11)
______________________________________Compound 11 10 mgCross-linked sodium carboxymethyl cellulose 15 mgLactose (spray dried) 41.5 mgMicrocrystalline cellulose 40 mgColloidal silicon dioxide 0.5 mgMagnesium stearate 1 mg.______________________________________
Example 15
Capsules containing compound (10)
______________________________________Compound 10 10 mgLactose (spray dried) 30 mgMicrocystalline cellulose 48.5 mgPre-gelatinized starch 10 mgMagnesium stearate 1 mgColloidal silicon dioxide 0.5 mg.______________________________________
Example 16
Capsules containing compound (11)
______________________________________Compound 11 10 mgLactose (spray dried) 30 mgMicrocrystalline cellulose 48.5 mgPre-gelatinized starch 10 mgMagnesium stearate 1 mgColloidal silicon dioxide 0.5 mg.______________________________________ | The present invention relates to novel derivatives of 10-deacetylbaccatine III and of 10-deacetyl-14 β-hydroxybaccatine III, having cytoxic and anti-tumoral activity. They are prepared starting from the so-called syntons or from other taxanes of natural origin, by selective oxidation of the hydroxyl in position 10 to keto function and subsequent esterification in position 13, if necessary, with isoserine chains variously substituted. The products of the invention can be administered by injection or orally, when suitably formulated. | 2 |
CROSS REFERENCE TO RELATED APPLICATION
This application claims priority of the European application No. 04028484.6 EP filed Dec. 01, 2004, which is incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
The invention relates to a process for coating a component in accordance with the preamble of the claims.
BACKGROUND OF THE INVENTION
Components are often provided with layers in order to achieve a certain function, such as for example resistance to corrosion, oxidation and/or heat (thermal barrier). In this case, the coated components may also be rotating components, such as for example blades of a compressor or a turbine of a gas turbine installation which have layers protecting against erosion or heat. In the case of large machines, a rotor is composed of a large number of individual parts (a plurality of disks each having a plurality of turbine blades), which are coated individually or in groups, and consequently it takes a long time for all the individual parts to be coated.
JP 06 099 125 A discloses a coating apparatus in which the substrate is coated during rotation.
JP 06 219 762 A discloses a coating method in which a circular cutting tool is coated while it is rotating.
U.S. Pat. No. 5,897,921 discloses a process for applying a thermal barrier coating.
U.S. Pat. No. 6,585,569 B2 discloses a process for cleaning a compressor of a gas turbine in which dry ice is introduced into the turbine.
U.S. Pat. No. 6,180,262 discloses a process in which a plurality of dismantled turbine blades of a rotor are coated all at once.
Therefore, it is an object of the invention to overcome the above problem.
SUMMARY OF THE INVENTION
This object is achieved by the process as claimed.
The subclaims list further advantageous measures which can be combined with one another in any advantageous way.
The maintenance time for a turbine is considerably shortened by the process according to the invention, since, for example in the case of a gas turbine, there is no need to wait for the turbine and turbine housing to have cooled, and/or there is no need for forced cooling, and since it is not necessary to remove all the feed lines and outer parts of the housing. Also, the turbine does not have to be reassembled and started up again. This considerably reduces the maintenance time and the associated downtime for the operator of a turbine and obviates the need for heavy machines required to lift the housing parts.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawing:
FIG. 1 diagrammatically depicts the process according to the invention,
FIG. 2 shows a turbine blade or vane,
FIG. 3 shows a combustion chamber,
FIG. 4 shows a gas turbine,
FIG. 5 shows a steam turbine.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows an apparatus 1 which includes a turbomachine with a rotor 10 .
The rotor 10 is to be coated within the interior of a housing 4 .
FIG. 1 diagrammatically depicts how the process according to the invention is to be carried out in order to coat the rotor 10 . The rotor 10 comprises a plurality of parts 7 , 120 . In the case of a rotor 103 for a turbine 100 , 300 , 303 or of a compressor 105 , the rotor 10 , 103 has, for example, at least one disk 11 , 11 ′ 133 ( FIG. 4 ), on which a plurality of turbine blades 120 , 354 ( FIG. 2 , 4 , 5 ) are arranged in a radial orientation distributed over the circumference.
The rotor 10 may comprise a plurality of disks 11 , 11 ′ each having a plurality of turbine blades 120 , 354 . A row 125 comprises, for example, a disk 11 , 133 ( FIG. 4 ) with turbine rotor blades 120 .
The rotor 10 , 103 is still arranged in its housing 4 , 138 ( FIG. 4 ) and can be rotated about a rotatable axis 16 , 102 ( FIG. 4 ).
The housing 4 , 138 is, for example, the housing of a turbine 100 , 300 , 303 or of a compressor 105 , in which the rotor 10 , 103 is operated.
According to the invention, coating material 13 is applied while the rotor 10 , 103 is therefore still in its installed position.
During the coating operation, the rotor 10 can also rotate about the axis of rotation 16 , 102 .
The coating material 13 may be in gas form, as in known from a PVD or CVD installation, and is then deposited on the surfaces of the parts 7 , 120 that are to be coated.
The coating material 13 may also be applied to the parts 7 in liquid form, in particular finely dispersed in the air.
By way of example, it is also possible to apply a slip which contains a binder and powder particles, which then produce the definitive layer. In this case, the carrier medium can also be evaporated and the binder burnt out when the coating material 13 has been applied. Then, for example by further increasing the temperature, the powder particles are sintered together, so as to produce a fixed coating. The increase in temperature can be achieved by applying a flame to the components 7 , 120 or, for example, by passing a hot gas or steam through the hollow turbine blades 120 , which leads to heating of the coated component 7 .
The coating of the rotor 10 can also be carried out while the rotor is operating. In this context, the term “operating” means that the rotor 10 is being used as intended. This means that the rotor of a compressor is compressing air, while a gas (steam, hot gas) is being expanded and performing work in the rotor of a turbine. Where the text refers to the rotor “rotating”, this does not necessarily mean that the rotor is operating. The rotor 10 is in this case, for example, part of a compressor 105 , for example, a gas turbine 100 , in which case the coating material is added as an additive to the air that is to be compressed.
It is also possible for the rotor 10 to be a rotor 103 of a gas turbine 100 , in which case the coating material 13 is added to the hot gas in operation during a reduction or increase in power of the gas turbine 100 , in order to coat the rotor blades 120 and/or guide vanes 130 of the rotor.
Furthermore, in operation the temperature of the gas can be deliberately matched to the required thermal boundary conditions for the respective coating process by more or less fuel being burnt and less compressed air being fed from the compressor to the turbine or by the temperature of the steam being controlled.
The coating material 13 may contain a metal halide (AlF 3 , AICl 3 , CrF, . . . ) which is in gas form or in the form of powder particles.
It is also possible for particles 13 in powder form (e.g. ceramics, hard metals) to be applied to the components 7 , 120 that are to be coated, and these particles are then embedded on the region of the rotors 10 , 103 which is close to the surface, if the surface or a layer in which the particles can be embedded is soft enough (for example by heating). These are, for example, coarser particles which are intended, for example, to increase the resistance to erosion of the component 7 , 120 .
The coating material 13 may, for example, be metallic (MCrAlX) or vitreous (compressor blade).
The coating process according to the invention can also be used to repair damaged blades or vanes of the compressor 105 or of the turbine 100 , 300 , 303 . In this case, the material can be selected in such a way that it is preferentially deposited on the damaged areas.
If the rotor 10 is a rotor 103 of a gas turbine 100 , the coating material 13 can, for example, be introduced into the combustion chamber 110 with the fuel, and the combustion of the fuel can heat the coating material 13 , so that it is deposited on the components 7 , 120 in a similar way to in the plasma spraying process.
It is also possible for the blades or vanes of a compressor, in particular of a compressor 105 of a turbine 100 , to be coated.
When air is being compressed in the compressor, water precipitates and can form an electrolyte in combination with other elements contained in the air, which can lead to corrosion and erosion at the compressor blades or vanes. To prevent the corrosion and erosion, it is possible for compressor blades or vanes to be provided with coatings. A coating of this type comprises, for example, a basecoat and a topcoat. A suitable basecoat is in particular a coating which comprises an inorganic binder composed of chromium phosphate compounds and contains, for example, spherical aluminum particles. Coatings of this type are disclosed in EP 0 142 418 B1 or in EP 0 905 279 A1, with the layer composition and layer structure of these patents forming part of the present disclosure. The topcoat used may, for example, be water-based chromium phosphate compounds with inert fillers and colored pigmentations.
The same procedure can also be adopted for internal coating of a turbine 100 or a compressor 105 . The turbine 100 comprises guide vanes 130 and a rotor 103 which has the rotor blades 120 .
The coating material 13 , as described above, is introduced into the turbine 100 , with the coating material 13 being deposited both on the rotor 103 and on the guide vanes 130 . The rotor 103 with the rotor blades 120 can in the process also rotate.
In this context, it is also possible to coat housing parts 4 , 138 and blades and vanes 120 , 130 or just the housing 4 , 138 .
This is done by controlled setting of temperature differences between housing 4 , 138 and blades and vanes 120 , 130 . The hollow rotor blades 120 and the hollow guide vanes 130 have separate feeds leading into their cavity for supplying a medium, so that the rotor blades 120 can be heated while the guide vanes 130 are not, or vice versa. The appropriate growth conditions for a layer to grow on a substrate (blades or vanes) are only established at a certain elevated temperature, or only this elevated temperature makes it possible to ensure that the layer will not flake off a substrate which is too cold.
A combustion chamber 110 may likewise be a component of an apparatus 1 , i.e. a gas turbine 100 , which is to be coated. In this case too, the coating material is fed into the combustion chamber 110 from the outside. As with the turbine, this can take place during operation. In this case, the coating material can be supplied via the burner 107 and is then deposited on the heat shield elements 155 , which have been suitably “temperature-controlled”.
Another way of feeding the coating material to the combustion chamber or the turbine for the coating operation is for the coating material to be added to the flow medium within the turbine 100 at the compressor outlet.
FIG. 2 shows a perspective view of a rotor blade 120 or guide vane 130 of a turbomachine, which extends along a longitudinal axis 121 .
The turbomachine may be a gas turbine of an aircraft or of a power plant for generating electricity, a steam turbine or a compressor.
The blade or vane 120 , 130 has, in succession along the longitudinal axis 121 , a securing region 400 , an adjoining blade or vane platform 403 and a main blade or vane part 406 .
As a guide vane 130 , the vane 130 may have a further platform (not shown) at its vane tip 415 .
A blade or vane root 183 , which is used to secure the rotor blades 120 , 130 to a shaft or a disk (not shown), is formed in the securing region 400 .
The blade or vane root 183 is designed, for example, in hammerhead form. Other configurations, such as a fir-tree or dovetail root, are possible.
The blade or vane 120 , 130 has a leading edge 409 and a trailing edge 412 for a medium which flows past the main blade or vane part 406 .
In the case of conventional blades or vanes 120 , 130 , by way of example solid metallic materials, in particular superalloys, are used in all regions 400 , 403 , 406 of the blade 120 , 130 .
Superalloys of this type are known, for example, from EP 1 204 776 B1, EP 1 306 454, EP 1 319 729 A1, WO 99/67435 or WO 00/44949; these documents form part of the disclosure. The blade or vane 120 , 130 may in this case be produced by a casting process, also by means of directional solidification, by a forging process, by a milling process or combinations thereof.
Work pieces with a single-crystal structure or structures are used as components for machines which, in operation, are exposed to high mechanical, thermal and/or chemical stresses.
Single-crystal work pieces of this type are produced, for example, by directional solidification from the melt. This involves casting processes in which the liquid metallic alloy solidifies to form the single-crystal structure, i.e. the single-crystal work piece, or solidifies directionally.
In this case, dendritic crystals are oriented along the direction of heat flow and form either a columnar crystalline grain structure (i.e. grains which run over the entire length of the work piece and are referred to here, in accordance with the language customarily used, as directionally solidified) or a single-crystal structure, i.e. the entire work piece consists of one single crystal. In these processes, a transition to globular (polycrystalline) solidification needs to be avoided, since non-directional growth inevitably forms transverse and longitudinal grain boundaries, which negate the favorable properties of the directionally solidified or single-crystal component.
Where the text refers in general terms to directionally solidified micro structures, this is to be understood as meaning both single crystals, which do not have any grain boundaries or at most have small-angle grain boundaries, and columnar crystal structures, which do have grain boundaries running in the longitudinal direction but do not have any transverse grain boundaries. This second form of crystalline structures is also described as directionally solidified micro structures (directionally solidified structures).
Processes of this type are known from U.S. Pat. No. 6,024,792 and EP 0 892 090 A1; these documents form part of the disclosure.
The blades or vanes 120 , 130 may likewise have coatings protecting against corrosion or oxidation (MCrAlX; M is at least one element selected from the group consisting of iron (Fe), cobalt (Co), nickel (Ni), X is an active element and represents yttrium (Y) and/or silicon (Si) and/or at least one rare earth element, or hafnium (Hf)). Alloys of this type are known from EP 0 486 489 B1, EP 0 786 017 B1, EP 0 412 397 B1 or EP 1 306 454 A1, which are intended to form part of the present disclosure.
It is also possible for there to be a thermal barrier coating, consisting for example of ZrO 2 , Y 2 O 4 —ZrO 2 , i.e. unstabilized, partially stabilized or completely stabilized by yttrium oxide and/or calcium oxide and/or magnesium oxide, to be present on the MCrAlX. Columnar grains are produced in the thermal barrier coating by means of suitable coating processes, such as for example electron beam physical vapor deposition (EB-PVD).
Refurbishment means that after they have been used, protective layers may have to be removed from components 120 , 130 (e.g. by sand-blasting). Then, the corrosion and/or oxidation layers and products are removed. If appropriate, cracks in the component 120 , 130 are also repaired by soldering or welding. This is followed by recoating of the component 120 , 130 , after which the component 120 , 130 can be reused.
The blade or vane 120 , 130 may be hollow or solid in form. If the blade or vane 120 , 130 is to be cooled, it is hollow and may also have film-cooling holes 418 (indicated by dashed lines).
FIG. 3 shows a combustion chamber 110 of a gas turbine. The combustion chamber 110 is configured, for example, as what is known as an annular combustion chamber, in which a multiplicity of burners 107 arranged circumferentially around the axis of rotation 102 open out into a common combustion chamber space. For this purpose, the combustion chamber 110 overall is of annular configuration positioned around the axis of rotation 102 .
To achieve a relatively high efficiency, the combustion chamber 110 is designed for a relatively high temperature of the working medium M of approximately 1000° C. to 1600° C. To allow a relatively long service life even with these operating parameters, which are unfavorable for the materials, the combustion chamber wall 153 is provided, on its side which faces the working medium M, with an inner lining formed from heat shield elements 155 .
On the working medium side, each heat shield element 155 is equipped with a particularly heat-resistant protective layer or is made from material that is able to withstand high temperatures. These may be solid ceramic bricks or alloys with MCrAlX and/or ceramic coatings. The materials of the combustion chamber wall and their coatings may be similar to the turbine blades or vanes.
A cooling system may also be provided for the heat shield elements 155 and/or their holding elements, on account of the high temperatures in the interior of the combustion chamber 110 .
FIG. 4 shows, by way of example, a partial longitudinal section through a gas turbine 100 .
In the interior, the gas turbine 100 has a rotor 103 which is mounted such that it can rotate about an axis of rotation 102 and is also referred to as the turbine rotor.
An intake housing 104 , a compressor 105 , a, for example, toroidal combustion chamber 110 , in particular an annular combustion chamber 106 , with a plurality of coaxially arranged burners 107 , a turbine 108 and the exhaust-gas housing 109 follow one another along the rotor 103 .
The annular combustion chamber 106 is in communication with a, for example, annular hot-gas passage 111 , where, by way of example, four successive turbine stages 112 form the turbine 108 .
Each turbine stage 112 is formed, for example, from two blade or vane rings. As seen in the direction of flow of a working medium 113 , in the hot-gas passage 111 a row of guide vanes 115 is followed by a row 125 formed from rotor blades 120 .
The guide vanes 130 are secured to an inner housing 138 of a stator 143 , whereas the rotor blades 120 of a row 125 are fitted to the rotor 103 for example by means of a turbine disk 133 . A generator (not shown) is coupled to the rotor 103 .
While the gas turbine 100 is operating, the compressor 105 sucks in air 135 through the intake housing 104 and compresses it. The compressed air provided at the turbine-side end of the compressor 105 is passed to the burners 107 , where it is mixed with a fuel. The mix is then burnt in the combustion chamber 110 , forming the working medium 113 . From there, the working medium 113 flows along the hot-gas passage 111 past the guide vanes 130 and the rotor blades 120 . The working medium 113 is expanded at the rotor blades 120 , transferring its momentum, so that the rotor blades 120 drive the rotor 103 and the latter in turn drives the generator coupled to it.
While the gas turbine 100 is operating, the components which are exposed to the hot working medium 113 are subject to thermal stresses. The guide vanes 130 and rotor blades 120 of the first turbine stage, as seen in the direction of flow of the working medium 113 , together with the heat shield bricks which line the combustion chamber 106 , are subject to the highest thermal stresses.
To be able to withstand the temperatures which prevail there, they have to be cooled by means of a coolant.
Substrates of the components may likewise have a directional structure, i.e. they are in single-crystal form (SX structure) or have only longitudinally oriented grains (DS structure).
By way of example, iron-base, nickel-base or cobalt-base superalloys are used as material for the components, in particular for the turbine blade or vane 120 , 130 and components of the combustion chamber 110 .
Superalloys of this type are known, for example, from EP 1 204 776 B1, EP 1 306 454, EP 1 319 729 A1, WO 99/67435 or WO 00/44949; these documents form part of the disclosure.
The blades or vanes 120 , 130 may also have coatings which protect against corrosion (MCrAlX; M is at least one element selected from the group consisting of iron (Fe), cobalt (Co), nickel (Ni), X is an active element and represents yttrium (Y) and/or silicon and/or at least one rare earth element or hafnium). Alloys of this type are known from EP 0 486 489 B1, EP 0 786 017 B1, EP 0 412 397 B1 or EP 1 306 454 A1, which are intended to form part of the present disclosure.
A thermal barrier coating, consisting for example of ZrO 2 , Y 2 O 4 —ZrO 2 , i.e. unstabilized, partially stabilized or completely stabilized by yttrium oxide and/or calcium oxide and/or magnesium oxide, may also be present on the MCrAlX. Columnar grains are produced in the thermal barrier coating by suitable coating processes, such as for example electron beam physical vapor deposition (EB-PVD).
The guide vane 130 has a guide vane root (not shown here), which faces the inner housing 138 of the turbine 108 , and a guide vane head which is at the opposite end from the guide vane root. The guide vane head faces the rotor 103 and is fixed to a securing ring 140 of the stator 143 .
FIG. 5 illustrates, by way of example, a steam turbine 300 , 303 with a turbine shaft extending along an axis of rotation 306 .
The steam turbine has a high-pressure partial turbine 300 and a medium-pressure partial turbine 303 , each with an inner housing 312 and an outer housing 315 surrounding it.
The high-pressure partial turbine 300 is, for example, of pot-like configuration.
The medium-pressure partial turbine 303 is of two-flow design.
It is also possible for the medium-pressure partial turbine 303 to be of single-flow design.
A bearing 318 is arranged between the high-pressure partial turbine 300 and the medium-pressure partial turbine 303 along the axis of rotation 306 , the turbine shaft 309 having a bearing region 321 in the bearing 318 . The turbine shaft 309 is mounted on a further bearing 324 next to the high-pressure partial turbine 300 . In the region of this bearing 324 , the high-pressure partial turbine 300 has a shaft seal 345 . The turbine shaft 309 is sealed by two further shaft seals 345 with respect to the outer housing 315 of the medium-pressure partial turbine 303 . Between a high-pressure steam inlet region 348 and a steam outlet region 351 , the turbine shaft 309 has the high-pressure rotor blading 354 , 357 in the high-pressure partial turbine 300 . This high-pressure rotor blading 354 , 357 , together with the associated rotor blades (not shown in more detail), represents a first blading region 360 . The medium-pressure partial turbine 303 has a central steam inlet region 333 . Assigned to the steam inlet region 333 the turbine shaft 309 has a radially symmetrical shaft shield, a covering plate, on the one hand for dividing the flow of steam into the two flows for the medium-pressure partial turbine 303 and for preventing direct contact between the hot steam and the turbine shaft 309 . In the medium-pressure partial turbine 303 , the turbine shaft 309 has a second blading region 366 comprising the medium-pressure rotor blades 354 , 342 . The hot steam which flows through the second blading region 366 flows out of the medium-pressure partial turbine 303 from an outlet connection piece 369 to a low-pressure partial turbine, which is connected downstream in terms of flow but is not illustrated. | A method for coating a component of a turbo-machine. The method allows arranging a turbine rotor in the turbo-machine and introducing a coating material into the interior of the turbo-machine such that the rotor is coated. The rotor is rotated while it is being coated. | 5 |
FIELD OF THE INVENTION
The present invention relates to nitrogen containing macronutrient composition for slow and sustained release in fertilizer applications. More particularly, the present invention relates to urea derivatives that are encapsulated within a cellulose structure comprising vascular canals, intercellular spaces and cells.
BACKGROUND OF THE INVENTION
Nutrient availability in the soil-plant system is dictated by complex interactions between plant roots, soil microorganisms, chemical reactions and pathways of losses. The macronutrients required by the plant can be lost by chemical processes such as exchange, fixation, precipitation and hydrolysis, and physical processes such as leaching, runoff and volatilization. Nitrogen, phosphorus and potassium (NPK), which are required in large amounts for plants, are not adequately available in natural soils to support the sustained growth of plants. Therefore, these macronutrients (NPK) are needed to be applied externally through fertilizers. Water soluble conventional fertilizers typically result in a large amount of macronutrients being lost by leaching and evaporation. There is an increased interest in developing slow release fertilizers that release macronutrients to plants over time. Advantages of slow release fertilizers are improved efficiency and quality as the fertilizer is released over time thus providing sufficient quantities of macronutrients as required for higher crop yields. In addition, slow release fertilizers result in reduced environmental damage from leaching of macronutrients into water and emissions as gasses, compared to conventional water soluble fertilizers.
Macronutrients in fertilizers can be applied to the soil as a solid in the form of a powder or pellets or as a spray. The uptake of macronutrients by the plant needs to be compensated by their external application to the soil periodically. Nitrogen is a key macronutrient source in agriculture particularly for economic crops such as tea, rubber and coconut. Large amount of fertilizer is applied to the soil of the tea plant to improve the quality and the yield of the leaves produced. For example, a study in Japan (Yamada et al., Journal of Water and Environmental Technology, 7, 4, 331-340, 2009) reported that of the large amount of amount of nitrogen fertilizer applied to tea, only 12% of the nitrogen input was up taken by the plant and the rest was discharged to the environment.
Coconut plants require an equatorial climate with high humidity to grow. Coconut plants and trees are grown in different soil types such as laterite, coastal sandy, alluvial, and also in reclaimed soils of the marshy lowlands. One of the unique features of coconut trees and plants are that it tolerates salinity and a wide range of pH (from 5.0-8.0). In terms of fertilizer application, the amount of N, P, and K required varies according to the type of coconut plantation. In addition Mg may become important in some soils.
Therefore, one of the unsolved problems of fertilizer application is, in relation to the amounts of nitrogen applied to soil, the low Nitrogen Use Efficiency (NUE) by crops. This is because an excessive amount of nitrogen, up to 70%, is lost in conventional fertilizers due to leaching, emissions, and long-term incorporation by soil microorganisms. As such, supplying N macronutrient is critical in preventing the decline of productivity and profitability due to degradation and aging of tea plants (Kamau et al., Field Crops Research 1, 108, 60-70, 2008). Attempts to increase the NUE have so far met with little success.
US2006/0135365 discloses wood chips containing macronutrient salts for short term plant growth and release of macronutrients over a period of one week. U.S. Pat. No. 7,165,358 disclose woodchips as a substrate for macronutrients for plant growth. U.S. Pat. No. 2,714,553 disclose converting wood lignin to sugar and forming a urea-formaldehyde condensation product for macronutrient delivery. U.S. Pat. No. 6,900,162 discloses a composition containing nitrogen particles adhered by a binder degraded by soil moisture to provide for the slow release. U.S. Pat. No. 7,211,275 B2 discloses a sustained release composite of water soluble materials that are adsorbed onto an inorganic material and is released by acidic fluids in medical applications.
Solutions are needed to provide slow and sustained release macronutrient formulations for plant growth applications. Therefore, macronutrients incorporated into cavities present in wood could be used to provide slow and sustained release of macronutrients for plant growth.
SUMMARY OF THE INVENTION
Accordingly provided herein is a macronutrient delivery system that contains nitrogen containing macronutrient compound adsorbed on the surface of hydroxyapatite phosphate (HAP) nanoparticles. These macronutrient adsorbed HAP nanoparticles are encapsulated within the cavities present in wood. Alternatively, macronutrient particles have been encapsulated within the cavities present in wood followed by a thin coating of cellulose modified HAP nanoparticles. In an embodiment, nitrogen containing macronutrient compounds such as urea, thiourea, or a mixture thereof are adsorbed onto the surface of HAP nanoparticles and encapsulated within the cavities present in wood. Also disclosed herein is a process for the encapsulation of macronutrient adsorbed HAP nanoparticles/macronutrients within the cavities present in wood. The encapsulated macronutrient adsorbed nanoparticles or macronutrients encapsulated nanoparticle coated compounds prepared by this process when applied to aqueous and terrestrialenvironments released the macronutrient in a slow and sustained manner. It is believed that macronutrient adsorbed HAP nanoparticles or macronutrient particles that are included in the cavities of the wood provide for the release of the macronutrient compound in aqueous and terrestrial environments. The soil in aqueous and terrestrial environments provides the medium for transport of the macronutrients to the roots of the plant. Embodiment plants and trees include and are not limited to any crop that grows in a low pH environment (low pH crop) such as tea, rubber and coconut.
DESCRIPTION OF THE FIGURES
FIG. 1 . XRD pattern of synthesized HAP nanoparticles
FIG. 2 . SEM images of synthesized HAP nanoparticles
FIG. 3 . XRD pattern of the urea adsorbed HAP nanoparticles
FIG. 4 . SEM image of urea adsorbed HAP nanoparticles
FIG. 5 . Schematic representation of the possible structure of the urea adsorbed HAP nanoparticles
FIG. 6 . Optical microscopic image of stem cross section of G. sepium
FIG. 7 . N release kinetics for soil from sandy soil (a) fertilizer composition based on urea adsorbed HAP nanoparticles encapsulated within cavities of G. sepium (b) Commercial fertilizer
FIG. 8 . N release kinetics for soil at an elevation of 1600 feet (a) fertilizer composition based on urea adsorbed HAP nanoparticles encapsulated within cavities of G. sepium (b) Commercial fertilizer
FIG. 9 . N release kinetics for soil at an elevation of 4000 feet (a) fertilizer composition based on urea adsorbed HAP nanoparticles encapsulated within cavities of G. sepium (b) Commercial fertilizer
DETAILED DESCRIPTION
Nitrogen containing macronutrient composition for slow and sustained release in fertilizer applications are described in detail herein below. Fertilizers contain micro- and macronutrients that are essential for plant growth.
As referred to herein primary macronutrients are nitrogen (N), phosphorous (P), and potassium (K) while calcium (Ca), magnesium (Mg), and sulfur (S) are secondary macronutrients. All six nutrients are important for plant growth.
As referred to herein, micronutrients required in small amounts for plant growth are boron (B), chlorine (CI), manganese (Mn), iron (Fe), zinc (Zn), copper (Cu), molybdenum (Mo) and selenium (Se).
As referred to herein sustained release of macronutrient is release in a constant and continual manner.
As referred to herein the slow release of macronutrient provides the plant with nutrients gradually over an extended period of time. Soils applied with slow release fertilizer that contain macronutrients will require less applications of such fertilizer and leads to higher efficiency of macronutrient release compared to conventional fast release fertilizers.
As referred to herein the encapsulation refers to localization of the macronutrients within cavities in the wood. Encapsulation can include covalent bonds, electrostatic bonds, Van der Waals bonds and hydrogen bonds.
Adsorption as defined herein refers to any means that forms a complex between the walls of the cavities and nitrogen containing macronutrient compound; and nitrogen containing macronutrient compound and HAP nanoparticles. Adsorption can include covalent bonds, electrostatic bonds, Van der Waals bonds and hydrogen bonds.
Urea is adsorbed on the surface of hydroxy apatite phosphate (HAP) nanoparticles. After these urea adsorbed HAP nanoparticles are encapsulated within the cavities present in a transporter medium both nitrogen and phosphorus will be released slowly.
If potassium ions are encapsulated separately into cavities of wood then they too would be released slowly.
Coating as defined herein refers to a thin layer of cellulose modified nanoparticles adsorbed onto the wood surface. Adsorption can include covalent bonds, electrostatic bonds, Van der Waals bonds and hydrogen bonds.
Plants as referred to herein include trees, seedlings and mature trees.
Transporter media as referred to herein include any media with sufficient cavities for the storage and transport of the macronutrient compound such as clays, layered double hydroxides, wood, orange peels, lemon peels, banana peels, or other lignin or cellulose containing materials.
Cavities as referred to herein include vascular canals, intercellular spaces, spaces present in clays and cells. These cavities are commonly found in wooded plants and clays. Examples of suitable wooded plants with cavities are Gliricidia sepium (Jacq.) Kunth ex Walp and coniferous plants such as those belonging to the family Pinaceae. The size of the cavities varies with maturity of the wooded plant. Cavities such as vascular canals, xylem and phloem, vary in size depending on the age of the wooded plant. The xylem transports water while the phloem transports nutrients and when the wooded plants are dried the aqueous nutrients present within the xylem and phloem are removed. The size of the vascular canals can range from 1 to 30 micrometer range. The intercellular spaces that are found can be in the nanoscale (i.e. below 100 nm).
Once encapsulated, these cavities will become reservoirs for storage of macronutrients.
Macronutrients in encapsulated HAP nanoparticles or macronutrients localized in vascular canals can be released early during fertilization due to the large volume of the vascular canals. Cells which are smaller in volume than vascular canals but larger than intercellular spaces can release the macronutrients at an intermediate stage during fertilization. Macronutrient in encapsulated HAP nanoparticles localized within smaller volumes of intercellular spaces may release the macronutrient at the final stages during fertilization. It is believed, not bound by any theory, that smaller cavities adsorb the macronutrient efficiently in encapsulated HAP nanoparticles on the surface walls comprising cellulose, lignin and hemi-cellulose.
Preparation of Macronutrient Adsorbed HAP Nanoparticles
HAP nanoparticles can be chemically synthesized using calcium hydroxide suspension and phosphoric acid (Mateus et al., Key Engineering Materials, 330-332, 243-246, 2007). Adsorption of nitrogen containing macronutrient compound such as urea can be facilitated by stirring the HAP nanoparticles in a concentrated urea solution. Other nitrogen containing macronutrient compounds can also be used for adsorption on the HAP nanoparticles. Such adsorbed nitrogen containing macronutrient compounds can be encapsulated within cavities present in wood or another suitable transport medium as defined herein.
Encapsulation of Macronutrient Adsorbed HAP Nanoparticles
Encapsulation of the nitrogen containing macronutrient compound adsorbed onto the surface of HAP nanoparticles into the cavities present in the wood is described herein below.
First the nitrogen containing macronutrient compound is adsorbed onto the surface of HAP nanoparticles which were prepared as described above.
Second the G. sepium wood was cut into pieces of approximately 1 inch in length and they were partially dried under vacuum. Finally, macronutrient compound adsorbed HAP nanoparticles were encapsulated into the partially dried G. sepium stem by pressurizing (1 bar-15 bar) the macronutrient compound adsorbed HAP nanoparticle dispersion into the cavities of the wood. Alternatively, macronutrient compound adsorbed HAP nanoparticle dispersion can be encapsulated into the cavities of the wood under vacuum (0-100 kPa). The percentage of N in the macronutrient compound adsorbed HAP nanoparticles encapsulated within the cavities can vary with age of the wooded plant. In an embodiment the nitrogen content of G. sepium wood ranged between 6-15% by weight.
Encapsulation of the nitrogen containing macronutrient compound into the cavities present in the wood and coating of the wood with cellulose modified HAP nanoparticles is described herein below.
G. sepium wood was cut into pieces of approximately 1 inch in length and were partially dried under vacuum. Macronutrient compound containing nitrogen was encapsulated into the partially dried G. sepium stem by pressurizing (1 bar-15 bar) a saturated solution of nitrogen containing macronutrient into the cavities of the wood. The micronutrient encapsulated wood was then coated by dipping or spraying with cellulose modified HAP nanoparticles.
The percentage of N in the macronutrient compound adsorbed HAP nanoparticles encapsulated within the cavities can vary with age of the wooded plant. In an embodiment the nitrogen content of G. sepium wood ranged between 10-20% by weight.
Release Behavior in Soils
In certain embodiments a uniform release of nitrogen over a period up to 3 months is observed. During fertilization of tea plants, the frequency of application can be attenuated depending on the fertilizer requirement of a given tea plantation. This can be done by starting a second round of application at a suitable period prior to reaching the end of the first application of the macronutrient adsorbed HAP nanocomposite. In another embodiment, multiple applications of the HAP nanocomposite are distributed on acidic soils within three months. In another embodiment soil found at about 4000 feet in tea plantations, for example from Thalawakelai, Sri Lanka, can be used for slow and sustained release of the nitrogen containing macronutrient. In another embodiment soil found at about 1600 feet in tea plantations, for example from Kandy, Sri Lanka, can be used for slow and sustained release of the nitrogen containing macronutrient.
Sandy soils are suitable for coconut growth and in an embodiment the encapsulated macronutrient releasing nitrogen can be used for fertilization. Further, in an embodiment, the encapsulated macronutrient can be used to fertilize rubber plants and trees.
Organic matter content of soil between 1600 to 4000 feet elevation can range from 2 to 3%. In general, higher elevations contain more organic matter compared to lower elevations such as sea level. Such high organic matter could lead to lowering of pH of the soil. The macronutrient encapsulated wood cavities are superabsorbent bio polymers such as cellulose, hemi-cellulose and lignin. Such superabsorbent bio polymers absorb moisture in large amounts and initiates microbial degradation when in contact with soils. Acidic products are formed due to the microbial degradation, and encapsulated macronutrients are released.
In an embodiment, low phosphorous release behavior indicates that P may be released slower than the depletion of nitrogen during the three month period.
This may be the result of HAP nanoparticles being held tightly within the cavities compared to the adsorbed urea. In an embodiment K can exhibit slow and sustained release over the three months period.
EXAMPLES
Example 1
Preparation of HAP Nanoparticles
HAP nanoparticles were synthesized by drop wise addition of phosphoric acid (250 ml of 0.6 M) into a suspension of calcium hydroxide (19.29 g/250 ml). The reaction was carried out under mechanical stirring (1000 rpm). The reaction takes place according to the following equation.
6H 3 PO 4 +10Ca(OH) 2 →Ca 10 (PO 4 ) 6 (OH) 2 +18H 2 O
HAP nanoparticles synthesized as described above were allowed to settle and the supernatant was decanted. This process was repeated three times using distilled water to purify the product. The solid obtained was dried at 100° C. for two hours to provide 25 g of HAP nanoparticles which were characterized using XRD, SEM/EDX, AFM and FTIR.
As seen from FIG. 1 , the XRD pattern indicated that the synthesized HAP nanoparticles were identical to a commercial sample obtained from Sigma Aldrich Chemical Company, USA. No other peaks were observed confirming the absence of any other crystalline impurities. As evidenced by EDX spectra, the presence of Ca and P was confirmed. As seen from FIG. 2 , SEM images of HAP nanoparticles, exhibited needle like morphology with a diameter less than 30 nm. AFM images corroborated the uniform particle size. The particle size distribution was also confirmed by the particle size measurements done using a Malvern, nanoZS, ZEN 3600.
FTIR spectrum further confirmed the presence of HAP nanoparticles and the peak assignments are given in Table 1 below:
TABLE 1
FTIR peak assignments for HAP nanoparticles
Wavenumber/cm −1
Peak assignment
1080-1020
P—O stretching of PO 4 3−
3600-3580, 633
O—H stretching
1640
O—H bending of adsorbed water
Example 2
Synthesis of Urea Adsorbed HAP Nanoparticles
HAP nanoparticles synthesized as described in Example 1 were treated with 250 ml of 1M urea solution. The solution was stirred mechanically at 750 rpm for 12 hours. In another experiment the solution was subjected to ultrasonic mixing at 30 kHz for 45 minutes. The excess liquid was decanted and the product was washed to remove the excess urea.
The product was characterized using XRD, SEM/EDX and FTIR. As seen in FIG. 3 , XRD pattern of the urea adsorbed HAP nanoparticles indicated the presence of peaks due to HAP, and an extra peak that was attributed to the adsorbed urea.
FIG. 4 represents the SEM image of urea adsorbed HAP nanoparticles; the particle size and the morphology of the HAP nanoparticles were not significantly changed by surface adsorption of urea.
Table 2 represents FTIR data obtained for urea, HAP nanoparticles and urea adsorbed HAP nanoparticles.
As seen from Table 2, N—H stretching frequency of pure urea appears as a doublet at 3430 cm −1 and 3340 cm −1 and once urea is bonded to HAP nanoparticles it gives rise to a noticeable shift to 3300 cm −1 . This shift reveals that the NH 2 groups of urea are bonded to OH groups of HAP nanoparticles via H-bonding. This can be confirmed further by the peak broadening in the corresponding N—H stretching frequencies of urea. The band at 1590 cm −1 for the N—H bending motion was still present although shifted to 1627 cm −1 for urea adsorbed HAP nanoparticles. This indicates the presence of free unbound NH 2 groups even after adsorption of urea onto the HAP nanoparticles. The relatively free NH 2 groups may be held within the encapsulated structure and may be released at the early stages during fertilization.
TABLE 2
FTIR peak assignment for urea, HAP nanoparticles and urea adsorbed HAP nanoparticles.
Urea adsorbed
Wavenumber/
Wavenumber/
HAP
Wavenumber/
HAP
cm −1
Urea
cm −1
nanoparticles
cm −1
nanoparticles
3430, 3340
N—H
~3300
N—H/O—H
doublet
stretching
broad
stretching
1680
carbonyl
1666
carbonyl
stretching
stretching
1590
N—H
1627
N—H bending
1460
N—C—N
1446
N—C—N
stretching
stretching
1030
P—O
1030
P—O stretching of
stretching of
PO 4 3
PO 4 3
3500, 633
O—H
3300
O—H stretching
stretching
broad
3350-3550
adsorbed or
3350-3550
adsorbed or
bound water
bound water
1640
O—H bending
1627
O—H bending
The carbonyl stretching frequency of pure urea appears at 1680 cm −1 while the corresponding peak for urea adsorbed HAP nanoparticles is at 1666 cm −1 . There is a clear shift in stretching frequency of the carbonyl group for urea adsorbed HAP nanoparticles indicating that urea is bonded to HAP nanoparticles through the carbonyl group. This can be further confirmed by a noticeable peak shift of the N—C—N stretching frequency (1460 cm −1 ) of urea to a lower frequency in urea adsorbed HAP nanoparticles (1446 cm −1 ).
Urea may be adsorbed on the surface of HAP by several binding modes of unequal binding strengths. This can give rise to different binding environments when encapsulated within the cavities of wood, giving rise to different patterns of release behavior when contacted with soils.
According to the elemental analysis, the urea adsorbed HAP nanoparticles contained 14%; C, 5%; H, 33%; N and 6%; P.
Schematic representation (not drawn to scale) of the structure of the urea adsorbedHAP nanoparticles is given in FIG. 5 .
Example 3
Encapsulation of Urea Adsorbed HAP Nanoparticles into the Cavities G. sepium
First, G. sepium wood was cut into 1-5 cm pieces and vacuum dried at 0.5 bar for 1 hr. The vacuum dried G. sepium pieces were soaked in excess amount of a dispersion made from urea adsorbed HAP nanoparticles. This system was subjected to a pressure of 1 kg cm −2 for 2-24 hrs. The pressure treated G. sepium pieces were oven dried at 50° C. for 5 hrs and characterized using NPK elemental analysis, SEM and FTIR.
The presence of nitrogen in G. sepium was confirmed by NPK analysis, 6%; N, 1%; P. The NPK analysis of untreated G. sepium was 1.26%; N, 0.29%; P and 1.79%; K.
As seen from FIG. 6 , the optical micrograph of the G. sepium wood showed the highly porous structure. In FTIR, the characteristic peaks of HAP nanoparticles, phosphate stretching vibrations around 1050 cm −1 , water bending motions 1680 cm −1 , and the broad hydroxyl stretching peak are found in urea adsorbed HAP nanoparticle encapsulated G. sepium wood confirming the presence of HAP nanoparticles within the cells. The characteristic doublet in the urea stretching frequency around 3500 cm −1 appears as one broad single peak suggesting a chemical bonding environment of urea within the cells of the G. sepium wood.
Example 4
Encapsulation of Urea into the Cavities G. sepium and Coating with HAP Nanoparticles
First, G. sepium wood was cut in to 1-5 cm pieces and vacuum dried at 0.5 bar for 1 hr. The vacuum dried G. sepium pieces (300 g) were soaked in a saturated urea solution (450 g of urea in 2 L of water). This system was subjected to a pressure of 1 kg cm −2 for 2 hrs. The pressure treated G. sepium pieces were oven dried at 50° C. for 5 hrs and characterized using NPK elemental analysis, SEM and FTIR.
Secondly, a surface coating of cellulose modified HAP nanoparticles was applied on urea encapsulated G. Sepium wood. HAP nanoparticles prepared as above was mixed with carboxymethyl cellulose (CMC) solution (50 g CMC in 250 ml water) by dipping. Cellulose modified HAP nanoparticle coated G. Sepium wood was dried at 50° C. for four hours.
The presence of nitrogen in G. sepium was confirmed by N and P analysis, 16%; N, 1%; P. The NPK analysis of untreated G. sepium was 1.26%; N, 0.29%; P and 1.79%; K.
Example 5
Release Kinetics of Urea Adsorbed HAP Nanoparticles Encapsulated G. sepium Wood and Commercial Fertilizer
Three soil samples (1000 g each of (a) sandy soil found at sea level; (b) soil found at an elevation of 1600 feet in a tea plantation; and (c) soil found at an elevation of 4000 feet in a tea plantation) were each mixed with 20 g of commercial fertilizer formulation for tea (T 65); the T65 formulation contained urea (N 11%), super phosphate (P 11%) and potash (K 11%); and was purchased from Hayleys Agro Ltd., Colombo, Sri Lanka.
These three soil samples containing commercial T65 fertilizer was filled into three glass columns. Similarly, three equal amounts of urea adsorbed HAP nanoparticles encapsulated G. sepium wood and urea adsorbed G. Sepium wood coated with cellulose modified HAP nanoparticles having an NPK content similar as those used in the commercial samples, were taken separately and filled into three glass columns containing three soil samples (a), (b) and (c) as described above. Next, 180 ml water was added to all six soil columns until they reached the soil water saturation point, and maintained the water content approximately constant throughout the period of study. Water (100 ml) was added at five day intervals prior to elution. The eluted solutions (50 ml) were collected for NPK analysis. NPK analysis was done by Kjeldhal (N), vanadamolybdate (P) and flame photometry (K).
The N release kinetics is shown in FIGS. 7 through 9 . As shown in FIGS. 7 through 9 , on day 55 the macronutrient adsorbed HAP nanoparticles encapsulated within cavities of the transporter medium are still releasing at a slow and sustained manner such that at least 100 ppm of nitrogen was being released into the soil, whereas the amount of nitrogen released by the commercial fertilizer at this time is less.
A slow and sustained release of N over a period of 2 months for both the acidic soils at elevations of 1600 feet (pH of 4.7) and 4000 feet (pH of 5.2) and sandy soil (pH 7) was observed. Fluctuations in the N release kinetics are observed in the columns which contained commercial fertilizer. This was attributed a release of a large quantity during the first two weeks followed by the release of very low quantities until about day 30 and subsequent depletion to negligible amounts (see FIGS. 7 to 9 ). The Nitrogen release conditions at soils at an elevation of 1600 feet and 4000 feet and the sandy soil at sea level indicated the sustained release behavior even after 30 days.
The P release amounts were less than optimal levels required for all three types of soils. | A macronutrient sustained release composition for a plant locus having nitrogen containing macronutrient compound adsorbed on the surface of hydroxyapatite phosphate nanoparticles, and a process for preparation thereof. The macronutrient adsorbed hydroxyapatite phosphate nanoparticles are encapsulated within cavities present in wood such that the biodegradation of the wood releases the adsorbed macronutrient compounds in a slow and sustained manner to the soil. Further, the macronutrient particles are encapsulated within the cell cavities of wood and wood is coated with cellulose modified hydroxyapatite phosphate nanoparticles such that the rupture of the nanocoating initiates the nitrogen release followed by the biodegradation of the wood releases the rest of the adsorbed macronutrient compounds in a slow and sustained manner to the soil. | 2 |
TECHNICAL FIELD
Embodiments of the present invention relate generally to integrated memory devices, and more specifically, in one or more embodiments, to an input buffer that can operate in a symmetrical manner despite receiving a single-ended input signal rather than complementary input signals.
BACKGROUND
Input buffers are used for a wide variety of functions in integrated circuits. Buffers generally have a high input impedance to avoid excessively loading circuits to which they are connected, and, conversely, have a low output impedance to drive electrical circuits without excessive loading. Buffers are typically used in digital circuits to condition electrical signals applied to internal circuitry so that internal signals are generated with well-defined logic levels and transition characteristics. For example, buffers may be utilized for coupling command, address and write data signals from respective buses in a memory device, such as a dynamic random access memory (“DRAM”) and a synchronous dynamic random access memory (“SDRAM”), so that clean, unambiguous signals are properly received by various components of the memory device.
Input buffer circuits may be used to convert high speed, small swing input signals to digital signals, such as signals required by internal circuitry in memory devices. Differential input buffers conventionally include differential amplifiers, which are symmetrically structured and typically have a differential pair of input terminals and/or output terminals. The symmetrical topography of these differential amplifiers causes them to operate in a symmetrical manner when they receive complementary signals. Differential input buffers are particularly useful in digital circuits for determining whether a single input signal is above a fixed reference voltage, signifying a logic “1” or below the fixed reference voltage, signifying a logic “0”. However, in such cases, the input buffers receive a single input signal rather than two complementary input signals. This lack of symmetry in applying signals to the input buffers can cause them to operate in a non-symmetrical manner. As a result, they may not respond to an input signal transitioning from a first level to a second level in the same manner that they respond to an input signal transitioning from the second level to the first level. Moreover, input buffers respond faster to a differential input and hence, can be used at higher frequencies for differential inputs.
There is, therefore, a need for an input buffer that operates more symmetrically when receiving a single-ended input signal so that it responds to transitions of the input signal in one direction in the same manner that it responds to transitions of the input signal in the opposite direction.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic of a differential input buffer circuit according to an embodiment of the invention.
FIG. 2 is signal diagram showing input and output signals of the differential input buffer circuit of FIG. 1 .
FIG. 3 is a functional block diagram illustrating a memory device that includes at least one differential input buffer circuit according to an embodiment of the invention.
FIG. 4 is a functional block diagram illustrating a computer system including the memory device of FIG. 3 .
DETAILED DESCRIPTION
Certain details are set forth below to provide a sufficient understanding of embodiments of the invention. However, it will be clear to one skilled in the art that embodiments of the invention may be practiced without these particular details. Moreover, the particular embodiments of the present invention described herein are provided by way of example and should not be used to limit the scope of the invention to these particular embodiments. In other instances, well-known circuits, control signals, and timing protocols have not been shown in detail in order to avoid unnecessarily obscuring the invention.
One embodiment of a differential input buffer 100 is shown in FIG. 1 that includes a pair of differential amplifiers 101 , 102 . The amplifiers 101 , 102 are connected in parallel between a PMOS transistor 105 coupled to a supply voltage V CC and an NMOS transistor 108 coupled to ground GND. The PMOS transistor 105 is turned ON by an active low ENABLE control signal that also turns ON the NMOS transistor 108 by coupling the ENABLE signal to the gate of the NMOS transistor 108 through an inverter 107 . When turned ON, the transistor 105 functions as a current source providing a constant current to the amplifiers 101 , 102 at a node 106 , and the transistor 108 functions as a current sink to discharge a constant current from the amplifiers 101 , 102 at a node 109 .
The amplifiers 101 , 102 have essentially the same components, but are configured complementary with respect to each other. The amplifier 101 includes a pair of PMOS transistors 116 , 118 whose gates are coupled to each other in a manner such that their gate-to-source voltages are the same. Therefore, the transistors 116 , 118 have the same ON-resistance (source-to-drain/drain-to-source resistance). The drains of the transistors 116 , 118 are respectively coupled to the drains of NMOS transistors 120 , 122 , whose gates are configured to receive input terminals to the buffer 100 . The gate of the transistor 120 receives an input signal V IN , and the gate of the transistor 122 receives a reference signal V REF that is applied to a node 103 . The drain of the transistor 116 is additionally coupled to an output node 110 . The sources of the transistors 120 , 122 are coupled to each other and to the drains of NMOS transistors 124 , 126 such that when the ON-resistance of the transistors 124 , 126 change, subsequently changing the voltage at the sources of the transistors 120 , 122 . Since the amplifier 102 has a topology that is complementary to the topology of the amplifier 101 , the amplifier 102 includes a pair of NMOS transistors 144 , 146 whose gates are coupled to each other and to the drain of the transistor 146 . The sources of the transistors 144 , 146 are coupled to the node 109 to be coupled to GND when the transistor 108 is turned ON. The drains of the transistors 144 , 146 are respectively coupled to the drains of PMOS transistors 140 , 142 . The output node 110 is similarly coupled between the drain of the transistor 144 and the drain of the transistor 140 . Like the transistors 120 , 122 , the input signals to the buffer 100 are received by the gates of the PMOS transistors 140 , 142 . The sources of the transistors 140 , 142 are coupled to the drains of PMOS transistors 132 , 134 . Similarly, the gate of the transistor 132 is coupled to the gates of the transistors 144 , 146 .
The amplifiers 101 , 102 as explained so far are conventional, and they are coupled to each other in a conventional manner. However, in contrast to the prior art, the amplifier 101 includes capacitively coupling the gate of the transistor 120 to the gates of the transistors 116 , 118 , 124 at node 111 , such as by a coupling capacitor 152 . Similarly, the gate of the transistor 140 may be capacitively coupled to the gates of the transistors 132 , 144 , 146 at node 113 . In a similar manner, a coupling capacitor 153 may be used to represent capacitively coupling the node 113 to the gate of the transistor 140 . These capacitors 152 , 153 couple transitions of the input signal V IN to the nodes 111 and 113 , respectively. As explained in greater detail below, this capacitive coupling makes the amplifiers 101 , 102 operate in a substantially symmetrical manner because they mimic the operation of the amplifiers 101 , 102 as if complementary signals were applied to the amplifiers 101 , 102 .
The V DIFF signal may be further refined by propagating the output signal through an output unit 155 coupled to the output node 110 . The output unit 155 may include a series of inverters, 157 A-C, that incrementally condition the voltage V DIFF at each stage to generate a desired output signal V OUT .
As previously described, the V IN signal swings between high and low voltage levels within a particular range for which the input buffer 100 is designed. In operation, when the magnitude of V IN transitions to a voltage level that is lower than the voltage level of the reference voltage V REF , the transistor 120 is turned OFF, and the transistor 140 is turned ON. Turning ON the transistor 140 decreases its ON-resistance to pull the magnitude of a V DIFF signal at the output node 110 towards V CC . Since the source terminals of the transistors 140 , 142 are connected, the gate-to-source voltage of the transistor 142 decreases due to voltage at the source terminal decreasing and the V REF remaining constant, thus the ON-resistance of the transistor 142 increases. Consequently, the voltage at the node 113 decreases. However, due to coupling the V IN signal to the node 113 through the coupling capacitor 153 , the voltage at the node 113 is further decreased responsive to the V IN signal transitioning low, thereby decreasing the ON-resistance of the transistor 132 and increasing the ON-resistance of the transistors 144 , 146 at a faster rate to further pull the output node 110 towards V CC at the faster rate. By coupling a portion of the V IN signal through the capacitor 153 , the voltage node 113 , which responds to the gate-to-source voltage change of the transistor 142 , changes as if the V REF input is transitioning in the opposite direction relative to the transition of the V IN signal. Therefore, the amplifier 102 operates as if it receives complementary input signals despite the V REF input at node 103 remaining constant.
Due to the high ON-resistance of the transistor 120 in the amplifier 101 , the transistor 120 is essentially turned off. Therefore, the source terminal voltages of the transistors 120 , 122 are low since the source terminal of the transistor 122 is coupled to GND through the transistor 126 . Thus the gate-to-source voltage of the transistor 122 is increased to decrease the ON-resistance of the transistor 122 , which is opposite to the increased ON-resistance of the transistor 120 due to V IN transitioning low. Consequently, the magnitude of the voltage at the node 111 decreases and further enables the transistors 116 , 118 while disabling the transistor 124 . As the V IN signal transitions lower, the feedback from the coupling capacitor 152 further drains the node 111 , which decreases the ON-resistance of transistors 116 , 118 at a faster rate. Consequently, the magnitude of the V DIFF signal at the output node 110 is further pulled towards V CC by the amplifier 101 .
The operation of the amplifiers 101 , 102 is opposite to that described operation above when the V IN signal transitions high. As the voltage of V IN increases, the ON-resistance of the transistor 120 in the amplifier 101 decreases and the transistor 140 in the amplifier 102 increases. As the ON-resistance of the transistor 120 decreases, the output node 110 is pulled towards GND, thereby decreasing the magnitude of V DIFF . Consequently, the gate-to-source voltages of the transistors 122 , 142 adjust such that the ON-resistance of the transistor 122 increases and the ON-resistance of the transistor 142 decreases due to the effects of the magnitude of V IN increasing and the V REF remaining constant. In response, the voltage at node 111 increases due to the higher ON-resistance of the transistor 122 . As a result, the node 111 provides a higher gate voltage to the transistors 116 , 118 , 124 . The higher voltage on the gate of transistor 124 decreases its ON-resistance, which further pulls the output node 110 towards GND. However, the higher voltage on the transistors 116 , 118 increase their ON-resistances, which gradually turns them off. Additionally, a portion of the input signal V IN is applied to the node 111 through the capacitor 152 in a manner that mimics a transition of the V REF signal in the opposite direction of the V IN signal, as previously described. Therefore, the amplifier 101 behaves in a symmetrical manner like a conventional differential amplifier. As a result, as the V IN signal transitions high, the voltage at node 111 responds as if the V REF transitions low as V IN transitions high. Therefore, the gate voltages are provided to the transistors 116 , 118 , 124 at a faster rate, which causes the output signal V DIFF to respond faster to the transition of V IN .
Similar to the previous operation, the voltage at node 113 increases due to the lower ON-resistance of the transistor 142 coupling the node 113 (at the drain of the transistor 146 ) to V CC through the transistor 134 . The voltage of node 113 is increased at a faster rate due to the V IN signal been partially fed through the coupling capacitor 153 . Thus the node 113 is driven to a higher voltage at a faster rate, which is applied to the transistors 144 , 146 and 132 . Therefore, the ON-resistance of the transistors 144 , 146 decrease at a faster rate and the ON-resistance of the transistor 132 increases at a faster rate, thereby further driving the output node 110 towards GND. As the input signal V IN transitions high, the amplifiers 101 , 102 operate to drive the V DIFF signal towards GND.
FIG. 2 is a signal diagram comparing an output signal 215 of the prior art buffer without the capacitors 152 , 153 to an output signal 225 of the buffer 100 using the capacitors 152 , 153 . Also shown in FIG. 2 are the input signal V IN and the reference voltage V REF , which are the same for both the prior art buffer and the buffer 100 . In response to the input signal V IN transitioning high at time T 1 , the output signal 225 of the buffer 100 transitions high at a time T 2 after a delay. However, the prior art buffer takes longer to generate its output signal 215 , which transitions high at a time T 3 . The buffer 100 , therefore, has a faster response time 235 than the prior art buffer by a time difference 245 (T 3 −T 2 ) due to the buffer 100 coupling a portion of the input signal V IN to the source/drain of the V REF input transistors 122 , 142 .
The buffer 100 is illustrated in a memory device, such as a synchronous dynamic random access memory (“SDRAM”) device 300 according to embodiments of the invention. The SDRAM device 300 includes an address register 312 that receives either a row address or a column address on an address bus 314 , preferably by coupling address signals corresponding to the addresses though one embodiment of input buffers 316 . The address bus 314 is generally coupled to a memory controller (not shown). Typically, a row address is initially received by the address register 312 and applied to a row address multiplexer 318 . The row address multiplexer 318 couples the row address to a number of components associated with either of two memory banks 320 , 322 depending upon the state of a bank address bit forming part of the row address. Associated with each of the memory banks 320 , 322 is a respective row address latch 326 , which stores the row address, and a row decoder 328 , which applies various signals to its respective array 320 or 322 as a function of the stored row address. The row address multiplexer 318 also couples row addresses to the row address latches 326 for the purpose of refreshing the memory cells in the arrays 320 , 322 . The row addresses are generated for refresh purposes by a refresh counter 330 , which is controlled by a refresh controller 332 .
After the row address has been applied to the address register 312 and stored in one of the row address latches 326 , a column address is applied to the address register 312 and coupled through the input buffers 316 . The address register 312 couples the column address to a column address latch 340 . Depending on the operating mode of the SDRAM 300 , the column address is either coupled through a burst counter 342 to a column address buffer 344 , or to the burst counter 342 which applies a sequence of column addresses to the column address buffer 344 starting at the column address output by the address register 312 . In either case, the column address buffer 344 applies a column address to a column decoder 348 which applies various signals to respective sense amplifiers and associated column circuitry 350 , 352 for the respective arrays 320 , 322 .
Data to be read from one of the arrays 320 , 322 is coupled to the column circuitry 350 , 352 for one of the arrays 320 , 322 , respectively. The data is then coupled through a read data path 354 to a data output register 356 . Data from the data output register 356 is coupled to a data bus 358 through data output buffers 359 . Data to be written to one of the arrays 320 , 322 is coupled from the data bus 358 to a data input register 360 through data input buffers 361 according to an embodiment of the invention. The data input register 360 then couples the write data to the column circuitry 350 , 352 where they are transferred to one of the arrays 320 , 322 , respectively. A mask register 364 may be used to selectively alter the flow of data into and out of the column circuitry 350 , 352 , such as by selectively masking data to be read from the arrays 320 , 322 .
The above-described operation of the SDRAM 300 is controlled by a command decoder 368 responsive to command signals received on a control bus 370 though command input buffers 372 according to an embodiment of the invention. These high level command signals, which are typically generated by a memory controller (not shown), are a clock enable signal CKE*, a clock signal CLK, a chip select signal CS*, a write enable signal WE*, a row address strobe signal RAS*, and a column address strobe signal CAS*, which the “*” designating the signal as active low. Various combinations of these signals are registered as respective commands, such as a read command or a write command. The command decoder 368 generates a sequence of control signals responsive to the command signals to carry out the function (e.g., a read or a write) designated by each of the command signals. These command signals, and the manner in which they accomplish their respective functions, are conventional. Therefore, in the interest of brevity, a further explanation of these control signals will be omitted.
Although, the memory device illustrated in FIG. 3 is a synchronous dynamic random access memory (“SDRAM”) 300 that includes the buffer 100 or a buffer according to another embodiment of the invention, the buffer 100 or other embodiments of a buffer can be used in other types of memory devices, as well as other types of digital devices.
FIG. 4 shows a computer system 400 containing the SDRAM 400 of FIG. 3 . The computer system 400 includes a processor 402 for performing various computing functions, such as executing specific software to perform specific calculations or tasks. The processor 402 includes a processor bus 404 that normally includes an address bus, a control bus, and a data bus. In addition, the computer system 400 includes one or more input devices 414 , such as a keyboard or a mouse, coupled to the processor 402 to allow an operator to interface with the computer system 400 . Typically, the computer system 400 also includes one or more output devices 416 coupled to the processor 402 , such output devices typically being a printer or a video terminal. One or more data storage devices 418 are also typically coupled to the processor 402 to allow the processor 402 to store data in or retrieve data from internal or external storage media (not shown). Examples of typical storage devices 418 include hard and floppy disks, tape cassettes, and compact disk read-only memories (CD-ROMs). The processor 402 is also typically coupled to cache memory 426 , which is usually static random access memory (“SRAM”), and to the SDRAM 100 through a memory controller 430 . The memory controller 430 is coupled to the SDRAM 300 through the normally control bus 370 and the address bus 314 . The data bus 358 is coupled from the SDRAM 300 to the processor bus 404 either directly (as shown), through the memory controller 430 , or by some other means.
From the foregoing it will be appreciated that, although specific embodiments of the invention have been described herein for purposes of illustration, various modifications may be made without deviating from the spirit and scope of the invention. Accordingly, embodiments of the invention are not limited except as by the appended claims. | Embodiments are described including those pertaining to an input buffer having first and second complementary input terminals. One such input buffer has a symmetrical response to a single input signal applied to the first input terminal by mimicking the transition of a signal applied to the second input terminal in the opposite direction. The aforementioned input buffer includes two amplifier circuits structured to be complementary with respect to each other. Each of the amplifier circuits includes a first transistor having a first input node that receives an input signal transitioning across a range of high and low voltage levels, and a second transistor having a second input node that receives a reference signal. The first input node is coupled to the second transistor through a capacitor that charges and discharges the drain of the second transistor responsive to the input signal transitioning to mimic the second input node transitioning in the direction opposite to the transition of the input signal, while the reference signal at the second input node is maintained at a constant voltage level. | 6 |
BACKGROUND OF THE INVENTION
The present invention relates to a connector plug for connecting electronic components. In particular, the present invention relates to an angular connector plug that can be used in connector sockets where a plurality of plug insertion openings are arranged side-by-side.
In general, when a connector plug connected to a connector sockets is unexpectedly pulled out from the connector socket, significant problems such as the loss of transmitted data can occur.
To handle this problem, Japanese Utility Model Laid-Open Publication Number 4-16885 discloses an invention wherein a lock member is disposed on a connector plug. This lock member engages a latch opening of the connector socket, thus preventing the connector plug from being unexpectedly pulled out from the connector socket. With this connector plug, removing the connector plug from the connector socket involves manually operating an unlock ring in order to force the lock member to the unlocked position.
In some connector sockets for audio-visual devices, a connector socket on which is formed a plurality of plug insertion openings is used (for example, to connect a plurality of media devices such as VCRs). This type of connector socket structure, however, has a very large number of connector pins, and the plug insertion openings are spaced very close to each other. Thus, there is insufficient space available for manually operating the unlock ring. Since these connectors cannot be designed as round connector plugs, unlock rings as described above cannot be used.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the present invention to overcome the problems of conventional connector plugs as described above and to provide an angular connector plug that can be used for connector sockets that provide limited space for manual operations and that have a plurality of plug insertion openings with many connector pins.
Briefly stated, the present invention provides a box-shaped main plug unit connected at one end to a cable. A plug of the main plug unit is insertable into plug insertion openings of a connector socket. A lock claw of a lock member is affixed to the main plug unit, and is positioned to lock into a latch opening of the plug insertion openings. A slider is slidably supported on the main plug unit. When the slider is slid on the main plug unit it forcibly disengages the lock claw from the latch opening. A pull-out handle is rotatably supported on the slider. The pull-out handle is rotatable between a protected inoperative position and a projecting operative position where it permits application of removal force on the main plug unit. A fixed projection is integrally formed on the slider to further aid in the application of a pull-out force to the main plug unit.
According to an embodiment of the invention, there is provided an angular connector plug for connection with a connector socket comprising: a main plug unit having an outer shape formed in a box shape, one end of the main plug unit being adapted for connection to a cable, a plug of the main plug unit insertable into a plug insertion opening of the connector socket, a lock claw on the main plug unit, a latch opening in the plug insertion opening, the lock claw engaging the latch opening when the plug is inserted into the plug insertion opening, a slider slidably supported on the main plug unit, a cooperating element between the slider and the lock claw, the cooperating element forcibly disengaging the lock claw and the latch opening in response to sliding of the slider, and a pull-out handle supported by the slider and which can be grasped to apply a pull-out force to the main plug unit, whereby removal of the main plug unit is assisted.
According to a feature of the invention, there is provided a connector plug for connection to a connector socket comprising: a main plug unit, a plug in the main plug unit insertable into the connector socket, a lock claw on the main plug unit, a latch opening on the connector socket, the lock claw engaging the latch opening when the plug is engaged in the connector socket, a slider slidably disposed on the main plug unit, cooperating element in the main plug unit, the cooperating element cooperating with sliding of the slider to disengage the lock claw from the latch opening for permitting unplugging the plug from the connector socket.
In order to achieve this object, the present invention provides an angular connector plug comprising: a main plug unit having an outer shape in the form of a long, thin box and connected on one length-wise end to a cable, a plug of the main plug unit which can be inserted into a plug insertion opening of a connector socket, a locking claw of a locking member that can be locked into a latch opening on the insertion opening of the plug, a slider that is slidably supported by the main plug unit and that makes it possible to manually perform forcible disabling of the lock claw from the latch opening, and a pull-out handle supported by the slider. By grasping the pull-out handle with the fingertips, it is possible to apply a pullout force.
The following preferred embodiments of the present invention will be described.
1) The pull-out handle is formed roughly in the shape of a "C". A support end of the pull-out handle is pivotably supported by a support shaft disposed on the slider, which is formed as a rectangular frame. The pull-out handle can be manipulated so that when it is not being used, it is held within the outer form of the main plug unit, and when the pull-out handle is being used, it is projected out from the main plug unit.
3) A click projection is disposed on either the outer surface of the main plug unit facing the pull-out handle or the pull-out handle. A click groove is disposed on the remaining one of the above two elements. The click projection engages with the click groove so that when the pull-out handle is not being used, it is stored within the outer form of the main plug unit.
4) A finger-operated projection is formed integrally with an outer surface of the slider opposite from the cable. An external force from a fingertip can be applied to the finger-operated projection when pulling out the slider from the connector socket.
The above, and other objects, features and advantages of the present invention will become apparent from the following description read in conjunction with the accompanying drawings, in which like reference numerals designate the same elements.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective drawing of a connector according to an embodiment of the invention showing the relationship between the angular connector plug and the connector socket.
FIG. 2 is a cross-section drawing of the connector socket.
FIG. 3 is a plan drawing of the angular connector plug.
FIG. 4 is a right-side view drawing of the angular connector plug with one portion cut away.
FIG. 5 is a cross-section drawing along the 5--5 line in FIG. 4.
FIG. 6 is a schematic enlarged cross-section drawing along the 6--6 line in FIG. 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 and FIG. 2, an angular connector plug according to the present invention, which will be described in detail below, is used in conjunction with a connector socket A. Connector socket A includes a molded block 1, which is formed by injection molding a synthetic resin. Two plug insertion openings 3A, 3B are formed on the surface of molded block 1. Plug insertion openings 3A and 3B receive plugs b1 of angular connector plugs B1, B2.
In order to shield the inside of connector socket A from external magnetic and electric fields, a shield case 4 formed by bending a thin metal plate into a box shape is used to cover the front surface, the side surfaces, and the upper surface of molded block 1.
A plurality of pin slots 5 is formed at the back of molded block 1 adjacent to each other along the width of molded block 1. A plurality of shared connector pins 6A, 6B are fitted into pin slots 5 using a fitting device (not shown). Shared connector pins 6A, 6B may be formed by any convenient method, but are preferably stamped from a thin metal plate.
The corresponding connection ends in plug insertion openings 3A, 3B perform common functions. Shared connector pins 6A, 6B connect together corresponding pairs of connection ends 6a, 6b, which are arranged adjacent to each other in the same manner as the arrangement of plug insertion openings 3A, 3B. Shared connector pins 6A, 6B each includes a shared section 6c extending vertically along corresponding pin slots 5. The base portions of connection ends 6a, 6b are supported by shared sections 6c in a cantilevered manner at roughly a right angle.
Connection ends 6a, 6b are inserted through openings 7A, 7B, which are formed between plug insertion openings 3A, 3B and pin slots 5. A fitting device is used so that the ends of connection ends 6a, 6b project into corresponding plug insertion openings 3A, 3B.
Latch openings 9A, 9B are formed in plug insertion openings 3A, 3B. A lock claw 8a of a lock member 8 projecting from plug b1 of angular connector plugs B1, B2, drops into latch opening 9A, 9B. Engagement of latch openings 9A, 9B with lock claw 8a of lock member 8 prevents angular connector plugs B1, B2 from unexpectedly slipping out from plug insertion openings 3A, 3B.
Referring to FIG. 3 through FIG. 6, angular connector plugs B1, B2 include a main plug unit 10 formed in a long, thin box shape. Main plug unit 10 includes: a contact block 12; and a shield member 14. Contact block 12 is made from an insulating resin. A plurality of contact openings 11 are formed on contact block 12. Contact openings 11 are arranged at the same pitch used for connection ends 6a, 6b of shared connector pins 6A, 6B. Shield member 14 covers wires k of a cable K that are crimped to contacts 13 of contact block 12. Contact block 12 and shield member 14, which make up plug b1, are covered by a housing cover 15, which forms a section of main plug unit 10. A guide end 15a at one end of housing cover 15 guides cable K to the outside. A clamping ring 16 is fixed to the outer perimeter surface of cable K between guide end 15 and shield member 14, thus preventing cable K from being pulled out from main plug unit 10.
Referring to FIG. 4, an attachment section 8b of lock member 8 is made from a metal plate having resilience. Attachment section 8b is fixed to shield member 14. Lock member 8 includes a projection 8c at its central portion. A lock claw 8a at the end of lock member 8 extends out from plug b1 at a holding groove 17 formed on the outer surface of contact block 12.
A rectangular frame-shaped slider 18 formed on the outer surface of main plug unit 10. Slider 18 is preferably made from resin. This frame-shaped slider 18 is able to move along main plug unit 10 in the direction of insertion of plug b1.
Referring to FIG. 3 and FIG. 6, two pairs of guide projections 19A, 19B are formed integrally on the upper and lower surfaces of housing cover 15. Guide projections 19A, 19B are positioned at slots 20A, 20B of frame-shaped slider 18. Slots 20A, 20B are oriented in the direction of insertion of plug b1.
An opening cam 18a is formed integrally at the opening of frame-shaped slider 18 that faces plug b1. Opening cam 18a can engages projection 8c when assembled as shown in FIG. 4. Displacement of opening cam 18a forces lock member 8 into the deflected position indicated by the dotted line.
The outer end surface of frame-shaped slider 18 opposite the entry of cable K includes an integral finger-operated projection 18b, which can be operated with a finger when necessary. Thus, if angular connector plugs B1, B2 are fixed rigidly in connector socket A, finger-operated projection 18b can be operated with a finger so that angular connector plugs B1, B2 can be pulled out from connector socket A.
A pivot shaft 18c is formed integrally at a central portion along the length of frame-shaped slider 18. Pivot shaft 18c projects in a direction opposite to the inner surface of frame-shaped slider 18. A support terminal 21a is formed in a C-shape on a pull-out handle 21. Support terminal 21a is rotatably supported by pivot shaft 18c. When pull-out handle 21 is at an unused position indicated by the solid line, pull-out handle 21 is held in main plug unit 10 within a cut-out 22 of frame-shaped slider 18. When pull-out to handle 21 is rotated to the position indicated by the dotted line, pull-out handle 21 can move over a wide range behind main plug unit 10 so that pull-out handle 21 can be grasped with the fingers thus allowing an external force to be applied.
Referring to FIG. 6, in order to prevent unexpected rotation of pull-out handle 21, small detent or clicking projections 23 project from sides 21b of pull-out handle 21. Clicking grooves 24 are formed on the outer surface of housing cover 15. Clicking grooves 24 are positioned in the path of clicking projections 23 so that clicking projections 23 can elastically fall into clicking grooves 24. Of course, clicking projections 23 can be formed on the outer surface of housing cover 15. In this case, clicking grooves 24 would be formed on sides 21b of pull-out handle 21.
Since angular connector plugs B1, B2 according to the embodiment shown in the drawings is configured as described above, the restorative force of lock member 8 urges frame-shaped slider 18 toward the position shown in the solid line in FIG. 4. In this state, pull-out handle 21 is in the unused state shown by the solid line and lock claw 8a of lock member 8 projects out from plug b1. When angular connector plugs B1, B2 are firmly pushed into plug insertion openings 3A, 3B of connector socket A, lock claws 8a engage latch openings 9A, 9B of corresponding insertion openings 3A, 3B. As a result, the connection between connector socket A and angular connector plugs B1, B2 is locked in, and angular connector plugs B1, B2 are prevented from being unexpectedly pulled out.
When angular connector plugs B1, B2 are to be pulled out from connector socket A, pull-out handle 21 is lightly pivoted around pivot shaft 18c. This cause clicking projection 23 to disengage from clicking groove 24, thereby moving pull-out handle 21 to its enabled position indicated by the dotted line. The space around this enabled positioned is not obstructed by other angular connector plugs B1, B2, thus allowing pull-out handle 21 to be easily grasped with the fingertips.
Thus, both pull-out handles 21 can be grasped so that angular connector plugs B1, B2 are pulled away from connector socket A. Pull-out handles 21 cause frame-shaped slider 18 to slide against main plug unit 10. Opening cam 18a of frame-shaped slider 18 engages projection 8c of lock member 8.
Referring to FIG. 4, lock member 8 is deformed inward as shown by the dotted lines, and latch claw 8a is moves out of engagement with latch openings 9A, 9B, thus disengaging a locked state between plugs b1 of angular connector plugs B1, B2 and connector socket A. When pull-out handles 21 are pulled out further, plugs b1 are pulled out from plug insertion openings 3A, 3B of connector socket A. However, if there is a strong connection between contact 13 and contact ends 6a, 6b of shared connector pins 6A, 6B, angular connector plugs B1, B2 can be easily pulled out from connector socket A by pressing on finger-operated projection 18b with the fingertip and pulling forward.
Once angular connector plugs B1, B2 have been pulled out, pull-out handle 21 can be released. Due to the restorative force from lock member 8, projections 8c will cause open cam 18a of frame-shaped slider 18 to naturally revert from the position indicated by the dotted line in FIG. 4 to the position indicated by the solid line. In this case, if pull-out handle 21 is returned to the position indicated by the solid line, the clicking projection 23 of pull-out handle 21 again engages clicking groove 24 of housing cover 15, thus preventing pull-out handle 21 from pivoting to a position that is difficult to access.
Thus, with angular connector plugs B1, B2 according to the embodiment shown in the drawings, connection to connector socket A is possible even if plug insertion openings 3A, 3B are close together and space is limited. Furthermore, a structure with a large number of pins is possible. Additionally, to pull out angular connector plugs B1, B2, pull-out handles 21, which are normally held in a stowed position within housing cover 15, are generally displaced to a more open area when necessary. This prevents objects from hitting and destroying pull-out handles 21 when they are not being used, and prevents pull-out handles 21 from obstructing the use of other parts in the surrounding region.
In the embodiment described above, pull-out handle 21 is pivotably supported by frame-shaped slider 18. However, pull-out handle 21 can also be stored in a guide groove formed in frame-shaped slider 18 when not in use and can be pulled outside of housing cover 15 from the guide groove when necessary.
As the description above makes clear, according to the present invention, a cable extends out from one end of a main plug unit shaped as a long, thin box shape. A frame-shaped slider is disposed on the main plug unit to allow lock member manipulation. A pull-out handle, that is generally stowed within the main plug unit, is pulled out when necessary. Thus, there is provided an angular connector plug suited for connector sockets having a plurality of plug insertion openings with many connector pins and having limited space with which to perform manual operations.
One skilled in the art will recognize that, although the above description covers a two-socket device, the same technique is applicable to more or less sockets. For example, a single socket, or three or more sockets may be use the present invention.
Having described preferred embodiments of the invention with reference to the accompanying drawings, it is to be understood that the invention is not limited to those precise embodiments, and that various changes and modifications may be effected therein by one skilled in the art without departing from the scope or spirit of the invention as defined in the appended claims. | A box-shaped main plug unit is connected at one end to a cable. A plug of the main plug unit is insertable into plug insertion openings of a connector socket. A lock claw of a lock member is affixed to the main plug unit, and is positioned to lock into latch openings of the plug insertion openings. A slider is slidably supported on the main plug unit. When the slider is slid on the main plug unit it forcibly disengages the lock claw from the latch opening. A pull-out handle is rotatably supported on the slider. The pull-out handle is rotatable between a protected inoperative position and a projecting operative position where it permits application of removal force on the main plug unit. A fixed projection is integrally formed on the slider to further aid in the application of a pull-out force to the main plug unit. | 7 |
TECHNICAL FIELD
[0001] This invention relates to a technique enabling access to packet-based services, such as IP, Frame Relay, and ATM, through an Ethernet Protocol network.
BACKGROUND ART
[0002] Presently, communication service providers, such as AT&T, offer high-speed data communications service to customers through a variety of access mechanisms. For example, a customer may gain network access through a private line connection, i.e., a direct link to the communications service provider's network. Private line access provides a dedicated port not shared by anyone else with facility bandwidth available exclusively to the particular customer. Unfortunately, private line access is expensive, and is practical only for customers that have very high traffic capacity requirements.
[0003] As an alternative to private line access, communications service providers such as AT&T also offer virtual circuit access allowing several customers to logically share a single circuit, thus reducing costs. Such shared circuits, typically referred to as Permanent Virtual Circuits, allow communication service providers to guarantee customer traffic flows that are distinguishable from each, secure, and allow customers to enjoy different service features. An example of such a technique for offering such shared service in a Multi-Protocol Label Switching Network is disclosed in U.S. Pat. No. 6,081,524, assigned to AT&T.
[0004] Presently, there is a trend towards using Ethernet networks in place of Frame Relay and ATM networks especially for transporting traffic among two or more premises belonging to the same customer. Ethernet-based Metropolitan Area Networks (MANs) currently exist in many areas and offer significant cost advantages on a per port basis, as compared to Frame Relay and ATM service. Transmission speeds as high as 100, 1000 or even 10,000 MB/second are possible with such Ethernet MANs. Moreover, optical Ethernet MANs typically offer a rich set of features, flexible topology and simple-end-to end provisioning.
[0005] Present-day Ethernet-based MANs lack the ability to logically separate traffic received from different customers, giving rise to issues of data security. Moreover, such present day Ethernet-based MANs lack the ability to manage bandwidth among customers, thus preventing the network from regulating customer traffic to assure equitable access. Thus, there is a need for a technique for routing data in an Ethernet protocol network that overcomes the aforementioned disadvantages.
BRIEF SUMMARY OF THE INVENTION
[0006] Briefly, in accordance with a preferred embodiment, a method is provided for routing data in an Ethernet protocol network having a plurality of platforms, each serving one or more customers. A first platform receives at least one frame from a sending site (e.g., a first customer's premises) that is destined for a receiving site (e.g., another premises belonging to the same or a different customer.) After receiving the frame, the first platform overwrites a portion of the frame with a customer descriptor that specifically identifies the sending customer. In practice, the first platform will overwrite a Virtual Local Area Network (VLAN) field that is typically employed by the sending customer for the purposes of routing data among various VLANs at the sending premises premises. Rather than overwrite the VLAN field in the frame, the first platform could overwrite another field, such as the source address field, or could even employ a “shim” header containing the customer descriptor. All further use of the term customer descriptor implies that any of the above or similar techniques could be used.
[0007] After overwriting the frame with the customer descriptor, the sending platform routes the frame onto the MAN network for routing among the other platforms, thereby sharing trunk bandwidth and other resources, but logically distinct from other customer's traffic with different customer descriptors. A destination address in the frame directs the frame to its corresponding receiving platform. Upon receipt of the frame, the receiving platform uses the customer descriptor to segregate the frame for delivery to the proper destination, especially in the event where different customers served by the same platform use overlapping addressing plans. Thus, the customer descriptor in each frame advantageously enables the receiving platform to distinguish between different customers served by that platform.
[0008] For traffic with a destination beyond the MAN, this method provides a convenient and efficient way to map the customer-descriptor to similar identifiers in a Wide Area Network (WAN), such as a Permanent Virtual Circuit (PVC), a Virtual Private Network (VPN), or an MPLS Label Switched Circuit.
[0009] Overwriting each frame with the customer-descriptor thus affords the ability to logically segregate traffic on the Ethernet MAN to provide Virtual Private Network (VPN) services of the type offered only on more expensive Frame Relay and ATM networks. Moreover, the customer descriptor used to tag each frame can advantageously include Quality of Service (QoS) information, allowing the sender to specify different QoS levels for different traffic types, based on the Service Level Agreement (SLA) between the customer and the communications service provider.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] [0010]FIG. 1 depicts an Ethernet Protocol Metropolitan Area Network (MAN) in which each information frame is tagged with a customer descriptor in its VLAN field in accordance with the present principles;
[0011] [0011]FIG. 2 illustrates a sample information frame for transmission over the network of FIG. 1;
[0012] [0012]FIG. 3 illustrates a portion of the MAN showing the various stages in the tagging process;
[0013] [0013]FIG. 4 illustrates a portion of a MAN showing the use of the priority bits within the VLAN field to establish different Quality of Service levels;
[0014] [0014]FIG. 5 illustrates a portion of a MAN showing the manner in which information frames are mapped to different Permanent Virtual Circuits by an ATM switch;
[0015] [0015]FIG. 6 illustrates a portion of a MAN showing the manner in which information frames are mapped into different Multi-Protocol Label Switching (MPLS) tunnels; and
[0016] [0016]FIG. 7 illustrates a portion of a MAN showing the manner in which information frames are mapped into different service networks.
DETAILED DESCRIPTION
[0017] [0017]FIG. 1 depicts an Ethernet Protocol Metropolitan Area Network (MAN) 10 comprised of a plurality of Multi-Service Platforms (MSPs) 12 1 - 12 n where n is an integer, each MSP taking the form of an Ethernet switch or the like. In the illustrated embodiment n=4 although the network 10 could include a smaller or larger number of MSPs. A fiber ring or SONET ring infrastructure 14 connects the platforms 12 1 - 12 4 in daisy-chain fashion allowing each MSP to statistically multiplex information onto, and to statistically de-multiplexing information off the ring infrastructure 14 .
[0018] Each of MSPs 12 1 - 12 3 serves at least one, and in some instances, a plurality of premises 16 belonging to one or more customers. In the illustrated embodiment of FIG. 1, the MSP 12 1 serves a single customer premises 16 1 belonging to customer 1 whereas, the MSP 12 2 serves premises 16 2 , and 16 3 belonging to customers 2 and 3 , respectively. The MSP 12 3 serves a single premises 16 4 that belongs to customer 3 . The MSPs 12 1 - 13 3 are linked to their corresponding premises via 10, 100 or 1000 MB links 18 . The MSP 12 4 bears the legend “CO MSP” because it serves as a central office to route traffic from the MAN 10 to a Provider Edge Router (PER) 18 for delivery to other networks, such as Frame Relay, ATM, MPLS networks or the Internet as discussed hereinafter. By the same token, the PER 18 can route traffic from such other networks onto the MAN 10 via the CO MSP 12 4
[0019] The traffic routed onto and off of the MAN 10 by each MSP takes the form of one or more information frames 20 depicted in FIG. 2. Heretofore, traffic routed onto the network 10 from a particular customer's premises was combined with other customer's traffic with no logical separation, thus raising security concerns. Moreover, since all customers' traffic share the same bandwidth, difficulties existed in prior art Ethernet MANs in regulating the traffic from each customer's premises, and in affording different customers different Quality of Service (QoS) level in accordance with individual Service Level Agreements.
[0020] These difficulties are overcome in accordance with the present principles by “tagging” each frame 20 routed onto the network 10 at a particular MSP, say MSP 12 3 , with a customer descriptor 22 ′ (best seen in FIG. 2) that identifies the customer sending that frame. As discussed in greater detail below, each MSP receiving a frame 20 on the fiber ring infrastructure 14 uses the customer descriptor 22 ′ in that frame to maintain distinct routing and addressing tables that are assigned to each customer served by that MSP. This permits each customer to use their own addressing plan without fear of overlap with other customers, as they are all maintained as logically separate.
[0021] [0021]FIG. 2 depicts the structure of an exemplary Ethernet protocol frame 20 specified by Ethernet Standard 802.1Q. Among the blocks of bytes within each frame 20 is a Virtual Local Area Network (VLAN) Identifier 22 comprised of sixteen bits. In practice, the VLAN identifier 22 , in conjunction with a VLAN flag block 23 within the frame, facilitates routing of the frame within a customer's premises to a particular VLAN. However, the VLAN identifier 22 has no influence on routing of the frame 20 after receipt at a MSP.
[0022] In accordance with the present principles, the prior disadvantages associated with conventional Ethernet networks, namely the lack of security and inability to regulate QoS levels, are overcome by overwriting the VLAN identifier 22 in each frame 20 with the customer descriptor maintained by the service provider. Overwriting the VLAN identifier 22 of FIG. 2 of each frame 20 with the customer descriptor 22 ′ serves to “tag” that frame with identity of its sending customer identity, thus affording each MSP in the network 10 the ability to route those frames only among the premises belonging to that same sending customer. Such tagging affords the operator of the network 10 the ability to provide security in connection with frames transmitted across the network, since frames with customer ID A would not be delivered to any premises of customer with ID B. As an example, two or more customers served by a single MSP may use overlapping IP addressing schemes. In the absence of any other identifier, the MSP receiving such frame lacks the ability to assure accurate delivery.
[0023] In the illustrated embodiment depicted in FIG. 2, each MSP of FIG. 1 tags the frame 20 by overwriting the VLAN identifier 22 with the customer descriptor 22 ′. However, tagging could occur in other ways, rather than overwriting the VLAN identifier 22 . For example, the source address block 25 within the frame 20 could be overwritten with the customer descriptor 22 ′. Alternatively, the data field 25 could include a shim header comprising the customer descriptor 22 ′.
[0024] The tagging of each frame 20 with the customer descriptor 22 ′ affords several distinct advantages in connection with routing of the frames through the MAN. First, as discussed above, the tagging affords each recipient MSP the ability to distinguish traffic destined for customers with overlapping address schemes, and thus allows for segregating traffic on the MAN. Further, tagging each frame 20 with the customer descriptor 22 ′ enables mapping of the frames from a MAN 100 depicted in FIG. 3 to corresponding one of a plurality of customer Virtual Private Networks 26 1 - 26 3 within an MPLS network 28 . As seen in FIG. 3, an MSP 120 2 within the MAN 100 receives traffic from premises 160 1 , 160 2 , and 160 3 belonging to customer 1 , customer 2 and customer 3 , respectively, which enjoy separate physical links to the MSP. Upon receipt of each from a particular customer, the MSP 120 2 overwrites that frame with the customer descriptor corresponding to the sending customer.
[0025] After tagging each data frame, the MSP 120 2 statistically multiplexes the frames onto the fiber ring infrastructure 14 for transmission to a CO MSP 120 4 for receipt at a destination PER 180 that serves the MPLS network 28 within which are customer Virtual Private Networks 26 1 - 26 3 . Using the customer descriptor in each frame, the PER 180 maps the frame to the corresponding VPN identifier associated with a particular one of customer Virtual Private Networks 26 1 - 26 3 to properly route each frame to its intended destination.
[0026] The tagging scheme of the present invention also affords the ability to route information frames with different QoS levels within a MAN 1000 depicted in FIG. 4. As seen in FIG. 4, an MSP 1200 2 within the MAN 1000 receives traffic from premises 1600 2 , and 1600 3 belonging to customer 2 and customer 3 , respectively, which enjoy separate physical links to the MSP, allowing each to send information frames into the MAN. In the illustrated embodiment of FIG. 4, the frames originating from the premise 1600 2 may contain either voice or data and have corresponding QoS level associated with each type of frame. Upon receiving such frames, the MSP 1200 2 overwrites the frame with the customer descriptor corresponding to the particular customer sending the frame. The customer descriptor will not only contain the identity of the sending customer, but the corresponding QoS level associated with that frame.
[0027] After tagging each data frame, the MSP 1200 2 statistically multiplexes the frames onto the fiber ring infrastructure 14 for transmission to a CO MSP 1200 4 for receipt at a destination PER 1800 that serves an MPLS network 280 within which are customer Virtual Private Networks 260 2 and 260 3 . Using the customer descriptor in each frame, the PER 1800 of FIG. 4 maps the frame to the corresponding customer VPN to properly route each frame to its intended customer premises. Further, the PER 1800 of FIG. 4 also maps the QoS level specified in the customer descriptor in the frame to assure that the appropriate quality of service level is applied to the particular frame.
[0028] In the above-described embodiments, the frames of customer traffic have been assumed to comprise IP packets that terminate on a router (i.e., Provider Edge Routers 18 , 180 and 1800 ) and that the VPNs employ MPLS-BGP protocols. However, some customers may require multi-protocol support, or may otherwise require conventional PVCs so that the traffic streams must be mapped into Frame Relay or ATM PVCs as depicted in FIG. 5, which illustrates a portion of a MAN 10000 having a CO MSP 12000 4 serving an ATM switch 30 that receives traffic from the MAN. As seen in FIG. 5, each of premises 16000 1 , 16000 2 and 16000 3 belonging to customer 1 , customer 2 and customer 3 , respectively 5 may originate information frames for receipt at MSP 12000 2 in the MAN 10000 . The MSP 12000 2 tags each frame with the corresponding customer descriptor prior to statistically multiplexing the data for transmission on the fiber ring infrastructure 14 to the CO MSP 12000 4 for receipt at the ATM switch 30 . The ATM switch 30 then maps the frame to the appropriate PVC in accordance with the customer descriptor in the frame in a manner similar to the mapping described with respect to FIG. 3. Thus, the ATM switch 30 could map the frame to one of Frame Relay recipients' 32 1 , 32 2 , or 32 3 , ATM recipients 32 4 or 32 5 or IMA (Inverse Multiplexing over ATM) recipient 32 6 .
[0029] [0029]FIG. 6 depicts a portion of a MAN network 100000 that routes frames onto separate MPLS tunnels 40 1 - 40 3 (each emulating a private line 32 in an MPLS network 2800 ) in accordance with the customer descriptor written into each frame by a MSP 120000 2 in the MAN. Each of customer premises 160000 1 , 160000 2 and 160000 3 depicted in FIG. 6 originate information frames for receipt at MSP 120000 2 . The MSP 120000 2 tags each frame with the customer descriptor prior to statistically multiplexing the data for transmission on the fiber ring infrastructure 14 for delivery to a CO MSP 120000 4 that serves a PER 18000 . The PER 18000 translates the customer descriptors written onto the frames by the MSP 120000 2 into the MPLS tunnels 40 1 - 40 3 to enable the PER to route the traffic to the intended customer.
[0030] [0030]FIG. 7 depicts a portion of a MAN network 1000000 for routing traffic (i.e., information frames) onto separate networks in accordance with the customer descriptor written into each the frame by a MSP 120000 2 in the MAN. Each of customer premises 1600000 2 and 16000003 depicted in FIG. 7 originates information frames for receipt by the MSP 1200000 2 . The MSP 1200000 2 tags each frame with the customer descriptor prior to statistically multiplexing the data for transmission on the fiber ring infrastructure 14 for delivery to a CO MSP 1200000 4 that serves a PER 180000 . In accordance with the customer descriptor, the PER 1800000 of FIG. 7 routes traffic to a particular one of several different networks, e.g., an Intranet VPN 42 1 , a voice network 42 2 and the Internet 42 3 , in accordance with the customer descriptor written onto the frame by the MSP 12 2 .
[0031] The above-described embodiments merely illustrate the principles of the invention. Those skilled in the art may make various modifications and changes that will embody the principles of the invention and fall within the spirit and scope thereof. descriptor, the PER 1800000 of FIG. 7 routes traffic to a particular one of several different networks, e.g., an Intranet VPN 42 1 , a voice network 42 2 and the Internet 42 3 , in accordance with the customer descriptor 22 ′ written onto the frame by the MSP 1200000 2 . | An Ethernet Metropolitan Area Network ( 10 ) provides connectivity to one or more customer premises ( 16 1 , 16 2 , 16 3 ) to packet-bases services, such as ATM, Frame Relay, or IP while advantageously providing a mechanism for assuring security and regulation of customer traffic. Upon receipt of each customer-generated information frame ( 20 ), an ingress Multi-Service Platform (MSP) ( 12 2 ) “tags” the frame with a customer descriptor ( 22 ′) that specifically identifies the recipient customer. In practice, the MSP tags each frame by overwriting the Virtual Local Area Network (VLAN) identifier ( 22 ) with the routing descriptor. Using the customer descriptor in each frame, a recipient Provider Edge Router (PER) ( 18 ) or ATM switch can map the information as appropriate to direct the information to the specific customer. In addition, the customer descriptor ( 22 ′) may also include Quality of Service (QoS) allowing the recipient Provider Edge Router (PER) ( 18 ) or ATM switch to vary the QoS level accordingly. | 7 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation application of International Application No. PCT/JP2015/003018, filed Jun. 17, 2015, which claims the benefit of Japanese Patent Application No. 2014-136718, filed Jul. 2, 2014. The contents of the aforementioned applications are incorporated herein by reference in their entireties.
TECHNICAL FIELD
[0002] The present invention relates to an optical communication method and an optical communication system for transmitting and receiving information by using photons.
BACKGROUND ART
[0003] In recent years, research and experiments have been made on quantum cryptography communication utilizing principles of quantum mechanics (Non Patent Documents 1 and 2). In the conventional quantum cryptography communication, studies have been made assuming that a photon in superposed states in the quantum mechanics exists in a communication path. When the photon in the superposed states is observed by an eavesdropper, the photon transitions from the superposed states to an eigenstate having definite information. Due to such an effect, the eavesdropper cannot perform eavesdropping without affecting the exchanged information, because the eavesdropper cannot reproduce the original superposed states. Hence, the fact that the proper sender and recipient can detect eavesdropping guarantees security.
[0004] For example, Non Patent Document 3 discloses an optical communication method for a quantum cryptography communication. In the optical communication method described in Non Patent Document 3, a sender phase-modulates a photon according to information desired to be transmitted and transmits the photon to a recipient. If an eavesdropper exists in a transmission pass and measures the photon, the eavesdropper may fail to retransmit a photon modulated by the same phase modulation because the eavesdropper cannot know the phase used by the sender. As a result, mismatch (error) between the information transmitted by the sender and the information received by the recipient increases and the existence of the eavesdropper can be thereby detected.
CITATION LIST
Non Patent Document
[0000]
Non Patent Document 1: H. Takesue et al., “Differential phase shift quantum key distribution experiment over 105 km fibre”, New Journal of Physics, 2005, Vol. 7, 232
Non Patent Document 2: H. Goto, “Mechanism and development trends of quantum cryptography communication”, Kinyu Kenkyu, 2009, 28(3), pp. 107-150, Institute for Monetary and Economic Studies, Bank of Japan
Non Patent Document 3: K. Inoue, “Quantum Key Distribution Technologies”, IEEE Journal of Selected Topics in Quantum Electronics, 2006, Vol. 12 (4), pp. 888-896
Non Patent Document 4: M. Morimoto, “Resolution of Single Photon and Electron Interference Enigma”, http://vixra.org/abs/1312.0097, 2013
SUMMARY OF INVENTION
[0009] The conventional optical communication method described above even enables detection of the existence of the eavesdropper after the eavesdropping, but still allows the eavesdropper to measure the photon exchanged in the communication path. When the existence of the eavesdropper is detected, the conventional optical communication method can take a countermeasure against the eavesdropping, such as destroying information (for example, encryption key) on a photon which may have been maliciously measured. However, it is undeniable that the conventional optical communication method allows the photon to give some information to the eavesdropper. Accordingly, it is more preferable to make it more difficult for the eavesdropper to measure the photon from the beginning.
[0010] The present invention has been made in view of the problems described above, and an object thereof is to provide an optical communication method and an optical communication system in which eavesdropping is more difficult than in conventional techniques.
[0011] A first aspect of the present invention is an optical communication system comprising: a photon pair generator which generates a correlated photon pair; a polarizer which is provided on an optical path of one photon of the correlated photon pair and direction of which is changeable based on information to be transmitted; a shutter which is provided between the photon pair generator and the polarizer on the optical path of the one photon of the correlated photon pair and which is capable of blocking the one photon of the correlated photon pair; and a photon detector which is provided on an optical path of another photon of the correlated photon pair.
[0012] A second aspect of the present invention is an optical communication method comprising: setting a direction of a polarizer based on information to be transmitted; generating a correlated photon pair with a photon pair generator after the direction of the polarizer is set; blocking one photon of the correlated photon pair with a shutter after the correlated photon pair is generated; and detecting another photon of the correlated photon pair with a detector after the correlated photon pair is generated, wherein the shutter and the polarizer are arranged on an optical path of the one photon of the correlated photon pair, and the detector is arranged on an optical path of the another photon of the correlated photon pair.
[0013] In the optical communication method and the optical communication system of the present invention, since the information is transmitted based on the direction of the polarizer and the one photon of the correlated photon pair is blocked by the shutter, it is difficult to perform eavesdropping by reading the photon.
BRIEF DESCRIPTION OF DRAWINGS
[0014] FIG. 1 is a schematic configuration diagram of an optical communication system in one embodiment of the present invention.
[0015] FIG. 2 is a view depicting a flowchart of an optical communication method in one embodiment of the present invention.
[0016] FIG. 3A is a view depicting a schematic plot of a result measured by the optical communication method in one embodiment of the present invention.
[0017] FIG. 3B is a view depicting a schematic plot of a result measured by the optical communication method in one embodiment of the present invention.
[0018] FIG. 4 is a schematic configuration diagram of an optical communication system in one embodiment of the present invention.
[0019] FIG. 5 is a view depicting a flowchart of an optical communication method in one embodiment of the present invention.
DESCRIPTION OF EMBODIMENTS
[0020] Embodiments of the present invention are described below with reference to the drawings. However, the present invention is not limited to the embodiments. Note that, in the drawings described below, parts with the same function are denoted by the same reference numeral and overlapping description thereof is omitted in some cases.
First Embodiment
[0021] FIG. 1 is a schematic configuration diagram of an optical communication system 100 in the embodiment. The optical communication system 100 includes a receiver 110 and a transmitter 120 , and the receiver 110 and the transmitter 120 are connected to each other by a communication path 130 which is a transmission path of information. Although the communication path 130 is a free space in the embodiment, the communication path 130 may at least partially be an optical waveguide such as an optical fiber or a PLC. Note that the names of the receiver 110 and the transmitter 120 are defined based on a direction in which the information is transmitted, and are opposite to a direction in which photons are transmitted as will be described later. Specifically, the transmission direction of the information is a direction from the transmitter 120 to the receiver 110 , but the transmission direction of the photons is a direction from the receiver 110 to the transmitter 120 .
[0022] In the receiver 110 , there are provided a photon source 111 which outputs photons according to control of a reception controller 119 and a photon pair generator 112 which generates correlated photon pairs by receiving photons from the photon source 111 . One photon of each photon pair is referred to as photon p, and the other photon is referred to as photon s. The photon p and the photon s are correlated to each other to have polarizations orthogonal to each other. Specifically, when the photon p is a vertically-polarized photon, the photon s is a horizontally-polarized photon or vise versa. In the embodiment, a BBO crystal (β-BaB 2 O 4 crystal) which generates pairs of photons correlated to each other by means of parametric down-conversion is used as the photon pair generator 112 . However, any material or device which generates pairs of photons correlated to each other can be used.
[0023] Two QWPs 113 a and 113 b (quarter wave plates) and a double slit plate 114 are provided corresponding to a direction in which the photons s are emitted by the photon pair generator 112 , that is, are provided on an optical path of the photons s. The double slit plate 114 has two slits parallel to each other. The first QWP 113 a is arranged such that the photons s having passed the first QWP 113 a enter one of the two slits, and the second QWP 113 b is arranged such that the photons s having passed the second QWP 113 b enter the other one of the two slits.
[0024] When the linearly-polarized photons s enter the QWPs 113 a and 113 b at an angle of −45° or 45° with respect to the fast axes of the QWPs 113 a and 113 b (the polarization of the photons s in this case is assumed to be diagonal polarization), the QWPs 113 a and 113 b convert the photons s to a circularly-polarized photons and output the converted photons s. Meanwhile, when the linearly-polarized photons s enter the QWPs 113 a and 113 b at an angle of 0° or 90° with respect to the fast axes of the QWPs 113 a and 113 b (the polarization of the photons s in this case is assumed to be vertical polarization or horizontal polarization), the QWPs 113 a and 113 b output the photons s as they are as linearly-polarized photons. Moreover, the directions in which the respective QWPs 113 a and 113 b convert the photons s to circularly-polarized photons are opposite to each other. Specifically, the first QWP 113 a converts the photons s to right circularly-polarized photons while the second QWP 113 b converts the photons s to left circularly-polarized photons (or vise versa). In such a configuration, when the vertically-polarized or horizontally-polarized photons s enter the QWPs 113 a and 113 b , interference occurs after the photons s pass through the double slit plate 114 . Meanwhile, when the diagonally-polarized photons s enter the QWPs 113 a and 113 b , no interference occurs after the photons s pass through the double slit plate 114 .
[0025] A slit plate 115 and a reception detector 116 are provided on a path of the photons s having passed the double slit plate 114 , that is, are provided on the optical path of the photons s. The slit plate 115 has a slit which allows the photons s to enter the reception detector 116 only in a predetermined direction.
[0026] The reception detector 116 outputs a predetermined signal to the reception controller 119 upon detecting the photons s. Although an APD (avalanche photodiode) is used as the reception detector 116 in the embodiment, any device capable of detecting photons can be used. A driver 117 which moves the reception detector 116 in a direction perpendicular to the direction in which the photons s are emitted by the photon pair generator 112 (optical path of the photons s) is connected to the reception detector 116 . The driver 117 is any driver such as a motor or an actuator. By repeating the detection of the photons s while moving the reception detector 116 with the driver 117 , the number of photons s detected by the reception detector 116 at each position can be obtained.
[0027] A shutter 118 is provided corresponding to a direction in which the photons p are emitted by the photon pair generator 112 , that is, is provided on an optical path of the photons p. The shutter 118 is switchable between an open state in which the photons p are allowed to pass and travel toward the communication path 130 and a closed state in which the photons p are blocked and prevented from traveling toward the communication path 130 , according to the control of the reception controller 119 . Any device which can be mechanically or electromagnetically switched between the open state and the closed state can be used as the shutter 118 .
[0028] The reception controller 119 is connected to the photon source 111 , the reception detector 116 , and the shutter 118 . The reception controller 119 electrically controls the members, communicates with the transmitter 120 via a synchronization transmission path 140 , records measured data, and performs input and output for the user. The reception controller 119 includes any computer or electric circuit.
[0029] In the transmitter 120 , a polarizer 121 (polarization plate) is provided corresponding to the direction in which the photons p from the receiver 110 enter, that is, is provided on the optical path of the photons p. The polarizer 121 is switchable between a first state in which the polarizer 121 allows photons having polarization in a predetermined direction to completely pass and a second state in which the direction to allow the photons to pass is rotated by +45° or −45° from that of the first state. In the embodiment, since the vertical polarization or the horizontal polarization is used as the polarization in the predetermined direction, the polarizer 121 in the first state allows the vertically-polarized or horizontally-polarized photons to pass while the polarizer 121 in the second state allows the diagonally-polarized photons to pass. The polarizer 121 is switchable between the first state and the second state according to the control by a transmission controller 122 .
[0030] A slit plate 123 and a transmission detector 124 are provided on a path of the photons p having passed the polarizer 121 . The slit plate 123 has a slit which allows the photons p to enter the transmission detector 124 only in a predetermined direction. The transmission detector 124 outputs a predetermined signal to the transmission controller 122 upon detecting the photons p. Note that, in the embodiment, since the information is transmitted from the transmitter 120 to the receiver 110 based on the direction of the polarizer 121 as will be described below, the transmission detector 124 is not necessarily required for the information transmission. The transmission detector 124 is used to align the optical axis of the communication path 130 between the transmitter 120 and the receiver 110 or to measure the distance between the transmitter 120 and the receiver 110 by receiving photons from the receiver 110 .
[0031] The transmission controller 122 is connected to the polarizer 121 and the transmission detector 124 . The transmission controller 122 electrically controls the members, communicates with the receiver 110 via the synchronization transmission path 140 , records measured data, and performs input and output for the user. The transmission controller 122 includes any computer or electric circuit.
[0032] The receiver 110 and the transmitter 120 are connected to each other by the synchronization transmission path 140 . The synchronization transmission path 140 may be any communication path such as an optical fiber communication path, a radio communication path, and the like. The transmission controller 122 transmits a synchronization signal to the reception controller 119 via the synchronization transmission path 140 to perform transmission-reception timing synchronization. The transmission-reception timing synchronization is performed by means of any synchronization method by using a signal indicating a transmission time, a periodic signal, and the like.
[0033] Principles of the present invention are described. It has been conventionally considered that: in a correlated photon pair (entangled photon pair) generated by a BBO crystal (photon pair generator), when one photon s has the vertical polarization |y>, the other photon p has the horizontal polarization |x> or vise versa; and these polarization directions are not determined until the photons are observed and the photons are in the superposed states. Specifically, it has been considered that the correlated photon pair is in a superposition of a state |y>s|x>p in which the photon s has the vertical polarization |y> and the photon p has the horizontal polarization |x> and a state |x>s|y>p in which the photon s has the horizontal polarization |x> and the photon p has the vertical polarization |y>. This state is expressed by formula (1).
[0000]
[
Math
1
]
|
Ψ
〉
=
1
2
(
|
x
〉
s
|
y
〉
p
+
|
y
〉
s
|
x
〉
p
)
(
1
)
[0034] However, in this concept, a paradox in which time seems to be reversed occurs and a special situation such as a situation in which cause and effect are switched occurs. Meanwhile, explanation can be made without using the conventional concept by accepting existence of a non-localized potential as described below.
[0035] Specifically, the horizontal polarization |x> and the vertical polarization |y> of the photons having passed a device, which allows only specific polarization to pass, such as the polarizer have been conventionally considered to be in a superposition of polarization rotated by +45° or −45° as expressed by formula (2).
[0000]
[
Math
2
]
|
x
〉
=
1
2
|
+
〉
+
1
2
|
-
〉
|
y
〉
=
1
2
|
+
〉
-
1
2
|
-
〉
(
2
)
[0036] In this formula, |+> represents polarization of +45° with respect to the x axis, and |−> represents polarization of −45° with respect to the x axis. Although this is correct in a classical electromagnetic field, applying this expression to a photon which cannot be divided such as a single photon leads to paradox. In the case of dealing with a very small number of photons as described above, such a situation can be explained well by using the non-localized potential which universally exists in a space, instead of considering such a situation as superposition. In this case, formula (3) in which a non-localized potential |ζ> is added to formula (2) needs to be considered as a correct expression.
[0000]
[
Math
3
]
|
x
〉
→
|
x
〉
+
|
ζ
1
〉
=
1
2
|
+
〉
+
1
2
|
-
〉
|
y
〉
→
|
y
〉
+
|
ζ
2
〉
=
1
2
|
+
〉
-
1
2
|
-
〉
(
3
)
[0037] Therefore, the non-localized potential |ζ> is expressed by formula (4).
[0000]
[
Math
4
]
|
ζ
1
〉
=
1
2
|
+
〉
+
1
2
|
-
〉
-
|
x
〉
|
ζ
2
〉
=
1
2
|
+
〉
-
1
2
|
-
〉
-
|
y
〉
(
4
)
[0038] In this formula, the letters attached to the non-localized potential |ζ> each represent the direction of the polarizer (polarizer 121 in the optical communication system 100 ), |ζ 1 > represents the horizontal direction, and |ζ 2 > represents the vertical direction. As described above, the direction of the non-localized potential |ζ> is determined by the existence of the polarizer. Specifically, the non-localized potential is |ζ 1 > when the direction of the polarizer is horizontal and the non-localized potential is |ζ 2 > when the direction of the polarizer is vertical.
[0039] Since the non-localized potential |ζ> follows the Maxwell's equations, the non-localized potential |ζ> propagates from the polarizer at the speed of light. When the propagated non-localized potential |ζ> reaches the BBO crystal (photon pair generator 112 in the optical communication system 100 ) which generates the photon pairs, the polarization of the photons which can be generated by the BBO crystal is determined by this non-localized potential |ζ> whose direction is determined.
[0040] Specifically, before the BBO crystal generates photons, the non-localized potential |ζ> reaches the BBO crystal from the polarizer existing in the direction in which the photons are to be emitted from the BBO crystal. When the direction of the polarizer is horizontal, the non-localized potential |ζ 1 > reaches the BBO crystal. Accordingly, the BBO crystal can generate only the photons p having the horizontal polarization |x> in the direction toward the polarizer. In this case, the other photons s of the correlated photon pairs have the vertical polarization |y>. Meanwhile, when the direction of the polarizer is vertical, the non-localized potential |ζ 2 > reaches the BBO crystal. Accordingly, the BBO crystal can generate only the photons p having the vertical polarization |y> in the direction toward the polarizer. In this case, the other photons s of the correlated photon pairs have the horizontal polarization |x>. As described above, the polarization of the photons which can be generated by the BBO crystal is restricted by the direction of the polarizer existing in the direction in which the photons are to be emitted from the BBO crystal. Note that, although description is given of the vertical polarization and the horizontal polarization, the polarization of the photons which can be generated by the BBO crystal is restricted by the direction of the polarizer in a similar way also in the diagonal polarization rotated by +45° or −45° from the vertical polarization or the horizontal polarization.
[0041] In other words, in the BBO crystal, the completely-correlated photon pair is generated from the beginning, and the correlated photon pair before being observed is not in the superposed states as in the conventional concept. However, since the non-localized potential itself cannot be observed and such determination of the direction cannot therefore be sensed, it has been conventionally considered that there is a strange correlation in the photon pairs.
[0042] Since probability amplitudes of the non-localized potential are <ζ 1 |ζ 1 >=0 and <ζ 2 |ζ 2 >=0, it can be seen that the non-localized potential cannot be observed. This can be easily derived by multiplying formula (4) as it is and by using the relationship of formula (5).
[0000] 1/√{square root over (2)}= x|+ = +|x = y|+ = +|y
[0000] = x|− = −|x =− y|− =− −|y (5)
[0043] In summary, the correlated photon pair generated by the BBO crystal has the complete correlation in which, when one photon has the vertical polarization |y>, the other photon has the horizontal polarization |x> (or vise versa). However, these directions of polarization are determined when the photon pair is generated, irrespective of whether the observation is performed or not, and the correlated photon pair is not in the superposed states as in the conventional concept. The non-localized potential |ζ> whose direction is determined determines the directions of polarization upon reaching the BBO crystal before the generation of the photon pairs.
[0044] FIG. 2 is a view depicting a flowchart of an optical communication method using the optical communication system 100 . First, in the state where the shutter 118 is open, the transmission controller 122 sets the direction of the polarizer 121 based on the information to be transmitted (step S 101 ). In the embodiment, in the case of transmitting “1” as first information, the polarizer 121 is set to the first state in which the vertically-polarized or horizontally-polarized photons are allowed to completely pass. Meanwhile, in the case of transmitting “0” as second information, the polarizer 121 is set to the second state in which the direction to allow the photons to pass is rotated by +45° or −45° from that of the first state. The direction of polarization allowed to pass in the first state may be set to a direction other than the horizontal polarization or the vertical polarization. Moreover, “0” and “1” which are the information to be transmitted may be opposite. In such a case, the receiver 110 may be configured such that definitions of relationships between the directions of polarization and the information to be transmitted are appropriately changed.
[0045] Next, the reception controller 119 generates photons from the photon source 111 (step S 102 ). A timing at which the photons are generated from the photon source 111 is set such that the photons from the photon source 111 reaches the photon pair generator 112 after the non-localized potential from the polarizer 121 reaches the photon pair generator 112 . Specifically, assume that a time point at which the direction of the polarizer 121 is set is t 1 , a time required for the non-localized potential from the polarizer 121 to reach the photon pair generator 112 is a, and a time required for the photons from the photon source 111 to reach the photon pair generator 112 is b. In this case, a time point t 2 at which the photons are generated from the photon source 111 is expressed by formula (6).
[0000] [Math 6]
[0000] t 2 >t 1 +a−b (6)
[0046] Since the non-localized potential and the photons travel at the speed of light, the times a and b can be calculated from the distances between the members. The time point t 1 at which the direction of the polarizer 121 is set is determined based on the synchronization signal received from the transmission controller 122 via the synchronization transmission path 140 .
[0047] Upon receiving the photons from the photon source 111 , the photon pair generator 112 generates the photons p and s which are the correlated photon pairs (step S 103 ). At this point, since the non-localized potential from the polarizer 121 has already reached the photon pair generator 112 , the polarization directions of the photons p and s are determined by the non-localized potential. Specifically, when the polarizer 121 is in the first state in which the vertically-polarized or horizontally-polarized photons are allowed to completely pass, the photons p traveling from the photon pair generator 112 toward the polarizer 121 are the vertically-polarized or horizontally-polarized photons, and the other photons s are also the vertically-polarized or horizontally-polarized photons. Meanwhile, when the polarizer 121 is in the second state in which the direction to allow the photons to pass is rotated by +45° or −45° from that of the first state and the diagonally-polarized photons are allowed to pass, the photons p traveling from the photon pair generator 112 toward the polarizer 121 are the diagonally-polarized photons and the other photons s are also the diagonally-polarized photons.
[0048] Next, the reception controller 119 closes the shutter 118 (step S 104 ). A timing at which the shutter 118 is closed is a timing after the photons p and s are generated in the photon pair generator 112 and before the photons p reach the shutter 118 . Specifically, assume that a time required to generate the photons p and s in the photon pair generator 112 is c and a time required for the photons p from the photon pair generator 112 to reach the shutter 118 is d. In this case, a time point t 3 at which the shutter 118 is closed is expressed by formula (7). Since the photons travel at the speed of light, the times c and d can be calculated from the distances between the members.
[0000] [Math 7]
[0000] t 2 +b+c<t 3 <t 2 +b+c+d (7)
[0049] In parallel with step S 104 , the reception detector 116 detects the photons s having passed through the QWPs 113 a and 113 b and the double slit plate 114 and records whether the photons s are detected or not in the reception controller 119 (step S 105 ). Thereafter, the reception controller 119 opens the shutter 118 (step S 106 ).
[0050] In the embodiment, in order to determine the transmitted information (direction of the polarizer 121 ) from whether interference occurs or not in a measurement result, the detection needs to be performed at multiple measurement positions and performed multiple times at each measurement position. To achieve this, the driver 117 moves the reception detector 116 by a predetermined distance (step S 107 ) and steps S 102 to S 106 are repeated predetermined times at each measurement position (step S 108 ), without the direction of the polarizer 121 being changed. For example, steps S 102 to S 107 are performed 50 times at each of 20 positions (total of 1000 times).
[0051] Lastly, the reception controller 119 determines the transmitted information by plotting a photon detection number measured at each measurement position (step S 109 ). Specifically, when the occurrence of interference is recognized in the plot, the photons s before entering the QWPs 113 a and 113 b are the vertically-polarized or horizontally-polarized photons, and the other photons p are therefore also the vertically-polarized or horizontally-polarized photons. From this, it is found that the polarizer 121 on the optical path of the photons p is in the first state in which the vertically-polarized or horizontally-polarized photons are allowed to completely pass. Hence, the reception controller 119 determines that the information transmitted from the transmitter 120 is “1” which is the first information. Meanwhile, when no occurrence of interference is recognized in the plot, the photons s before entering the QWPs 113 a and 113 b are the diagonally-polarized photons, and the other photons p are therefore also the diagonally-polarized photons. From this, it is found that the polarizer 121 on the optical path of the photons p is in the second state in which the direction to allow the photons to pass is rotated by +45° or −45° from that of the first state. Hence, the reception controller 119 determines that the information transmitted from the transmitter 120 is “0” which is the second information.
[0052] FIGS. 3A and 3B are views depicting schematic plots of results measured by the reception detector 116 . When the plot has a mountain shape with one peak as illustrated in FIG. 3A , no interference is occurring. Accordingly, the photons s before entering the QWPs 113 a and 113 b are the diagonally-polarized photons. Meanwhile, when the plot has a wave shape with multiple peaks as illustrated in FIG. 3B , interference is occurring. Accordingly, the photons s before entering the QWPs 113 a and 113 b are the vertically-polarized or horizontally-polarized photons. Such determination can be performed by the reception controller 119 or by the user.
[0053] In the optical communication system 100 of the embodiment, the information is transmitted by utilizing the fact that the non-localized potential which cannot be observed is sent from the transmitter 120 to the receiver 110 and the polarization of the photons which can be generated in the photon pair generator 112 is restricted by the non-localized potential. Although the receiver 110 and the transmitter 120 of the optical communication system 100 are arranged at positions capable of transmitting and receiving the photons, the shutter 118 blocks the photons before the photons are actually emitted from the receiver 110 to the transmitter 120 . Accordingly, an eavesdropper cannot intercept the exchanged photons and read information. Moreover, since no observable photons travel through the transmission path of the information from the transmitter 120 to the receiver 110 , it is difficult for the eavesdropper to know the transmission path.
Second Embodiment
[0054] In the optical communication system 100 of the first embodiment, the information is statistically determined by utilizing the existence or absence of interference. Accordingly, transmission needs to be performed multiple times for one piece of information (“1” or “0”). Meanwhile, in the embodiment, information can be determined by performing transmission once for one piece of information.
[0055] FIG. 4 is a schematic configuration diagram of an optical communication system 200 of the embodiment. The optical communication system 200 includes a receiver 210 and a transmitter 220 , and the receiver 210 and the transmitter 220 are connected to each other by a communication path 230 which is a transmission path of information. Although the communication path 230 is a free space in the embodiment, the communication path 230 may at least partially be an optical waveguide such as an optical fiber or a PLC.
[0056] In the receiver 210 , there are provided a photon source 211 which outputs photons according to control of a reception controller 219 and a photon pair generator 212 which generates correlated photon pairs by receiving photons from the photon source 211 . One photon of each photon pair is referred to as photon p, and the other photon is referred to as photon s. The photon p and the photon s are correlated to each other to have polarizations orthogonal to each other. Specifically, when the photon p is a vertically-polarized photon, the photon s is a horizontally-polarized photon or vise versa. In the embodiment, a BBO crystal (β-BaB 2 O 4 crystal) which generates pairs of photons correlated to each other by means of photometric down-conversion is used as the photon pair generator 212 . However, any material or device which generates pairs of photons correlated to each other can be used.
[0057] A second shutter 213 and a second polarizer 214 (polarization plate) are provided corresponding to a direction in which the photons s are emitted by the photon pair generator 212 , that is, are provided on an optical path of the photons s. The second shutter 213 is switchable between an open state in which the photons s are allowed to pass and travel toward the second polarizer 214 and a closed state in which the photons s are blocked and prevented from traveling toward the second polarizer 214 , according to the control of the reception controller 219 . Any device which can be mechanically or electromagnetically switched between the open state and the closed state can be used as the second shutter 213 .
[0058] The second polarizer 214 allows photons having polarization of a predetermined direction to pass and does not allow photons having polarization of directions other than the predetermined direction to pass. In the embodiment, since the horizontal polarization is used as the polarization of the predetermined direction, the second polarizer 214 allows the photons s to pass when the photons s are horizontally-polarized and does not allow photons s to pass when the photons s are polarized in other directions, that is, vertically-polarized or diagonally-polarized.
[0059] A slit plate 215 and a reception detector 216 are provided on a path of the photons s having passed the second polarizer 214 . The slit plate 215 has a slit which allows the photons s enter the reception detector 216 only in a predetermined direction.
[0060] The reception detector 216 outputs a predetermined signal to the reception controller 219 upon detecting the photons s. Although an APD (avalanche photodiode) is used as the reception detector 216 in the embodiment, any device capable of detecting photons can be used.
[0061] A first shutter 218 is provided corresponding to a direction in which the photons p are emitted by the photon pair generator 212 , that is, is provided on an optical path of the photons p. The first shutter 218 is switchable between an open state in which the photons p are allowed to pass and travel toward the communication path 230 and a closed state in which the photons p are blocked and prevented from traveling toward the communication path 230 , according to the control of the reception controller 219 . Any device which can be mechanically or electromagnetically switched between the open state and the closed state can be used as the first shutter 218 .
[0062] The reception controller 219 is connected to the photon source 211 , the reception detector 216 , the first shutter 218 , and the second shutter 213 . The reception controller 219 electrically controls the members, communicates with the transmitter 220 via a synchronization transmission path 240 , records measured data, and performs input and output for the user. The reception controller 219 includes any computer or electric circuit.
[0063] In the transmitter 220 , a first polarizer 221 (polarization plate) is provided corresponding to the direction in which the photons p from the receiver 210 enter, that is, is provided on the optical path of the photons p. The first polarizer 221 is switchable between a first state in which the first polarizer 221 allows photons having polarization in a predetermined direction to completely pass and a second state in which the direction to allow the photons to pass is rotated by a predetermined angle (for example, +90° or −90°) from that of the first state. In the embodiment, since the vertical polarization is used as the polarization in the predetermined direction, the polarizer 221 in the first state allows the vertically-polarized photons to pass while the polarizer 221 in the second state allows the horizontally-polarized photons to pass. The first polarizer 221 is switchable between the first state and the second state according to the control by a transmission controller 222 .
[0064] A slit plate 223 and a transmission detector 224 are provided on a path of the photons p having passed the first polarizer 221 . The slit plate 223 has a slit which allows the photons p to enter the transmission detector 224 only in a predetermined direction. The transmission detector 224 outputs a predetermined signal to the transmission controller 222 upon detecting the photons p. Note that, in the embodiment, since the information is transmitted from the transmitter 220 to the receiver 210 based on the direction of the first polarizer 221 as in the first embodiment, the transmission detector 224 is not necessarily required for the information transmission. The transmission detector 224 is used to align the optical axis of the communication path 230 between the transmitter 220 and the receiver 210 or to measure the distance between the transmitter 220 and the receiver 210 by receiving photons from the receiver 210 .
[0065] The transmission controller 222 is connected to the first polarizer 221 and the transmission detector 224 . The transmission controller 222 electrically controls the members, communicates with the receiver 210 via the synchronization transmission path 240 , records measured data, and performs input and output for the user. The transmission controller 222 includes any computer or electric circuit.
[0066] The receiver 210 and the transmitter 220 are connected to each other by the synchronization transmission path 240 . The synchronization transmission path 240 may be any communication path such as an optical fiber communication path, a radio communication path, and the like. The transmission controller 222 transmits a synchronization signal to the reception controller 219 via the synchronization transmission path 240 to perform transmission-reception timing synchronization. The transmission-reception timing synchronization is performed by means of any synchronization method by using a signal indicating a transmission time, a periodic signal, and the like.
[0067] FIG. 5 is a view depicting a flowchart of an optical communication method using the optical communication system 200 . First, in the state where the second shutter 213 is closed and the first shutter 218 is open, the transmission controller 222 sets the direction of the first polarizer 221 based on the information to be transmitted (step S 201 ). In the embodiment, in the case of transmitting “1” as first information, the first polarizer 221 is set to the first state in which the vertically-polarized photons are allowed to completely pass. Meanwhile, in the case of transmitting “0” as second information, the first polarizer 221 is set to the second state in which the direction to allow the photons to pass is rotated by the predetermined angle (for example, +90° or −90°) from that of the first state. The direction of polarization allowed to pass in the first state may be set to a direction other than the vertical polarization. Moreover, “0” and “1” which are the information to be transmitted may be opposite. In such cases, the receiver 210 may be configured such that definitions of relationships between the directions of polarization and the information to be transmitted are appropriately changed.
[0068] Next, the reception controller 219 generates photons from the photon source 211 (step S 202 ). A timing at which the photons are generated from the photon source 211 is set such that the photons from the photon source 211 reaches the photon pair generator 212 after the non-localized potential from the first polarizer 221 reaches the photon pair generator 212 . This timing can be calculated by using formula (6) as in the first embodiment.
[0069] Upon receiving the photons from the photon source 211 , the photon pair generator 212 generates the photons p and s which are the correlated photon pairs (step S 203 ). At this point, since the non-localized potential from the first polarizer 221 has already reached the photon pair generator 212 , the polarization directions of the photons p and s are determined by the non-localized potential. Specifically, when the first polarizer 221 is in the first state in which the vertically-polarized photons are allowed to completely pass, the photons p traveling from the photon pair generator 212 toward the first polarizer 221 are the vertically-polarized photons, and the other photons s are the horizontally-polarized photons. Meanwhile, when the first polarizer 221 is in the second state in which the direction to allow the photons to pass is rotated by the predetermined angle (+90° or −90° in this case) from that of the first state and the horizontally-polarized photons are allowed to pass, the photons p traveling from the photon pair generator 212 toward the first polarizer 221 are the horizontally-polarized photons and the other photons s are the vertically-polarized photons.
[0070] Next, the reception controller 219 closes the first shutter 218 (step S 204 ). A timing at which the first shutter 218 is closed is a timing after the photons p and s are generated in the photon pair generator 212 and before the photons p reach the first shutter 218 . This timing can be calculated by using formula (7) as in the first embodiment.
[0071] In parallel with step S 204 , the reception controller 219 opens the second shutter 213 (step S 205 ). A timing at which the second shutter 213 is opened is a timing after the photons p and s are generated in the photon pair generator 212 and before the photons s reach the second shutter 213 . Specifically, assume that a time required for the photons s from the photon pair generator 212 to reach the second shutter 213 is e, in addition to t 2 , b, and c used in formulae (6) and (7). In this case, a time point t 4 at which the second shutter 213 is opened is expressed by formula (8). Since the photons travel at the speed of light, the time e can be calculated from the distances between the members.
[0000] t 2 +b+c<t 4 <t 2 +b+c+e (8)
[0072] The reception detector 216 detects the photons s having passed through the second polarizer 214 and records whether the photons s are detected or not in the reception controller 219 (step S 206 ). Thereafter, the reception controller 219 opens the first shutter 218 and closes the second shutter 213 (step S 207 ).
[0073] Lastly, the reception controller 219 determines the transmitted information by using a result measured by the reception detector 216 (step S 208 ). Specifically, when the photons are detected by the reception detector 216 , the photons s before entering the second polarizer 214 are horizontally-polarized photons, and the other photons p are therefore vertically-polarized photons. From this, it is found that the first polarizer 221 on the optical path of the photons p is in the first state in which the vertically-polarized photons are allowed to completely pass. Hence, the reception controller 219 determines that the information transmitted from the transmitter 220 is “1” which is the first information. Meanwhile, when no photons are detected by the reception detector 216 , the photons s before entering the second polarizer 214 are not the horizontally-polarized photons, and the other photons p are therefore the horizontally-polarized photons. From this, it is found that the first polarizer 221 on the optical path of the photons p is in the second state in which the direction to allow the photons to pass is rotated by the predetermined angle from that of the first state. Hence, the reception controller 219 determines that the information transmitted from the transmitter 220 is “0” which is the second information.
[0074] The optical communication system 200 in the embodiment has effects of the first embodiment and can also transmit one piece of information by performing transmission once. Accordingly, the optical communication system 200 can further increase the transmission speed.
[0075] The present invention is not limited to the embodiments described above, and appropriate changes can be made within a scope not departing from the purport of the present invention.
[0076] In this description, the present invention is described by using words such as vertical polarization, horizontal polarization, and diagonal polarization as the polarization of photons. However, the polarization in the present invention is not limited to polarization of specific directions. In the case of carrying out the present invention, polarization of other directions may be used based on the symmetry of polarization. In the case of using the polarization of other directions, the statements of the description may be replaced as appropriate. | The present invention provides an optical communication method and an optical communication system in which eavesdropping is more difficult than in conventional techniques. An optical communication system in one embodiment of the present invention comprises: a photon pair generator which generates a correlated photon pair; a polarizer which is provided on an optical path of one photon of the correlated photon pair and direction of which is changeable based on information to be transmitted; a shutter which is provided between the photon pair generator and the polarizer on the optical path of the one photon of the correlated photon pair and which is capable of blocking the one photon of the correlated photon pair; and a photon detector which is provided on an optical path of another photon of the correlated photon pair. | 7 |
FIELD OF THE INVENTION
The present inventions concerns a coupling or connecting device between the suspension of a front wheel and the suspension of a rear wheel of a wheeled vehicle such as a motorcycle, in which the suspension deflections are transformed into substantially axial displacements of a support of at least one suspension spring such as a helical spring.
BACKGROUND OF THE INVENTION
In the field of suspension of automobile vehicles, it is known to obtain a connection between the right side and the left side of the vehicle, generally by means of using a torsion bar often called "antiroll bar", so that overloading that occurs on one side of the vehicle can be partially supported by the other side of the vehicle. It is thus obtained, by means of a slight stiffening of the suspension, improved riding qualities of the vehicle, particularly in the case of lateral overloading and an improved dynamic aspect of the vehicle of which the body thus remains substantially parallel to the ground even on sloped surfaces, that correspondingly reduces risks of overturning and rolling. On the other hand, it is sought to reduce the pitch of the vehicles which is apparent from oscillations from front to rear and vice versa, especially by a dipping of the front during braking. This dipping of the front is particularly troublesome on motorcycles where it is known as "jump" or "bow". Its reduction can be carried out by a mechanical connection between the front and rear suspensions gears of the vehicle that are relatively far apart from each other.
In order to obtain the connection between the front and rear suspensions, it has already been proposed to assemble the front and rear suspensions in a single housing and to have them compressed by means of links mechanically connected to suspension arms of the wheels, but this compact and advantageous disposition of the front and rear suspension springs does not produce an effective connection for correcting the rolling or "jumping or bowing" movements of the vehicle.
SUMMARY OF THE INVENTION
One of the aims of the present invention is to connect the suspension of the front wheel of a vehicle such as a motorcycle achieved by means of a suspension arm and a suspension spring such as a compressed helical spring, to the rear suspension of the same type of vehicle so that an overloading on the front wheel is practically distributed between the front wheel and the rear wheel and vice versa.
With this purpose, the connecting device between the front and rear suspension gear comprises on each front and rear side of the vehicle a push-rod or equivalent one end of which is hinged near the abutment of the suspension spring while the other end is hinged to an arm of rotary resilient connecting member between the front and rear suspension gears of the vehicle, each push-rod being connected to the corresponding arm in a direction opposite to the other push-rod, so that, with respect to a pre-adjusted situation for distributing the compressions of the front and rear suspension gears of the vehicle, an overloading on the front wheel with respect to the pre-adjusted situation is partially supported, through the rotary connecting member, by the rear wheel and vice versa for an overload on the rear wheel or for a reduction of the load supported by one of the suspension gears.
The resilient rotary connecting member is preferably a torsion bar mounted rotary-wise on at least one bearing carried by the vehicle and each end of which is connected at least in rotation to the arm hinged to one of the push-rods which is itself hinged near the abutment of the respectively front or rear suspension spring.
According to another embodiment, the length of at least one of the push-rods or equivalent is adjustable under load so as to allow to modify the pre-adjustment of the compression of the front suspension and the rear suspension gears.
When at least one of the suspension springs is constituted by a helical spring compressed on an annular bracket by a movable plate connected to a compression rod through-crossing the helical spring and the movable plate in a substantially axial manner, the push-rod or equivalent cooperating with the suspension spring is hinged to a tip fixed to the end of the compression rod after its passage through the movable plate. The tip is thus preferably fixed to the end of the compression rod by adjustable screwing in a threaded boring of this tip on an end thread of the compression rod. The end thread of the compression rod is intended to be simultaneously utilized for adjusting the position of the tip on which is hinged the push-rod or equivalent and for adjusting the movable compression plate of the suspension spring.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features, advantages and objects of the invention will become more apparent from reading the following embodiment, given by way of non-limitative illustration and with reference to the appended drawings in which:
FIG. 1 is a schematic representation in perspective of the resilient connecting device between a front suspension and a rear suspension of a vehicle;
FIG. 2 is a side view in elevation of a motorcycle utilizing the rotary connecting device according to the invention between the suspension gear of the rear wheel and that of the front wheel.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The device for connecting the front and rear suspension gears represented in FIG. 1 proposes connecting the active portion of the front suspension constituted by a helical compression spring 1 held pressed between a movable plate 2 and a support collar 3 hinged to the vehicle by a support lug 4 with the active portion of the rear suspension gear similarly constituted by a helical compression spring 5 held pressed between a movable plate 6 and a support collar 7 connected by a support lug 8 to the vehicle chassis. Movable plates 2 and 6 are connected by compression rods 9 and 10, levers or other suspension members that provoke a traction on these rods as a function of the suspension loads, said traction being constantly balanced by the reaction force of the corresponding helical spring 1 or 5 through the intermediary of corresponding movable plate 2 or 6. Rods 9 and 10 extend corresponding support collars 3 or 7 that act as a bearing for them as well as the corresponding helical spring 1 and 5, and movable plate 2 or 6 to which they are connected by a nut 11 or 12 screwed upon a threaded end portion 13 or 14 of rod 9 or 10.
According to the invention, the connecting device is constituted by a torsion bar 15, the axis of which is substantially perpendicular to that of rods 9 and 10 and which is rotatably mounted in bearings 16 and 17 integral with the vehicle chassis (not represented). At each end of torsion bar 15 are provided arms 18 and 19 allowing to apply thereto a torsion moment. Arm 18, the deflection plane of which is situated in the vicinity of the axis of rod 9, is connected thereto by a push-rod 20, one end of which is fixed or hinged to rod 9 through the intermediary of adjustable bolts 21, whereas the other end is hinged to arm 19 by an axis of articulation 22. Arm 19, the deflection plane of which is situated at a distance from the axis of compression spring 10, is connected thereto by a curved extension 23 acting as a flexible push-rod and one end of which is fixed by adjustable nuts 24 to the threaded portion 14 of rod 10.
The functioning of the suspension connecting device represented at FIG. 1 will now be explained. It will be supposed that the front suspension gear has been subjected to an overloading, due for example, to a brake application. Rod 9 undergoes a supplementary traction that compresses spring 1 and displaces nuts 21 toward the left-hand side of the figure thereby extending a force through the intermediary of push-rod 20 on the axis of articulation 22. Arm 18 thus turns in a counter clockwise direction and drives torsion bar 15 in rotation in such direction.
Through the rotation of torsion bar 15 and lever arm 19 which is connected to it, rod 10 of the rear suspension gear is pushed towards the right-hand side of the figure and movable plate 6 connected to rod 10 compresses helical spring 5 of the rear suspension gear while no supplementary load issuing from the vehicle is applied to this spring 5 which is, on the contrary, rather an overload of the load applied to the front through the consecutive deceleration upon braking of the vehicle. The rear suspension spring 5 thus reacts to the urging of torsion bar 15 through a reaction force that subjects torsion bar 15 to a torsion moment so that a part of the overloading applied to the front suspension gear of the vehicle is thus supported by the rear suspension spring which is compressed. The coupling device according to the invention finally produces a stiffening of the front suspension gear subjected to an overloading when the rear suspension is not subjected to the same overloading, thereby preventing an exaggerated compression of the front with respect to the rear. In the case of front outload or rear overcharge with respect to the front, a similar compensating phenomenon is produced between the front and the rear suspension gears.
The motorcycle represented in FIG. 2 presents a motor driving assembly 26 with exhaust pipes 27 mounted on top and a handlebar 28, the assembly being extended by a front plate 29 on which is hinged main arm 30 of the front suspension gear. An upper arm 31 hinged to the motor driving assembly 26 cooperates with main arm 30 in order to support on fulcrums (only upper fulcrum 32 is represented) an inclined pivoting axis of a fulcrum bracket 33 of axle 34 of front wheel 35 the orientation of which is controlled by a push-rod 36 connected by cardan shafts to handlebar 28.
The connection between main arm 30 and front suspension spring 37 is achieved by means of a series of push-rods and levers the functions of which are described in a copending patent application of the applicant of the present application.
Spring 37 is mounted on a shock-absorbing body 38 hinged by a collar 39 on the small lower arm 40 of a three-arm lever 41 hinged at 42 on an extension of front plate 29. A long arm 43 of lever 41 is connected by a push-rod 44 to a hinging plate 45 mounted at the end of a sliding rod 46 that crosses through shock-absorber body 38. Hinging plate 45 is connected by a push-rod 47 to the main arm 30 and by a push-rod 48 to a support block 49 of front brake linings. As explained with reference to FIG. 1, the through-crossing bears at its right end on the figure a movable plate 50 that maintains front suspension spring 37 compressed on collar 39 and the medium arm of the three-arm lever 41 is connected by a rod 41a to a nose 30a of the main arm 30. Rod 46 comprises at its right-hand end a threaded portion on which is adjustably fixed plate 50 by means of adjusting screws 51 and the threaded portion protrudes towards the right-hand side in order to receive a hinging head 52 on which is hinged the end of an inclined coupling rod 53 that is hingedly fixed at its other end to the end of a lever arm 54 towards the top of this figure and mounted at the end of a torsion bar 55 mounted in bearings transversely to the longitudinal axle of the motorcycle and shown in end view in FIG. 2.
At its other end, torsion bar 55 is integral with a lever arm 56 directed towards the bottom of the figure and towards the ground and itself hingedly connected through a curved arm 57 to a hinging head 58 fixed to the left end of a through-crossing rod 59 identical to or of the same type as through-crossing rod 46 utilized for the suspension of the front wheel. Rear helical suspension spring 60 is mounted similarly to front suspension spring 37 and its connection with rear suspension arm 61 that carries rear wheel 62 will not be described in detail. It will be noted that coupling rod 53 is made of two parts, assembled by an adjustable thread with a blocking screw 63 so that it is possible to vary the length of rod 53.
The working of the motorcycle suspension represented in FIG. 2 will now be described. It is first of all necessary to specify that rear and front spring-shock-absorber blocks 38, 64 remain substantially horizontal during displacements of the suspension gear that they control, only rods 46 and 59 and movable plates 50 and 65 being displaced in order to cause to vary the axial compression of the helical suspension springs 37 and 60 and to cause to displace the internal pistons (not represented) of the shock-absorbers.
The front and rear suspensions are represented in position of normal load with the driver riding the motorcyle. It is supposed that the driver initiates a rough brake application on the motorcycle. The vehicle load is thus partially transferred onto the front wheel due to the deceleration that follows braking and spring 37 tends to be more compressed, thereby provoking the displacement towards the left-hand side of the figure of rod 46 and hinging head 52 and tends to cause lever arm 54 to turn in the trigonometric direction.
Torsion bar 55 resiliently drives opposite lever arm 56 in rotation in the same direction, thereby compressing spring 60 which had the tendency to unload due to the load transfer onto the front. Under the supplementary reaction effect to rear suspension spring 60, torsion bar 55 is partially twisted so that only a part of the front overload is transmitted to the rear, thereby nervertheless preventing the shifting of the motorcycle towards the front during braking, typically known as "jump or bow" or at least considerably reduces it.
In the opposite case, for example, at the reacceleration that follows a braking, front wheel 35 is unloaded of part of its load and movable plate 50 is displaced towards the right-hand side of the figure with hinging head 52, thereby tending to cause to turn lever arm 54 in clock-wise direction. Lever arm 56 turns in the same direction and curved arm 57 thus drives rod 59 towards the left-hand side of FIG. 2 and also unloads the rear suspension. Front unloading is thus limited and the rider maintains a good direction adherence on the front wheel during sudden reaccelerations. It is seen that the coupling according to the invention between the front and rear suspension gears efficiently hinders the development of compression dissymmetries between the front and rear suspension gears, this prevention even being able to be effective in the case where one of the suspension gears tends to accidentally fall out, for example, following break of one of suspension springs 37 and 60.
The coupling that has been proposed in FIGS. 1 and 2 by means of rods, of levers and of a torsion bar can be achieved, where necessary, by other means such as cable and sheath systems (bowden cable). Similarly it is understood that helical suspension springs 37 and 60 can be disposed according to other orientations, for example, according to vertical or inclined axes, provided that their inclination veries only slightly during displacements of the suspension. By modifiying the length of rod 53 by means of corresponding screwing when the front and rear suspension gears are loaded, the balance point between the front and rear suspension loads is modified and it is thus possible to correct the loaded seat of the vehicle while ensuring a good coupling between the front and the rear.
It will be well understood that the present invention is in no way limited to the embodiments described and represented herein-above and can be adapted to numerous variants available to the man skilled in the art, without departing front the scope and spirit of the invention. | Coupling device between the suspension gear of a front wheel and the suspension gear of a rear wheel of a wheeled vehicle such as a motorcycle, in which the suspension deflections are transformed into substantially axial deplacements, comprising on each front and rear side of the vehicle a push-rod or equivalent hinged to the abutment of the suspension spring whereas its other end is hinged to an arm of a resilient rotary coupling member such as a torsion bar, this device being applied to the transfer of front and rear overloads of a vehicle. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation of International Application No. PCT/EP2013/054708 filed Mar. 8, 2013, which claims the benefit of U.S. Provisional Application Ser. No. 61/614,040, filed Mar. 22, 2012 and claims benefit under 35 U.S.C. §119(a) of German Patent Application No. 10 2012 005 658.3, filed Mar. 22, 2012, the entire contents of all of which are incorporated herein by reference.
BACKGROUND
1. Field of the Disclosure
The invention relates to an arrangement for generating in particular white light using blue light and a converter for converting blue light into yellow light and by combining these spectral components.
2. Description of Related Art
Such white light generating arrangements are widely known such as, for example, those disclosed in: WO 2004/105647A1, JP 2009105125, U.S. Pat. No. 7,654,712 B2, U.S. 2007/189352A1, U.S. Pat. No. 7,758,224 B2, U.S. Pat. No. 7,433,115 B2, U.S. Pat. No. 7,356,054 B2, and DE 10 2010 028949. The ratio of the blue light component to the yellow light component in the illumination light generated depends on the conversion medium which converts the blue light incident from an excitation light source into yellow light as a component of the illuminating light. In order to arrive in the white region of the chromaticity diagram, various parameters of the converter must be met precisely, including the doping of the converter material, light scattering in the converter material, and the thickness of the converter. Only with a precise adjustment of such parameters it is possible to achieve the correct spectral ratio of blue to yellow light so as to obtain white light.
SUMMARY
The invention is based on the object to provide an arrangement for adjusting the color location of light, which allows for greater tolerances in material parameters such as thickness of the converter, doping of the converter material, light scattering in the converter, and which allows for use of converter materials in which the white spectral region cannot be achieved by conversion alone.
Specifically, an excitation light source for blue light is provided, and a converter for converting substantially all the entering blue light into yellow light. A support or carrier aligns the surface of the converter relative to the excitation light source and in the direction of illumination, in a remission geometry. In order to convert, in the converter, substantially all blue light that enters into yellow light, the thickness of the converter is chosen appropriately large. For adjusting, in the chromaticity diagram, the desired color location which results from a combination of the converted and unconverted light, the surface of the converter is provided with an optical coating. In this manner, white light can be mixed from reflected blue light and remitted yellow light irrespectively of the material parameters of the converter.
In order to obtain an appropriate mixing ratio between blue and yellow light, the optical coating may have a reflection factor in a range from R=0.1 to R=0.3 for incident light of a wavelength in a range from 430 to 460 mm, and a reflection factor of R<0.05, more preferably R<0.01, for exiting converted light of a wavelength in a range from 480 to 650 nm. Thus, in this embodiment of the invention, 70% to 90% of the blue light will enter the converter, where it is virtually completely converted into yellow light (and heat). The optical coating is, however, capable of substantially completely transmitting the converted light, so that the yellow light generated will form a component of the emitted illumination light, which will appear white because of the combination of blue and yellow. A dichroic layer or a thin metallic layer may be used as the optical coating.
However, it is also possible to work with a scattering layer, for example a thin paint coat. Usually, an advantage of such a layer is that the portion of excitation light which is reflected, is not reflected specularly but diffusely, i.e. is backscattered. In this manner, the angular distribution of the reflected excitation light better combines with the converted light. If, however, separation of the two light components is not disadvantageous in the optical system, or is even desirable, specular reflection at a dichroic or metallic layer may be favorable as well. If, when using a scattering layer, specular reflection at the interface to the optically denser medium of the converter is absolutely undesirable, for example because the specular portion would produce undesirable optical effects or because the fraction of converted light is to be increased without reducing the fraction of scattered light, an anti-reflection layer (R<0.05, more preferably R<0.01) for the excitation light and the converted light is applied to the converter first, and thereupon the scattering layer.
By virtue of the scattering layer, also light exiting from the converter is inevitably backscattered into the converter. However, since the absorption length for the converted light in the converter is long, most of the backscattered light will again leave the converter.
The layer composition and the thickness of the optical coating is used as a regulator for adjusting the ratio of entering light to the reflected blue light.
The specific value of the reflection factor R in the application will depend on the wavelength of the excitation light and the spectrum of the converted light and the efficiency of the converter.
The object of the invention may also be solved without an optical coating on the surface of the converter, by taking into account the refractive index of the converter medium in determining the appropriate angle of the excitation light source relative to the surface of the converter. When light is incident on the surface of the converter at an oblique angle, then a portion will be reflected and another portion will enter the converter medium. The entering fraction of the excitation light is almost completely converted into yellow light and leaves the converter in the illumination direction, according to a remission geometry, where it combines with the reflected blue light from the excitation light source to ultimately produce a white light appearance.
Further details of the invention will become apparent from the description of exemplary embodiments, from the drawings and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view through a converter having a dichroic surface layer, and a support of the converter;
FIG. 2 is a sectional view through another converter having a thin metallic surface layer, and a support of the converter; and
FIG. 3 is a sectional view through another converter.
DETAILED DESCRIPTION
FIG. 1 schematically illustrates an arrangement for generating white light, which comprises an excitation light source for blue light 1 , e.g. a diode laser, and a converter 2 which has a coating 3 on its surface and which is attached on a carrier or support 4 . The converter material may be a Ce:YAG ceramic material. Coating 3 is an optical coating for which a dichroic layer or a thin metallic layer is employed. Coating 3 divides the excitation light beam into a portion of reflected light and a portion of entering light. For the purpose of defining these fractions of light, an angle of the incident light to the surface of the converter is usually adjusted to be unequal to 90°. The entering blue light 1 is converted into yellow light 6 by the converter 2 , and this the more, the more deeply the light penetrates into the converter, and is output as a light lobe, not shown. A conversion point is indicated at 60 . From there, the converted light propagates in all directions. According to the invention, the thickness (d) of the converter is selected to have at least a dimension so that substantially all the light that enters the converter is converted.
The carrier or support 4 is configured to be reflective, in order to reflect the entering blue light 1 and especially converted yellow light, which is illustrated at 7 . Due to the reflectivity of the carrier or support 4 , converter material may be economized.
The proportion of reflected blue light is determined through the composition and layer thickness of coating 3 . The reflected light is illustrated at 5 , and the emitted yellow light at 6 . The blue and yellow light combine to produce white light in the illumination direction of the arrangement.
Coating 3 is an optical coating whose configuration additionally depends on the refractive index of the conversion medium, in order to reflect or to transmit the proper fraction at the proper angle. Optical coating 3 has a pre-selectable reflection factor in the blue light spectrum ranging from 430 to 460 nm, in order to achieve the desired result of white light by combination with the emitted yellow component of the light. An appropriate value for the reflection factor is R=0.2. The reflection factor of the optical coating also depends on the angle of incidence on the converter. This is taken into account in the design of the optical coating.
The converted yellow light is to be emitted as completely as possible in a spectral range from 480 nm to 650 nm and with an angular distribution from 0° to 60° to the surface normal of the converter. The optical coating is designed to exhibit a reflection factor of <0.05, more preferably <0.01, in the spectral range from 480 to 650 nm.
FIG. 2 shows an embodiment of the arrangement for adjusting the color location of light, which includes a scattering layer 30 . The other elements correspond to those of the embodiment of FIG. 1 . Again, the thickness (d) of the converter is at least as large that essentially all the light that enters the converter is converted. The proportion of reflected blue light is defined through the scattering layer 30 . The scattering layer 30 may, for example, be a thin coat of white paint. Below scattering layer 30 , an anti-reflection layer may extend which minimizes unwanted reflection of the excitation light.
FIG. 3 shows a third embodiment of the invention. Elements similar to those of the embodiments described above are designated with the same reference numerals. The blue excitation light 1 is irradiated at an angle to the surface normal of the converter and is thereby progressively converted into yellow light, and part of the blue light reaches the reflective surface of the carrier or support 4 and is reflected there, but is substantially entirely absorbed before reaching the surface of the converter. An absorption and conversion point is shown at 60 . The converted light propagates to all sides, i.e. also in the illumination direction, as indicated at 6 . Part of the converted light is also reflected by the reflective surface of the carrier or support 4 and leaves the converter in the illumination direction.
The carrier or support 4 may be formed as a wedge-shaped plate which is rotatable around a rotation axis 40 . When the converter 2 is turned around this rotation axis 40 , the angle of incidence of excitation light 1 is altering. This permits fine-tuning of the angle of incidence with respect to the surface of the converter, which may also be done subsequently, when the excitation light source is not provided with a uniform excitation wavelength.
The fraction of reflected blue light 5 is determined by the laws of reflection at a transition of light from a thinner medium into an optically denser medium. By suitably choosing the angle of incidence of the excitation light 1 to the surface of the converter 2 , the ratio between converted and non-converted light is adjusted, and thus the mixing ratio between reflected blue light and emitted yellow light. In this way, it is possible to adjust the color location in the chromaticity diagram so as to generate white light.
Exemplary Embodiment
The converter material used was a Ce:YAG ceramic material having a refractive index of 1.833. The reflected fraction was chosen to be 0.2. This gives an angle of incidence of 68.3°. A deviation in the angle of incidence of +/−one degree only leads to a change of +/−1% of the reflected fraction (0.19 and 0.21). A deviation in the refractive index of 0.05 also leads to a change of only +/−1% of the reflected fraction. Both parameters may be adjusted more precisely without great technical effort.
In case a converter platelet of 0.2 mm thickness is used in transmission or in remission in a manner so that the unconverted fraction is 0.2, the thickness thereof has to be adjusted exactly within +/−6 μm in order to likewise obtain an accuracy of +/−1% of the fraction of unconverted light.
If a light source with polarized light is provided, the latter may be used to obtain the fraction of 0.2 of reflected light already at smaller angles. With vertical polarization, this condition is already satisfied at 50.6°. In this case, the light spot on the converter will not be distorted so much as with non-polarized light. In this case an angular accuracy of +/−1.5° will suffice to keep the reflected fraction between 0.19 and 0.21. | An arrangement for generating white light is provided. The arrangement generates the white light by combining blue light and yellow light. The yellow light originates from a converter which transforms into yellow light virtually all blue light that enters the converter. | 5 |
[0001] This application claims priority from provisional application Serial No. 60/288,905, filed May 4, 2001, and which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates generally to scanning of objects. More particularly, the invention relates to mass automated scanning of objects, such as dental study casts, housings for electronic devices including cellular telephones and electronic organizers, and other objects.
BACKGROUND OF THE INVENTION
[0003] Scanning of three-dimensional objects is generally known from the prior art. As disclosed in commonly assigned U.S. Pat. No. 6,217,334, dental study casts are scanned, and the data obtained from scanning the study casts is used for a variety of purposes, such as displaying a three-dimensional image of the static bite relationship of a particular patient for diagnostic and teaching purposes, or creating similar study casts in a suitable fabrication device based upon the scan data. Using the teachings from U.S. Pat. No. 6,217,34, individual objects can also be scanned for displaying a three-dimensional image of the objects or for use in fabricating similar objects based upon the scan data.
[0004] Scanning can also be used to verify a mating relationship between mating housing parts, such as housing parts for electronic devices including cellular telephones and electronic organizers. When housing parts are scanned, the scan data can be used to display three-dimensional images of the parts, with the displayed images being electronically brought together and displayed as a three-dimensional image, from which the accuracy of the fit between the housing parts can be determined.
[0005] Although scanning of objects is previously known, extensive human operator interaction is typically required in conventional scanning processes to monitor the process. For example, an operator typically must be present to load as well as unload the object(s) to be scanned onto and from the scanner. The need for human interaction in the scanning process creates problems. If the object is not loaded properly onto the scanner by the operator, inaccurate scan data can result. Further, the presence of an operator adds a labor cost to the scanning process, thereby increasing overall costs. Costs are increased even further if scanning is to be performed 24 hours a day, which is necessary for scanning large numbers of objects. In this case, additional employees must be hired for second and third shifts in order to operate and monitor the scanner.
[0006] Therefore, there is a need for an automated scanning system and method which reduces or eliminates the need for operator interaction, thereby facilitating mass scanning operations, improving the accuracy of the scan data and reducing the costs associated with the scanning operation.
SUMMARY OF THE INVENTION
[0007] The present invention provides a system and method for mass, automated scanning of objects, including dental study casts, housing parts, and other objects. The system and method are able to function with little or no human operator intervention, thereby facilitating high volume, automated scanning and reducing scanning costs.
[0008] In one aspect of the invention, a scanning system is provided. The system comprises a scanner having a scanning table, a conveyor mechanism adjacent the scanner for delivering an object to be scanned to the scanner, and a pick and place mechanism for taking the object from the conveyor mechanism and mounting it on the scanning table of the scanner.
[0009] In yet another aspect of the invention, a method of scanning of objects by a scanner having a scanning table is provided. The method comprises conveying one or more objects to be scanned to the scanner using a conveyor mechanism; picking an object from the conveyor mechanism and mounting the object on the scanning table of the scanner; scanning the object; and removing the scanned object from the scanning table and delivering the scanned object to a discharge location.
[0010] In still another aspect of the invention, a system for mass, automated scanning of dental study casts is provided. The system comprises a scanner having a scanning table, and a plurality of cassettes, each of which has a maxilla and mandible study cast for a single patient mounted thereon in known positions relative to each another. The system also includes a conveyor adjacent the scanner for delivering the cassettes to the scanner; and a pick and place mechanism engageable with the cassettes for picking one of the cassettes from the conveyor and mounting the picked cassette on the scanning table.
[0011] These and various other advantages and features of novelty which characterize the invention are pointed out with particularity in the claims annexed hereto and forming a part hereof. However, for a better understanding of the invention, its advantages and objects obtained by its use, reference should be made to the drawings which form a further part hereof, and to the accompanying description, in which there is described a preferred embodiment of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Referring to the drawings, wherein like numerals represent like parts throughout the several views:
[0013] [0013]FIG. 1 illustrates the method steps used to practice the principles of the present invention.
[0014] [0014]FIG. 2 diagrammatically illustrates functional blocks associated with the scanning process and processing data from the scanner.
[0015] [0015]FIG. 3 is a perspective view of an automated scanning system according to the present invention.
[0016] [0016]FIG. 4 illustrates a portion of the scanner and the infeed conveyor.
[0017] [0017]FIG. 5 is a perspective view of the rotary table of the scanner.
[0018] [0018]FIG. 6 illustrates an exemplary tool used to implement the automated scanning system and method according to a preferred embodiment of the present invention.
[0019] [0019]FIG. 7 illustrates a cassette used with the tool of FIG. 6.
[0020] [0020]FIG. 8 illustrates a calibration procedure for determining reference points.
[0021] [0021]FIG. 9 schematically illustrates the use of the tool and cassette in FIGS. 6 and 7.
[0022] [0022]FIG. 10 schematically illustrates a pair of housing shells that can be scanned in order to verify their mating relationship.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0023] A detailed discussion of a preferred embodiment of the automated scanning system and method of the present invention will be deferred pending a discussion of the concepts of the invention.
[0024] 1. Overview
[0025] Referring first to FIG. 1, the overall method of the present invention is illustrated, and is designated generally by the numeral 10 . First, at block 12 , the object(s) to be scanned is fixedly mounted onto a cassette. Any object(s) which one finds desirable to scan can be mounted onto the cassette. Examples of suitable objects include dental study casts and mating housing parts for electronic devices such as cell phones and electronic organizers. The preferred embodiment will be described below with respect to scanning dental study casts. The cassette and the procedure for mounting dental study casts on the cassette are described below with respect to FIGS. 6 - 9 .
[0026] At block 14 , the cassette is transported to the scanner by a suitable transport mechanism, and at block 16 , the cassette is picked from the transport by a picking mechanism and placed onto a table 32 of a scanner 30 . The transport mechanism and picking mechanism are described below and best seen in FIGS. 3 - 5 .
[0027] Once the cassette is properly mounted, the object(s) is then scanned at block 18 . In the preferred embodiment described below, two dental study casts are mounted on the cassette and the data obtained from scanning the study casts is used to create and display study cast images. The scan data can also be used to fabricate replicas of the study casts in a fabrication device based upon the scan data. In the preferred embodiment, the scanner 30 is a laser scanner with a laser 31 that is capable of movements along x-y-z axes to permit scanning of the complex geometries of dental study casts. However, other scanning concepts can also be used to practice the system and methods described herein, such as digitizing scanning.
[0028] Next, at block 20 , once the scan of the object(s) is complete, the cassette is removed from the scanner by the picking mechanism and placed onto a transport for subsequent transport away from the scanner. As described in the preferred embodiment below, the transport that conveys a scanned object(s) away from the scanner is preferably a transport mechanism that is separate from the transport mechanism that conveys the object(s) to the scanner. However, a single transport mechanism could be used to both convey the object(s) to and away from the scanner. It is also contemplated that instead of conveying the cassette away from the scanner after scanning, the cassette could be placed in a suitable discharge location for later removal.
[0029] With reference to FIG. 2, the image data obtained from the scanner 30 is processed by processor 501 of a computer 500 to create the image(s) of the scanned object(s), which in the preferred embodiment is the dental study casts. The processing by the processor 501 may include converting the scan data into images for display on a video display unit 503 ; converting the scan data into CNC or other format of output for use by a fabrication device 507 (also known as a prototyping apparatus); storing the scan data in a memory location or device 504 ; and/or transmitting the scan data to a remote processor 505 via modem block 502 . A user input device 506 permits input commands to control operation of the scanner, as well as permits the input of information concerning the object(s) to be scanned.
[0030] It will be appreciated by those of skill in the art that the computer 500 may be a personal computer (e.g., a Pentium based PC) or a special purpose computer. Further, the video display unit 503 may include any number of display devices such as cathode ray tubes, LCD displays, etc. Still further, the memory device 504 may include hard drives, floppy drives, magnetic tape, CD-ROM, random access memory, and readonly memory devices. Further, the modem 502 is illustrated to show a communications capability. Such capability may also be by way of a network, etc.
[0031] Fabrication device 507 may be connected directly to the computer 500 or may be connected to the remote computer 505 . The fabrication device 507 may be any number of devices which can utilize computer generated data and create a threedimensional object from such data. One example of such a machine are the devices utilizing stereo lithography technology manufactured by 3-D Systems of Valencia, Calif. under the model designations SLA-250 and SLA-500. Another example is the device utilizing filament technology (fused deposition modeling) manufactured by Statasys Corporation of Minneapolis, Minn. under the model designation FDM1500.
[0032] Further details on scanning, in the preferred embodiment, dental study casts and processing the image data can be found in U.S. Pat. Nos. 6,217,334, 6,206,693, and 6,200,135, which are incorporated herein by reference.
[0033] 2. Automated Scanning
[0034] The preferred embodiment will now be discussed. In the preferred embodiment, a pair of dental study casts 250 , 252 are mounted onto a cassette 100 for scanning by the scanner 30 . The study casts 250 , 252 are three-dimensional models of a patient's maxilla (i.e. upper) and mandible (i.e. lower) sets of teeth, respectively. The specifics of creating dental study casts from impressions that are taken of a patient's teeth is well known in the art. See, for example, U.S. Pat. Nos. 6,217,334, 6,206,693, and 6,200,135.
[0035] Turning now to FIGS. 3 - 5 , a system 50 to achieve automated scanning of the study casts is illustrated. Prior to explaining the system in detail, some of the difficulties that are faced in implementing automated scanning will be discussed. An automated scanning system should be able to operate with minimal or no operator input. This reduces the costs associated with scanning, and increases throughput of the system because the system is able to run essentially all the time, day and night, with minimal operator input.
[0036] One of the primary factors in being able to implement automated scanning of dental study casts is the ability to achieve an accurate bite registration of the images that result from the scanned upper and lower study casts. Without some basis by which the computer is able to properly register the scanned images of the upper and lower casts, an accurate visual representation of the bite registration cannot be achieved. Therefore, a suitable method for achieving bite registration is needed. A bite registration method that is suitable for use with the automated scanning system 50 is described later in this specification, as well as in copending U.S. patent application Ser. No. 09/746,468, filed on Dec. 22, 2000.
[0037] Returning now to FIGS. 3 - 5 , the automated scanning system 50 includes a scanning station 52 at which the study casts 250 , 252 are scanned by the scanner 30 . The scanner 30 is preferably a laser scanner as discussed above. Alternatively, other scanning concepts can be used, such as a digitizing scanning. Regardless of the particular scanner that is utilized, the scanner 30 is capable of scanning both the upper and lower casts 250 , 252 , with the scan data therefrom being processed by the computer 500 as discussed above. An operator input station 58 is provided that preferably includes a controller, such as the computer 500 , for controlling operation of the system 50 . The station 58 also preferably includes the display unit 503 and input device 506 for displaying system information and allowing operator inputs, such as system operation commands and patient data for each pair of study casts to be scanned.
[0038] The system 50 further includes a conveyor mechanism 60 for transporting the cassettes 100 to and from the station 52 . The conveyor mechanism 60 includes an infeed conveyor 62 with a conveyor belt 63 upon which the cassettes 100 with the study casts 250 , 252 mounted thereon are placed for subsequent feeding to the station 52 . The conveyor mechanism 60 further includes an outfeed conveyor 64 with a conveyor belt 65 that feeds the cassettes 100 , after scanning, to a downstream location for subsequent handling. Alternatively, the outfeed conveyor 64 could be eliminated, and the conveyor 62 extended past the station 52 so that the conveyor 62 acts both as the infeed conveyor and the outfeed conveyor. In addition, conveying mechanisms other than belts can be used.
[0039] Each cassette 100 is picked by a pick and place mechanism 66 , best seen in FIGS. 3 and 4, from the infeed conveyor 62 and placed onto the table 32 of the scanner 30 where it is fixed in place for scanning. After scanning, the cassette 100 is removed from the table 32 by the pick and place mechanism 66 and placed onto the outfeed conveyor 64 for subsequent handling.
[0040] The system 50 permits automated, mass scanning of dental study casts, as well as other objects. As long as the system 50 is able to correlate the scanned data from each pair of study casts with a particular patient, such as through operator input via the input station 58 or by system identification of patient identifying indicia on the cassettes 100 or study casts 250 , 252 , the system is able to operate independently while performing its scanning and data collection functions, with little or no human operator interaction.
[0041] With reference to FIGS. 3 and 4, it is seen that the scanner 30 is mounted on a support structure 70 , such as a table, located adjacent the conveyor mechanism 60 . An L-shaped support arm 72 of the scanner 30 extends upwardly from the support 70 and towards the conveyor mechanism 60 . A y-axis slide 74 is fixed on top of the support 70 , and a support 76 for the rotary table 32 is mounted on the y-axis slide 74 so as to movable along the y-axis. An actuator 78 , such as a reversible electric motor, is mounted to the slide 74 and is in driving engagement with the support 76 for actuating the support 74 along the y-axis. An actuator 80 , such as a reversible electric motor, is also mounted to the support 76 and is in driving engagement with the rotary table 32 for rotating the table 32 about a central axis X-X.
[0042] An x-axis slide 82 is fixed to the overhanging portion of the support arm 72 to allow movement of the laser 31 along the x-axis. In addition, a z-axis slide 84 is mounted to the x-axis slide 82 to allow movement of the laser 31 along the z-axis. An actuator 86 , such as a reversible electric motor, is mounted to the x-axis slide 82 and is in driving engagement with the z-axis slide 84 for actuating the z-axis slide 84 along the x-axis. In addition, an actuator 88 , such as a reversible electric motor, is mounted to the z-axis slide 84 and is in driving engagement with a support arm 90 for actuating the support arm 90 along the z-axis. The support arm 90 forms part of the pick and place mechanism 66 and supports the laser 31 .
[0043] Therefore, the laser 31 of the scanner 30 is mounted for linear movements along the x-axis slide 82 and the z-axis slide 84 . Further, the scanning table 32 is mounted for linear movement along the y-axis slide 74 , as well as for rotary movement about the axis X-X. The entire surface area of the study casts 250 , 252 can thus be completely scanned through suitable movements of the laser 31 or the study casts 250 , 252 along the x-y-z axes and about the X-X axis.
[0044] [0044]FIG. 4 illustrates the details of the pick and place mechanism 66 that is used to pick a cassette 100 from the conveyor 62 and place the cassette 100 on the rotary table 32 for scanning of the study casts 250 , 252 . The mechanism 66 is also used to remove the cassette from the rotary table and place it onto the conveyor 64 . The laser 31 is fixed to the support arm 90 of the pick and place mechanism 66 through a laser support 92 , whereby the laser 31 moves up and down along the z-axis when the arm 90 is actuated along the z-axis slide 84 . In addition, a cassette engagement finger 94 and a release finger 96 are fixed to the arm 90 at locations spaced from each other as shown in FIG. 4.
[0045] The mechanism for fixedly mounting the cassette 100 onto the rotary table 32 will now be described with reference to FIG. 5. The rotary table 32 includes a face plate 102 on the top surface thereof. A stop 104 , a pin 106 and a spring loaded lever arm 108 are all disposed on top of the face plate 102 for interacting with the cassette 100 and retaining the cassette 100 on the rotary table 32 .
[0046] The stop 104 includes a beveled surface 110 (also seen in FIG. 4) that is designed to engage a beveled edge 112 of the cassette 100 . The pin 106 is positioned to interact with a notch 114 that is formed in the side of the cassette 100 and counteract a rotational force that is applied to the cassette 100 by the lever arm 108 . The lever arm 108 includes a pivot post 116 that is pivotally mounted on the face plate 102 directly opposite the stop 104 . The post 116 is resiliently biased by a spring or other suitable resilient means in order to provide a force F in the direction of the arrow against the cassette 100 thereby forcing the cassette 100 against the stop 104 and the pin 106 . A tooling ball 118 is fixed to the lever arm 108 directly opposite the pin 106 , and engages a beveled edge 120 on the cassette 100 .
[0047] When the cassette 100 is disposed on the face plate 102 , the force provided by the lever arm 108 pushes the cassette 100 against the stop 104 and the pin 106 . Further, the engagement between the beveled surface 110 of the stop and the beveled edge 112 , as well as between the tooling ball 118 and the beveled edge 120 , create a downward force that presses the cassette downward against the face plate, firmly holding the cassette in place for subsequent scanning. The pin 106 , because it is located directly opposite the tooling ball 118 , counteracts any tendency for the cassette 100 to rotate about the stop 104 as a result of the force F applied by the lever arm 108 .
[0048] The procedure for picking a cassette from the conveyor 62 and placing it onto the rotary table 32 using the pick and place mechanism 66 will now be described with reference to FIGS. 4 and 5. The cassette 100 is formed with a key hole slot 130 (shown in dashed lines in FIG. 4) proximate the center thereof and extending generally parallel to the x-axis slide 82 . The cassette engagement finger 94 of the pick and place mechanism 66 includes a male tab 132 that has a shape that is complimentary to the slot 130 . The finger 94 further includes tab 134 that engages the exterior of the cassette when the male tab 132 is within the slot 130 . It is further evident from FIG. 4 that the removal finger 96 , which is intended to engage the lever arm 108 and remove the bias force F, projects a distance below the male tab 132 for a purpose which will become evident.
[0049] In order to pick a cassette 100 from the conveyor 62 , the z-axis slide 84 is actuated along the x-axis (i.e. to the left in FIG. 4) so that the finger 94 is positioned over the slot 130 . The arm 90 is then actuated along the z-axis (i.e. downward in FIG. 4) so that the male tab 132 enters the slot 130 . The z-axis slide 84 is then once again moved to the left to lock the male tab 132 in the slot 130 , with the tab 134 engaging the exterior surface of the cassette 100 for stabilization purposes. The arm 90 is then lifted upward, thereby lifting the cassette 100 off of the conveyor 62 . The z-axis slide 84 is then actuated to the right to bring the cassette to a position above the rotary table 32 . The arm 90 is then lowered until the removal finger 96 is next to the inside surface of the lever arm 108 , between the post 116 and the tooling ball 118 . Then, by moving the z-axis slide 84 to the left, the finger 96 forces the lever arm 108 in the opposite direction about the post 116 . The cassette 100 can then be lowered onto the face plate 102 by lowering the arm 90 further. Once the cassette 100 is fully lowered, the z-axis slide 84 is moved slightly to the right and the arm 90 is then raised, thereby removing the male tab 132 from the slot 130 . As this occurs, the finger 96 disengages from the lever arm 108 , and the biasing force F of the lever arm forces the cassette against the stop 104 and the pin 106 , thereby firmly retaining the cassette on the rotary table for subsequent scanning.
[0050] Removal of the cassette 100 from the rotary table 32 after scanning occurs in a similar fashion to the mounting of the cassette. The finger 96 removes the force of the lever arm 108 as the male tab 132 is being locked into the slot 130 . When the lever arm 108 has been moved sufficiently and the male tab 132 is firmly secured in the slot 130 , the cassette 100 can be moved slightly to the left and lifted upward, thereby removing the cassette. The cassette 100 is then carried to the conveyor 64 , or other suitable discharge location, for conveyance away from the scanner 30 .
[0051] It is to be realized that the x-axis slide 82 and the arm 90 must be of sufficient dimensions so as to be able to reach the two conveyors 62 , 64 . When side-by-side conveyors 62 , 64 are used, as illustrated in FIG. 3, the x-axis dimensions of the x-axis slide 82 and the arm 90 are generally increased. For the case of a conveyor 62 that is used as both the infeed and the outfeed, the x-axis dimensions of the x-axis slide 82 and the arm 90 need not be as large.
[0052] As was described above, a suitable method for achieving an accurate bite registration of the images that result from the scanned study casts 250 , 252 is needed. FIGS. 6 - 9 illustrate one embodiment of how an accurate bite registration can be achieved. This method can be used with study casts 250 , 252 that have roughly formed (i.e. not machined to precise geometric specifications) bases. In this method, the study casts 250 , 252 are initially mounted on the cassette 100 in known locations relative to each other, prior to placement of the cassette 100 onto the conveyor 62 for conveyance to the scanner 30 . Because the positioning of each study cast relative to the other is known, once scanning is complete, the scanned images can be brought into registration using predetermined reference points.
[0053] FIGS. 6 - 9 illustrate the tooling and other apparatus used to implement this method. FIG. 6 illustrates a tool 256 that is provided with a precision vertical slide 258 that is mounted so as to move vertically up and down relative to the tool 256 . The tool 256 includes a base 260 and a vertical support 262 provided with a guide rail 264 . The slide 258 includes a base 266 that is slidable on the rail 264 and an arm 268 that overhangs the base 260 . The arm 268 includes a pair of locating holes 270 , 272 on the bottom surface of the arm 268 facing the base 260 . In addition, the base 260 includes a pair of locating pins 274 , 276 .
[0054] [0054]FIG. 7 illustrates the cassette 100 upon which the study casts 250 , 252 are to be mounted. The study cast 252 is schematically illustrated in position on the cassette 100 . The cassette 100 includes a ridge 278 that separates the cassette into two halves, the first half receiving the study cast 252 and the second half receiving the study cast 250 . A removable plate 280 , upon which the study cast 250 is to be mounted, is provided on the second half of the cassette 100 . A pair of locating holes 274 ′, 276 ′ are formed in the bottom of the cassette 100 which interact with the locating pins 274 , 276 , respectively, so as to permit mounting of the cassette onto the base 260 of the tool 256 . In addition, the removable plate 280 includes a pair of locating pins 270 ′, 272 ′ formed on the bottom thereof that are designed to fit within the locating holes 270 , 272 , respectively, on the arm 268 of the slide 258 . The second half of the cassette 100 includes holes (not visible) that receive the locating pins 270 ′, 272 ′ when the plate 280 is disposed on the cassette.
[0055] With reference to FIG. 9, in implementing this method, the study cast 252 is first fixed onto the first half of the cassette 100 such as by using hot melt glue or other suitable temporary fastening means. The cassette 100 is then mounted onto the base 260 of the tool 256 via the locating pins 274 , 276 and locating holes 274 ′, 276 ′, with the study cast 252 disposed underneath the arm 268 of the slide 258 .
[0056] A wax wafer 282 , or other similar impression material, which has been previously bit into by the patient corresponding to the study casts 250 , 252 to record the patient's bite registration, is then placed onto the study cast 252 . The wafer 282 is placed onto the study cast so that the impression that corresponds to study cast 252 fits onto the teeth of the cast 252 . The study cast 250 is then placed on top of the wafer 282 with the teeth fitting into their corresponding impressions in the wafer. It should be realized that the wafer 282 permits the study casts 250 , 252 to be registered with each other while on the tool 256 . Once the study casts are registered, the plate 280 is fixed onto the bottom surface of the study cast 250 such as by using hot melt glue or other fixing means.
[0057] The slide 258 is then slid downward, either manually using a knob 284 fixed to the arm 268 or through suitable mechanical means (not illustrated), toward the plate 280 . The arm 268 then captures the plate 280 , with the locating pins 270 ′, 272 ′ fitting into the locating holes 270 , 272 . A fastener 286 connected to the plate 280 extends upwardly through a hole provided in the arm 268 to permit the plate 280 , and the study cast 250 now fixed thereto, to be fixed to the arm 268 so when the slide 256 is again raised, the study cast 250 and plate 280 are raised with the slide 256 . Raising the slide 256 separates the study casts 250 , 252 while precisely maintaining the relative positioning of the study casts so that the registration is maintained.
[0058] After the slide 258 is raised, the plate 280 , with the study cast 250 fixed thereto, is removed from the arm 268 , flipped over so that the study cast 250 faces upward, and mounted onto the second half of the cassette 100 so that both study casts are now fixed on the cassette. The cassette can then be placed onto the conveyor 62 for transport to the scanner so that the study casts can be scanned to create scanned images. It should be realized that the study casts are mounted on the cassette 100 in positions that maintain the bite registration of the patient. However, what is also needed are reference points so that the images resulting from the scan can be aligned.
[0059] Reference points are used in this method to achieve alignment, with the reference points being determined in accordance with a calibration process illustrated in FIG. 8. The calibration process is performed prior to mounting the study casts on the cassette. To perform calibration, the cassette 100 is provided with a removable plate 290 , in place of the plate 280 . The plate 290 includes a plurality of tooling balls 292 thereon. In the preferred embodiment, three tooling balls 292 are used, however a larger number of tooling balls could also be used. A layer of clay 294 or other impression material is placed on the other half of the cassette 100 . The cassette 100 is then mounted on the tool 256 as discussed above, with the clay 294 located underneath the arm 268 , and the plate 290 is mounted on the arm 268 with the tooling balls 292 facing downward toward the clay 294 . The slide 258 is then moved downward until the balls 292 move into the clay 294 in order to form tooling ball impressions 296 . The slide 258 is then moved upwardly and the plate 290 removed therefrom and remounted onto the cassette 100 .
[0060] The cassette 100 is then mounted onto the rotary table 32 of the scanner 30 , as discussed above, and the scanner scans the tooling balls 292 and the impressions 296 . Mounting of the cassette can be done using the pick and place mechanism 66 , or manually. By scanning the tooling balls 292 and impressions 296 , the computer 500 can find the centers of the balls 292 and impressions 296 , with the centers providing fixed reference points for use in aligning subsequently scanned study casts. These fixed reference points are retained within the memory device 504 , so that the computer 500 knows ahead of time the reference points to be used. Due to the construction of the tool 256 and the cassette 100 , the relative positions of the centers of the tooling balls 282 and the centers of the impressions 296 correspond to identical positions on the study casts 250 , 252 . Therefore, once the images of the study casts are generated, the three fixed points can be aligned to register the scanned impressions. After the points are aligned, the scanned images can be brought together by the computer 500 to a position representative of the patient's actual bite registration. The reference points are fixed in system memory, so that once the study casts are properly positioned on the cassette 100 , the scanning and registration can be completed automatically by the computer 500 , without requiring further operator input. It is further contemplated that the use of the tool 256 and the related process of positioning the study casts on the cassette 100 can be automated as well.
[0061] Periodically, the calibration process should be repeated so as to obtain updated reference points. This is necessary due to loosening of tolerances and general degradation of equipment.
[0062] As part of the automation of scanning, the system 50 needs to know which of the study casts 250 , 252 being scanned belong to which patient, so that the scan data can be saved to the appropriate memory location belonging to that patient in the memory device 504 . To accomplish this objective, the cassette 100 can be provided with a patient identification tag 150 , such as a radio frequency tag, a bar code or other suitable means. The tag 150 can contain patient data such as the patient's name and address, as well as more extensive patient data pertaining to the patient's past medical history, such as previous dental procedures. A sensor 152 is provided at a suitable location, such as on the support 76 as shown in FIG. 3, to read the tag 150 . The sensor 152 , as is shown in FIG. 2, is connected to the central processor 501 of the computer so that the information that is read from the tag 150 is provided to the computer. The sensor 152 can be located at any convenient point in the system 50 , such as on the tool 256 as shown in FIG. 6. However, it is preferred that the sensor 152 be positioned at a location so that it performs a read of the tag 150 just prior to, or immediately after, scanning of the study casts 250 , 252 .
[0063] The preferred embodiment of the invention has been described in relation to automated scanning of dental study casts. However, as discussed above, the concepts described herein can also be used in implementing automated scanning of a variety of other objects as well. For instance, automated scanning can be applied to parts that are to be mated together, such as molded housing shells for cellular phones, electronic organizers, pacemakers, and a host of other parts having complex geometries. When applied to mated parts, the accuracy of the parts, and the molds used to create the parts, can be verified by scanning the parts and determining from the scanned images whether a suitable fit between the parts will be achieved. This verification can be performed at the manufacturing level by the supplier of the molded parts as the molded parts are molded, or at an assembly level by the user of the molded parts to ensure the quality of received parts. Molded parts can include plastic molded parts, metal parts formed by metal molding techniques, and mating parts formed from other materials and other molding techniques suitable for those other materials.
[0064] [0064]FIG. 10 illustrates a pair of housing shells 300 , 302 that are to be mated together to form a housing for a device such as a cellular phone, electronic organizer or a pacemaker. The inside of each housing shell 300 , 302 is schematically illustrated to show an example of the possible complex geometry inside each shell. In use, the shell 300 is flipped over and mated with the shell 302 to enclose the electronics and other components of the device formed by the mated shells 300 , 302 . The shells 300 , 302 can be scanned and images created from the scan data in order to display the mating relationship (i.e. “verify” the parts) to determine whether the shells fit together adequately. A plurality of reference points would have to be used to achieve alignment of the shell images once they are scanned. For instance, three points R, S, T on the shell 300 , and three points R′, S′, T′ on the shell 302 , corresponding to, for example, mounting posts on the shells 300 , 302 , could be used to align the images once the shells are scanned. The method described above for registering the dental study casts could also be used to register the shells 300 , 302 .
[0065] In addition, automated scanning can be applied to single objects that are not mated or fitted with a corresponding object. For instance, single objects can be scanned for subsequent display of an image of the object created from the scan data, or the scan data can be used to fabricate a replica of the object based upon the scan data.
[0066] While a particular embodiment of the invention has been described, it will be understood that by those skilled in the art that the invention is not limited by the application, embodiment or the particular devices disclosed and described herein. It will be appreciated that other devices that embody the principles of this invention and other applications therefor other than as described herein can be configured within the spirit and intent of this invention. The system described herein is provided as only one example of an embodiment that incorporates and practices the principles of this invention. Other modifications and alterations are well within the knowledge of those skilled in the art and are to be included within the broad scope of the appended claims.
[0067] The above specification, examples and data provide a complete description of the manufacture and use of the composition of the invention. Since many embodiments of the invention can be made without departing from the spirit and scope of the invention, the invention resides in the claims hereinafter appended. | A system and method for mass, automated scanning of objects, including dental study casts, housing parts, and other objects. The system and method are able to function with little or no human operator intervention, thereby facilitating high volume scanning and reducing scanning costs. The system includes a scanner having a scanning table, a conveyor mechanism adjacent the scanner for delivering objects to be scanned to the scanner, and a pick and place mechanism for taking an object from the conveyor mechanism and mounting it onto the scanning table of the scanner. | 1 |
PRIORITY CLAIMS
This application claims the benefit of priority to U.S. Provisional Application No. 60/676,926, filed on May 2, 2005, entitled “HIGH TENSION CABLE TO W-BEAM TRANSITION”, invented by John Williams, which is hereby incorporated by reference in its entirety.
This application also claims the benefit of priority to U.S. Provisional Application No. 60/718,886, filed on Nov. 17, 2005, entitled “HTCB-MBGF TRANSITION”, invented by John Williams, which is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to the field of protecting vehicles from roadside hazards, and more particularly to an apparatus for providing a transition from a High Tension Cable Barrier to a Metal Beam Guide Fence.
DESCRIPTION OF THE RELATED ART
A Metal Beam Guide Fence attached to a bridge abutment is designed to prevent a collision between a vehicle and the bridge abutment. A vehicle exiting a driving lane near the bridge abutment may first contact the Metal Beam Guide Fence. The Metal Beam Guide Fence then absorbs at least a portion of the energy of the impact of the vehicle and/or redirects the vehicle past the bridge abutment and back into the driving lane. In some accidents, the vehicle may impact the end of the Metal Beam Guide Fence and extensively damage the vehicle and the people within the vehicle may be injured. In other accidents, the vehicle may pass behind the Metal Beam Guide Fence with other possibly severe consequences.
Low tension cable barriers have been positioned prior to Metal Beam Guide Fences in an attempt to prevent vehicles from impacting the end of the Metal Beam Guide Fence. The deflections of the low tension cable barriers are large and allowed for a more gentle ridedown in areas where larger deflections can be accommodated.
A High Tension Cable Barrier is typically installed in a median between driving lanes to prevent vehicles from crossing the median and colliding with other oncoming vehicles. A High Tension Cable Barrier is typically not used at a bridge abutment, however, because the deflection of the High Tension Cable Barrier by an impacting vehicle may be too large and may allow the vehicle to impact off-road obstructions. In these areas, Metal Beam Guide Fence is commonly used.
An apparatus is desired that could be used in addition to the Metal Beam Guide Fence that would extend the protection to vehicles exiting a driving lane.
SUMMARY OF THE INVENTION
The present invention comprises a transition device attached to a modified guardrail section of a Metal Beam Guide Fence for transferring a collision load from a High Tension Cable Barrier to the Metal Beam Guide Fence. The Metal Beam Guide Fence may be attached to a roadside hazard, such as a bridge abutment. A vehicle exiting a driving lane near the roadside hazard may first contact and deflect the cables of the High Tension Cable Barrier. The High Tension Cable Barrier may redirect the vehicle away from the end of the Metal Beam Guide Fence and may transfer the vehicle and the collision load to other portions of the Metal Beam Guide Fence. A transition device attached to the Metal Beam Guide Fence may interact with the high-tension cables of the High Tension Cable Barrier to transfer the impact tension of the high-tension cables to the Metal Beam Guide Fence. In this manner, the combination of a High Tension Cable Barrier interacting with a Metal Beam Guide Fence may not only prevent a collision between the vehicle and an off-road obstruction, but may also prevent a collision between the vehicle and the end portion of the Metal Beam Guide Fence, and may prevent the vehicle from passing behind the Metal Beam Guide Fence.
In some embodiments of the present invention, the High Tension Cable Barrier may be in-line with a portion of the Metal Beam Guide Fence that is situated in front of an off-road obstruction. In other embodiments of the present invention, the High Tension Cable Barrier may be offset from the portion of the Metal Beam Guide Fence that is situated in front of an off-road obstruction, and instead interacts with an angled portion of the Metal Beam Guide Fence.
In some embodiments, the transition device comprises a plate and one or more tubes. Each of the one or more tubes may be attached to the plate. In other embodiments, the transition device further comprises one or more support members. Each of the one or more support members may be positioned between a corresponding tube and the plate and may be attached to both the corresponding tube and the plate. The attachment method may be welding.
The transition device may be attached to the modified guardrail section by bolts or other fasteners. The transition device may also be attached to the modified guardrail section by welding.
The plate may be formed into a shape to conform to the shape of a modified guardrail section such as the shape of a W-beam panel. The shape of the plate may allow the transition device to nest against the modified guardrail section. The plate may have attachment holes for bolting to the modified guardrail section and cable slots to allow passage of cables through the plate.
The inner diameter of the tubes may be selected to enable one or more cables of the High Tension Cable Barrier to be inserted through the tubes. The tubes may be modified with an angled cut so that the ends of cables passing through the tubes may be angled away from the modified guardrail section. The angled cut of each of the tubes may also increase the strength of the attachment of each tube to the plate. The support members may also be attached to the tubes and the plate.
In another embodiment, the transition device may be attached to an angled end of a guardrail section.
BRIEF DESCRIPTION OF THE DRAWINGS
A better understanding of the present invention can be obtained when the following detailed description of the preferred embodiment is considered in conjunction with the following drawings, in which:
FIG. 1A is a perspective illustration of a set of embodiments of an in-line transition of a High Tension Cable Barrier to a Metal Beam Guide Fence;
FIG. 1B is an overhead view of the in-line transition of a High Tension Cable Barrier to a Metal Beam Guide Fence shown in FIG. 1A ;
FIG. 1C is a more detailed illustration of the in-line transition portion of the High Tension Cable Barrier to the Metal Beam Guide Fence shown in FIG. 1B ;
FIG. 2A is an overhead view of an embodiment of a transition of a High Tension Cable Barrier to a Metal Beam Guide Fence where the transition is offset;
FIG. 2B is a more detailed illustration of the offset transition portion of the High Tension Cable Barrier to the Metal Beam Guide Fence shown in FIG. 2A ;
FIG. 2C is an overhead view of another embodiment of the transition of a High Tension Cable Barrier to the Metal Beam Guide Fence where the transition is offset;
FIG. 3A is an illustration of an embodiment of a transition device 200 B for transferring a tension load from a High Tension Cable Barrier to a Metal Beam Guide Fence;
FIG. 3B is an end view of transition device 200 B;
FIG. 3C is a perspective view of transition device 200 B; and
FIG. 4 is another embodiment of a transition device 201 for an in-line transition of a High Tension Cable Barrier to a Metal Beam Guide Fence.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and are herein described in detail. It should be understood, however, that the drawings and detailed description thereto are not intended to limit the invention to the particular form disclosed, but on the contrary, the intention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the present invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A High Tension Cable Barrier Coupled to a Metal Beam Guide Fence
In some embodiments, a High Tension Cable Barrier may be coupled to a Metal Beam Guide Fence, which may be substantially parallel to an adjacent road 199 and include a guardrail panel 197 supported by posts (e.g., support post 195 ), as shown in FIG. 1A . FIGS. 1A-2C show various views of a set of embodiments of a transition device 200 A attached to a modified guardrail section 100 , of the Metal Beam Guide Fence that may transfer an impact tension load from cables 150 A-F of the High Tension Cable Barrier to the Metal Beam Guide Fence. FIGS. 3A-C show various views of a transition device 200 C. A typical installation of a High Tension Cable Barrier may have three cables (e.g., cables 150 A-C, 150 D-F, 150 G-I, or 150 J-L), however, a number of cables other than three is possible and contemplated.
FIG. 1A is a perspective illustration of a set of embodiments of an in-line transition of a High Tension Cable Barrier to a Metal Beam Guide Fence. FIG. 1A shows the cables 150 A-C passing through slots 209 A-C of a modified guardrail section 100 of the Metal Beam Guide Fence. One example of a modified guardrail section 100 may be a W-beam panel modified with cable slots (such as slots 209 A-C) and mounting holes (not shown in FIG. 1A ) for attaching the transition device 200 A. The transition device 200 A may be attached to the modified guardrail section 100 by bolts or other fasteners. In some embodiments, the transition device 200 may also be attached to the modified guardrail section 100 by welding 500 . The Metal Beam Guide Fence may be attached to a roadside hazard such as a bridge abutment (not shown in FIG. 1A ) that would be located at the left side of FIG. 1A . W-beam panels are produced in a variety of lengths, and any length may be selected for modification as modified guardrail section 100 .
A vehicle exiting a driving lane near the bridge abutment may first collide with the tensioned cables 150 A-C of the High Tension Cable Barrier. The High Tension Cable Barrier may then reduce the vehicle's speed and may transfer the impact tension load in the cables to the Metal Beam Guide Fence. In this manner, the combination of a High Tension Cable Barrier interacting with a Metal Beam Guide Fence may reduce the severity of a collision between the vehicle and a bridge abutment, but may also prevent the vehicle from passing behind the Metal Beam Guide Fence.
The High Tension Cable Barrier may utilize three 3×7 steel cables 150 A-C with static tension of up to 5,600 lbs. (25 KN). The cables 150 A-C of the High Tension Cable Barrier may be anchored at one or both ends into end terminals that may be restrained by end terminal posts (such as the end terminal post 120 as shown in FIG. 2A , or 120 A,B as shown in FIGS. 2 B,C). Each of the three cables may be separately terminated at an end terminal post or a plurality of cables may be terminated at one end terminal post.
FIG. 1B is an overhead view of the in-line transition of a High Tension Cable Barrier to a Metal Beam Guide Fence as shown in FIG. 1A . FIG. 1B shows a transition device 200 A attached to the back of the modified guardrail section 100 of the Metal Beam Guide Fence. In some embodiments, the transition device 200 A may be attached to the modified guardrail section 100 by bolts or other fasteners. In other embodiments, the transition device 200 may be attached to the modified guardrail section 100 by welding 500 . The cables 150 A-C pass through the modified guardrail section 100 and the transition device 200 A and in some embodiments may be terminated in a cable end termination 250 B. Cables 150 A,C may also have end terminations (not shown in FIG. 1B since they are primarily hidden by the formed edges of the modified guardrail section 100 in this view). The static tension in cable 150 B may press the cable end termination 250 B tight against portion 210 B of the transition device 200 A. Similarly the end terminations for cables 150 A,C may also be pressed tight against the transition device 200 A. Guardrail section 105 A may overlap the modified guardrail section 100 . The portion of guardrail section 105 A that does overlap may be a straight section or a formed section.
FIG. 1C is a more detailed illustration of the in-line transition portion of the High Tension Cable Barrier to a Metal Beam Guide Fence shown in FIG. 1B . Guardrail section 105 A may also be a curved section (such as section 105 D, as shown in FIG. 2C ).
FIG. 2A is an overhead view of a set of embodiments of a transition of a High Tension Cable Barrier to a Metal Beam Guide Fence in which the High Tension Cable Barrier is not in-line with the Metal Beam Guide Fence. In these embodiments, the High Tension Cable Barrier may be offset and the cables 150 D-F may couple to the angled portion of the Metal Beam Guide Fence. Each of the cables 150 D-F of the High Tension Cable Barrier may pass through a modified guardrail section 105 C and an attached transition device 200 B and then be anchored into an end terminal (such as end terminal 250 B) restrained by an end terminal post 120 . In these embodiments, tension in the cables may transfer to the modified guardrail section 105 C due to forces on the attached transition device 200 B from the cables 150 D-F. In this manner, an impact by a vehicle against the cables of the High Tension Cable Barrier may transfer a force load to the Metal Beam Guide Fence.
The angle “theta 2” may be selected so that the end of the Metal Beam Guide Fence may be separated from the High Tension Cable Barrier by approximately 4′ 6″ or more. This separation may avoid a vehicle contacting the end of the Metal Beam Guide Fence as a result of deflections of the High Tension Cable Barrier.
FIG. 2B is a more detailed illustration of the offset transition portion of the High Tension Cable Barrier to a Metal Beam Guide Fence shown in FIG. 2A . Cable 150 D and 150 F may terminate at the end terminal post 120 A. Cable 150 E may terminate at the end terminal post 120 B. Cable 150 F may also terminate at a separate end terminal post (not shown in FIG. 2B ). In these embodiments, the distance “x 1 ” may define the amount of offset of the High Tension Cable Barrier. The amount of offset may be defined as the distance between the position the cables 150 D-F may couple to the angled portion of the Metal Beam Guide Fence and the bend in the Metal Beam Guide Fence.
FIG. 2C is an overhead view of another embodiment of an offset transition of a High Tension Cable Barrier to a Metal Beam Guide Fence. In this embodiment, the modified guardrail section 105 D is shown as a curved section. A transition device 200 C may be similarly curved to match the radius of the curve of modified guardrail section 105 D in such an embodiment.
Transition Device
FIGS. 3A-C show various views of an embodiment of a transition device 200 B that may be effective in transferring an impact tension load in high tension cables from a High Tension Cable Barrier to a Metal Beam Guide Fence. FIG. 3A shows an edge view of the transition device 200 B comprising a plate 206 and one or more tubes 202 A-C. The one or more tubes 202 A-C may be attached to the plate 206 . In some embodiments, transition device 200 B may further comprise one or more support members 204 A-C. In these embodiments, the one or more tubes 202 A-C may be attached to both a corresponding support member and the plate 206 . The attachment method may be welding. However, a variety of other attachment methods may be used as well.
The plate 206 (also referred to as a nesting plate) may be a sheet of 3/16 inch thick steel, although other materials and thicknesses are contemplated. The plate 206 may be formed into a shape to conform to the shape of a modified guardrail section 100 . The shape of plate 206 may be the shape of a W-beam panel as shown in FIG. 3B (an end view of transition device 200 B). The shape of plate 206 may allow transition device 200 B to nest against the modified guardrail section 100 . In some embodiments, the transition device 200 B may be attached to the modified guardrail section 100 by bolts or other fasteners. In other embodiments, the transition device 200 B may be attached to the modified guardrail section 100 by welding. The plate 206 may have mounting holes 220 for bolting to the modified guardrail section 100 and cable slots 208 A-C as shown in FIG. 3C .
The tubes 202 A-C may be modified sections of steel pipe. The ID of the pipe may be selected to enable a high tension cable of the High Tension Cable Barrier to be inserted through the tubes 202 A-C. A 1″ OD steel pipe may be selected. Tubes of other materials and dimensions are contemplated. The tubes 202 A-C may be modified with an angled cut from the center of one end to the side of each of the tubes 202 A-C as shown in FIG. 3A . The angled cut may enable the tubes to be welded to the plate along the outside edge of the angled cut to increase the strength of the attachment of the tube to the plate 206 . In some embodiments, the angle of the cut may be selected so that the surface of the tube at the angled cut may contact the plate 206 when the tube is supported by a corresponding one of the support members 204 A-C. Each of the tubes 202 A-C may also be welded to a corresponding one of the support members 204 A-C in the configuration shown in FIGS. 3A-B .
The support members 204 A-C (also referred to as gusset plates) may be ¼ inch thick steel plate. In some embodiments, the support members 204 A-C may be made from U shaped channels. The support members 204 A-C may be welded to the plate 206 and the tubes 202 A-C.
FIG. 4 shows another embodiment of a transition device 201 that may enable transfer of impact tension from cables of a High Tension Cable Barrier to a Metal Beam Guide Fence. In this embodiment, the transition device 201 may be fabricated by attaching transition device 200 A to a first end of a modified guardrail section. The guardrail section is modified with an angled cut at the first end. The angle of the cut is selected to provide a specified angle between the transition device 200 A and the modified guardrail section. In an alternate embodiment, transition device 200 A is also modified with an angled cut at the attaching end, and the angle of each cut is selected to provide a specified angle between the transition device 200 A and the modified guardrail section. The method of attachment may be by welding, however, other methods are possible and contemplated.
In still another embodiment of a transition device 201 , plate 206 may be replaced by a modified guardrail section with a formed end portion and one or more tubes and corresponding support members attached to the formed end portion. The formed end may have a length equivalent to the length of the plate 206 . The guardrail section may be modified with cable slots and attachment holes to bolt transition device 201 to a modified guardrail section 100 . Guardrail section 100 may be modified with cable slots and attachment holes.
Although the embodiments above have been described in considerable detail, numerous variations and modifications will become apparent to those skilled in the art once the above disclosure is fully appreciated. It is intended that the following claims be interpreted to embrace all such variations and modifications. | An apparatus for preventing a collision between a vehicle and an end of a Metal Beam Guide Fence. A transition device is attached to a modified section of the Metal Beam Guide Fence. The transition device and modified section are configured to allow passage of cables of a High Tension Cable Barrier through the Metal Beam Guide Fence and the transition device. The High Tension Cable Barrier redirects the colliding vehicle away from the end of the Metal Beam Guide Fence. The transition device and modified section are also configured to interact with the cables of the High Tension Cable Barrier to transfer and spread the collision load from the high tension cables to the Metal Beam Guide Fence. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a robot arm mechanism having arms contracted and extended, and more particularly to a robot arm mechanism incorporating an arm driving mechanism for driving the arms to assume its contracted and extended positions.
2. Description of the Related Art
The robot arm mechanism of this type is used in the process of producing semiconductors in which the robot arm mechanism is operated to have arms contracted and extended to handle works, i.e., objects to be treated. These objects include for example such as wafers and other precision parts that are to be transferred and then unloaded onto a work table by the robot arm mechanism.
A conventional robot arm mechanism of this kind is disclosed in, for example, Japanese patent laying-open publication Tokkaihei 7-227777 and comprises a handling member for holding and releasing objects, and robot arms for operating and moving the hand. The robot arms are constituted by a plurality of parallel links having joint portions on which are provided synchronous gears for maintaining the links in their parallel attitudes. The synchronous gears are rotated to have the hand maintained in its predetermined direction by moving the hand forwardly and rearwardly while the parallel links are operated. Another conventional robot arm mechanism of this kind is disclosed in Japanese patent laying-open publication Tokkaihei 9-272084 and comprises robot arms constituted by a plurality of parallel links to form a parallelogram linkage contractable and extensible, and a synchronous motion mechanism including gears, belts and pulleys operatively mounted on the links. The synchronous motion mechanism is operated to have gears, belts and pulleys driven so that the parallelogram linkage can be contracted and extended.
It is another object of the present invention to provide a robot arm mechanism which is exempt from such driven gears, belts and pulleys of the synchronous motion mechanism necessitated by the conventional robot arm mechanisms to ensure that no dust is produced and fallen in the vacuum working chamber of highly pure air.
SUMMARY OF THE INVENTION
According to the first aspect of the present invention there is provided a robot arm mechanism comprising: a handling member for supporting and handling an object; a robot arm connected to the handling member, the robot arm comprising a first arm link having first and second end portion, a second arm link having first and second end portion, and a link retaining mechanism having a center line, the link retaining mechanism pivotably retaining the first and second arm links respectively at the first end portions of the first and second arm links and keeping parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link and the second line being a line symmetrical with respect to the center line with the line passing through the first and second end portions of the second arm link, the link retaining mechanism comprising a first joint cross linkage including a first short link having first and second end portions, a first long link having first and second end portions and longer than the first short link of the first joint cross linkage of the link retaining mechanism, the first short and long links of the first joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the first short link of the first joint cross linkage of the link retaining mechanism and the first end portion of the first long link of the first joint cross linkage of the link retaining mechanism, a second short link having first and second end portions and substantially equal in length to the first short link of the first joint cross linkage of the link retaining mechanism, the first long link of the first joint cross linkage of the link retaining mechanism and the second short link of the first joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the first long link of the first joint cross linkage of the link retaining mechanism and the first end portion of the second short link of the first joint cross linkage of the link retaining mechanism, and a second long link having first and second end portions and substantially equal in length to the first long link of the first joint cross linkage of the link retaining mechanism, the second short and long links of the first joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the second short link of the first joint cross linkage of the link retaining mechanism and the first end portion of the second long link of the first joint cross linkage of the link retaining mechanism, the second long link of the first joint cross linkage of the link retaining mechanism and the first short link of the first joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the second long link of the first joint cross linkage of the link retaining mechanism and the first end portion of the first short link of the first joint cross linkage of the link retaining mechanism under the state that the second long link of the first joint cross linkage of the link retaining mechanism is crossed with the first long link of the first joint cross linkage of the link retaining mechanism, and a second joint cross linkage including a first short link having first and second end portions, a first long link having first and second end portions and longer than the first short link of the second joint cross linkage of the link retaining mechanism, the first short and long links of the second joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the first short link of the second joint cross linkage of the link retaining mechanism and the first end portion of the first long link of the second joint cross linkage of the link retaining mechanism, a second short link having first and second end portions and substantially equal in length to the first short link of the second joint cross linkage of the link retaining mechanism, the first long link of the second joint cross linkage of the link retaining mechanism and the second short link of the second joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the first long link of the second joint cross linkage of the link retaining mechanism and the first end portion of the second short link of the second joint cross linkage of the link retaining mechanism, and a second long link having first and second end portions and substantially equal in length to the first long link of the second joint cross linkage of the link retaining mechanism, the second short and long links of the second joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the second short link of the second joint cross linkage of the link retaining mechanism and the first end portion of the second long link of the second joint cross linkage of the link retaining mechanism, the second long link of the second joint cross linkage of the link retaining mechanism and the first short link of the second joint cross linkage of the link retaining mechanism pivotably connected with each other at the second end portion of the second long link of the second joint cross linkage of the link retaining mechanism and the first end portion of the first short link of the second joint cross linkage of the link retaining mechanism under the state that the second long link of the second joint cross linkage of the link retaining mechanism is crossed with the first long link of the second joint cross linkage of the link retaining mechanism, the length ratio of each of the first and second short links of the first joint cross linkage of the link retaining mechanism to each of the first and second long links of the first joint cross linkage of the link retaining mechanism substantially equal to the length ratio of each of the first and second short links of the second joint cross linkage of the link retaining mechanism to each of the first and second long links of the second joint cross linkage of the link retaining mechanism, the first short link of the first joint cross linkage of the link retaining mechanism integrally formed with and in parallel relationship with the first long link of the second joint cross linkage of the link retaining mechanism under the state that the second end portion of the first short link of the first joint cross linkage of the link retaining mechanism is connected with the first end portion of the first long link of the second joint cross linkage of the link retaining mechanism, the first long link of the first joint cross linkage of the link retaining mechanism integrally formed with and in parallel relationship with the first short link of the second joint cross linkage of the link retaining mechanism under the state that the first end portion of the first long link of the first joint cross linkage of the link retaining mechanism is connected with the second end portion of the first short link of the second joint cross linkage of the link retaining mechanism, the first end portion of any one of the first and second arm links integrally formed with the second short link of the first joint cross linkage of the link retaining mechanism, the first end portion of the other one of the first and second arm links integrally formed with the second long link of the second joint cross linkage of the link retaining mechanism; and a robot arm driving mechanism for driving the robot arm.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects, features and advantages of the present invention will become apparent as the description proceeds when taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIG. 2 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 2 is a skeleton view of one condition of the first preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 2 a and FIG. 2 b are schematic illustrations used to explain the operation of the robot arm mechanism of FIG. 2 .
FIG. 3 is a skeleton view of another condition of the first preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 4 is a cross-sectional view taken on the lines F 1 —F 1 in FIG. 2;
FIG. 5 is a skeleton view of one condition of the second preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 6 is a skeleton view of another condition of the second preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 7 is a skeleton view of the third preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 8 is a cross-sectional view taken on the lines F 2 —F 2 in FIG. 7;
FIG. 9 is a skeleton view of one condition of the fourth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 10 is a skeleton view of another condition of the fourth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 11 is a cross-sectional view taken on the lines F 3 —F 3 in FIG. 9;
FIG. 12 is a skeleton view of one condition of the fifth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 13 is a skeleton view of another condition of the fifth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 14 is a skeleton view of one condition of the sixth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 15 is a skeleton view of another condition of the sixth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 16 is a skeleton view of the seventh preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 17 is a skeleton view of the eighth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 18 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIGS. 19, 24 , and 25 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 19 is a skeleton view of the ninth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 20 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIGS. 21, 22 , and 23 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 21 is a skeleton view of the tenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 22 is a skeleton view of the eleventh preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 23 is a skeleton view of the twelfth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 24 is a skeleton view of the thirteenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 25 is a skeleton view of the fourteenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 26 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIG. 27 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 27 is a skeleton view of the fifteenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 28 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIG. 29 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 29 is a skeleton view of the sixteenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 30 is an enlarged fragmentary skeleton view of the robot arm mechanism shown in FIG. 31 to be used for explaining the principle of the robot arm mechanism according to the present invention;
FIG. 31 is a skeleton view of one condition of the seventeenth preferred embodiment of the robot arm mechanism according to the present invention;
FIG. 32 is a skeleton view of another condition of the seventeenth preferred embodiment of the robot arm mechanism according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Throughout the following detailed description, similar reference characters and numbers refer to similar elements in all figures of the drawings.
Referring to FIGS. 1 to 4 of the drawings, there is shown a first preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 101 is shown in FIGS. 1 to 4 as comprising a handling member 125 for supporting and handling an object.
The handling member 125 should be configured to be available for handling, i.e., holding and releasing a wafer and other materials to be used for producing semiconductors. In this embodiment particularly shown in FIG. 2, the handling member 125 is formed with a recess 125 a which is designed suitably to receive and release such materials. The configuration of the handling member 125 depends upon the sizes and shapes of the materials to be handled by the handling member 125 according to the present invention.
The robot arm mechanism 101 further comprises a robot arm 810 connected to the handling member 125 . The robot arm 810 comprises a first arm link 811 having first and second end portion, a second arm link 812 having first and second end portion, and a link retaining mechanism 200 having a center line 201 .
The link retaining mechanism 200 pivotably retains the first and second arm links 811 and 812 respectively at the first end portions of the first and second arm links 811 and 812 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link 811 and the second line being a line symmetrical with respect to the center line 201 with the line passing through the first and second end portions of the second arm link 812 . In fact the first and second arm links 811 and 812 are in symmetrical relationship with each other with respect to the center line 201 . The above-described parallel relationship is illustrated in FIGS. 2 a and 2 b . FIG. 2 a illustrates the specific relationship shown in FIG. 2 wherein the first line L 1 passing through the first and second end portions of the link 811 is maintained colinear with the line L 2 , which is symmetrical with respect to the center line 201 with the line passing through the first and second end portions of the second arm link 812 . FIG. 2 b illustrates the parallel relationship wherein the first line L 1 passing through the first and second end portions of the link 811 is maintained parallel, but not colinear, with the second line L 2 which is symmetrical with respect to the center line 201 with the line passing through the first and second end portions of the second arm link 812 .
The link retaining mechanism 200 comprises a first joint cross linkage 210 which includes a first short link 211 having first and second end portions.
The first joint cross linkage 210 further includes a first long link 212 having first and second end portions and longer than the first short link 211 . The first short and long links 211 and 212 are pivotably connected with each other at the second end portion of the first short link 211 and the first end portion of the first long link 212 .
The first joint cross linkage 210 further includes a second short link 213 having first and second end portions and substantially equal in length to the first short link 211 . The first long link 212 and the second short link 213 are pivotably connected with each other at the second end portion of the first long link 212 and the first end portion of the second short link 213 .
The first joint cross linkage 210 further includes a second long 214 link having first and second end portions and substantially equal in length to the first long link 212 . The second short and long links 213 and 214 are pivotably connected with each other at the second end portion of the second short link 213 and the first end portion of the second long link 214 .
The second long link 214 and the first short link 211 are pivotably connected with each other at the second end portion of the second long link 214 and the first end portion of the first short link 211 under the state that the second long link 214 is crossed with the first long link 212 .
The robot arm 810 comprises a second joint cross linkage 220 which includes a first short link 221 having first and second end portions. The first long link 212 and the first short link 221 are substantially equal in length to each other.
The second joint cross linkage 220 further includes a first long link 222 having first and second end portions and longer than the first short link 221 . The first short and long links 221 and 222 are pivotably connected with each other at the second end portion of the first short link 221 and the first end portion of the first long link 222 .
The second joint cross linkage 220 further includes a second short link 223 having first and second end portions and substantially equal in length to the first short link 221 . The first long link 222 and the second short link 223 are pivotably connected with each other at the second end portion of the first long link 222 and the first end portion of the second short link 223 .
The second joint cross linkage 220 further includes a second long link 224 having first and second end portions and substantially equal in length to the first long link 222 . The second short and long links 223 and 224 are pivotably connected with each other at the second end portion of the second short link 223 and the first end portion of the second long link 224 .
The second long link 224 and the first short link 221 are pivotably connected with each other at the second end portion of the second long link 224 and the first end portion of the first short link 221 under the state that the second long link 224 is crossed with the first long link 222 .
The length ratio of each of the first and second short links 211 and 213 to each of the first and second long links 212 and 214 is substantially equal to the length ratio of each of the first and second short links 221 and 223 to each of the first and second long links 222 and 224 .
The first short link 211 is integrally formed with and in coaxial relationship with the first long link 222 under the state that the second end portion of the first short link 211 is connected with the first end portion of the first long link 222 . The first long link 212 is integrally formed with and in coaxial relationship with the first short link 221 under the state that the first end portion of the first long link 212 is connected with the second end portion of the first short link 221 .
The first end portion of the second arm link 812 is integrally formed with the second short link 213 . The first end portion of the first arm link 811 is integrally formed with the second long link 224 . The center line 201 passes through the first and second end portions of the first long link 212 . The first end portions of the first and second arm links 811 and 812 are positioned on the center line 201 .
The robot arm 810 further comprises a third arm link 813 having first and second end portions. The handling member 125 has first and second portions. The third arm link 813 and the handling member 125 are pivotably connected with each other at the second end portion of the third arm link 813 and the first portion of the handling member 125 .
The robot arm 810 further comprises a fourth arm link 814 having first and second end portions. The fourth arm link 814 and the handling member 125 are pivotably connected with each other at the second end portion of the fourth arm link 814 and the second portion of the handling member 125 . The first and second arm links 811 and 812 are substantially equal in length to each other. The third and fourth arm links 813 and 814 are substantially equal in length to each other.
The robot arm 810 further comprises a first joint mechanism 140 retaining the first and third arm links 811 and 813 respectively at the second end portion of the first arm link 811 and the first end portion of the third arm link 813 under the state that the first arm link 811 is pivotable around the second end portion of the first arm link 811 with respect to the third arm link 813 . The second end portion of the first arm link 811 and the first end portion of the third arm link 813 are connected with each other.
The first joint mechanism 140 comprises a first link 141 having first and second end portions and substantially equal in length to the first arm link 811 . The first link 141 is integrally formed with and in coaxial relationship with the first arm link 811 under the state that the first end portion of the first link 141 is connected with the first end portion of the first arm link 811 .
The first joint mechanism 140 further comprises a second link 142 having first and second end portions. The first and second links 141 and 142 are pivotably connected with each other at the second end portion of the first link 141 and the first end portion of the second link 142 . The second link 142 is pivotably connected with the first end portion of the third arm link 813 .
The first joint mechanism 140 further comprises a third link 143 having first and second end portions and substantially equal in length to the first link 141 . The second and third links 142 and 143 are pivotably connected with each other at the second end portion of the second link 142 and the first end portion of the third link 143 .
The first joint mechanism 140 further comprises a fourth link 144 having first and second end portions and substantially equal in length to the second link 142 . The third and fourth links 143 and 144 are pivotably connected with each other at the second end portion of the third link 143 and the first end portion of the fourth link 144 . The fourth and first links 144 and 141 are pivotably connected with each other at the second end portion of the fourth link 144 and the first end portion of the first link 141 under the state that the first link 141 is in parallel relationship with the third link 143 and that the second link 142 is in parallel relationship with the fourth link 144 . The second end portion of the fourth link 144 is integrally connected with the first long link 212 .
The robot arm 810 further comprises a second joint mechanism 132 retaining the second and fourth arm links 812 and 814 respectively at the second end portion of the second arm link 812 and the first end portion of the fourth arm link 814 under the state that the second arm link 812 is pivotable around the second end portion of the second arm link 812 with respect to the fourth arm link 814 . The second end portion of the second arm link 812 and the first end portion of the fourth arm link 814 are connected with each other.
The robot arm 810 further comprises a stabilizing mechanism 160 which includes a first link 161 having first and second end portions and substantially equal in length to the third arm link 813 . The first link 161 is integrally formed with and in coaxial relationship with the third arm link 813 under the state that the first end portion of the first link 161 is connected with the first end portion of the third arm link 813 .
The stabilizing mechanism 160 further includes a second link 162 having first and second end portions. The first and second links 161 and 162 are pivotably connected with each other at the second end portion of the first link 161 and the first end portion of the second link 162 . The second link 162 is integrally formed with the handling member 125 .
The stabilizing mechanism 160 further includes a third link 163 having first and second end portions and substantially equal in length to the first link 161 . The second and third links 162 and 163 are pivotably connected with each other at the second end portion of the second link 162 and the first end portion of the third link 163 .
The stabilizing mechanism 160 further includes a fourth link 164 having first and second end portions and substantially equal in length to the second link 162 . The third and fourth links 163 and 164 are pivotably connected with each other at the second end portion of the third link 163 and the first end portion of the fourth link 164 . The fourth and first links 164 and 161 are pivotably connected with each other at the second end portion of the fourth link 164 and the first end portion of the first link 161 under the state that the first link 161 is in parallel relationship with the third link 163 and that the second link 162 is in parallel relationship with the fourth link 164 . The second end portion of the fourth link 164 is integrally connected with the second link 142 .
The robot arm mechanism 101 further comprises a robot arm driving mechanism 120 for driving the robot arm 810 .
The arm driving mechanism 120 comprises a first driving shaft 121 rotatable around a rotation axis 123 .
The arm driving mechanism 120 further comprises a second driving shaft 122 in the form of a hollow shape to rotatably receive therein the first driving shaft 121 and rotatable around the rotation axis 123 .
The second driving shaft 122 is integrally connected with the first long link 212 and rotates the first long link 212 around the rotation axis 123 . The first driving shaft 121 is integrally connected with the first arm link 811 and rotates the first arm link 811 around the first end portion of the first arm link 811 .
When the second driving shaft 122 rotates the first long link 212 around the rotation axis 123 , the center line 201 is rotated around the rotation axis 123 . This results in the rotation of the robot arm mechanism 101 around the rotation axis 123 .
When the first arm link 811 is rotated by the first driving shaft 121 with respect to the first long link 212 , the fact that the first and second arm links 811 and 812 are respectively and integrally formed with the second long link 224 and the second short link 213 results in the rotation of the second arm link 812 with respect to the first long link 212 and the first arm link 811 . This results in the contracted or extended condition of the robot arm mechanism 101 .
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 212 and that the first driving shaft 121 is integrally connected with the first arm link 81 , the first driving shaft 121 may be integrally connected with the second arm link 812 instead of the first arm link 811 , according to the present invention.
In this case that the first driving shaft 121 is integrally connected with the second arm link 812 instead of the first arm link 811 , the operation of the robot arm mechanism 101 is similar to the robot arm mechanism 101 in the case that the first driving shaft 121 is integrally connected with the first arm link 811 .
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 212 and that the first driving shaft 121 is integrally connected with the first arm link 811 , the second driving shaft 122 may be integrally connected with the second arm link 812 instead of the first long link 212 , according to the present invention.
In this case that the first long link 212 is replaced by the second arm link 812 , the second long link 224 is rotated around the rotation axis 123 when the first arm link 811 is rotated by the first driving shaft 121 , resulting from the fact that the first arm link 811 is integrally formed with the second long link 224 . When the second arm link 812 is rotated by the second driving shaft 122 , the fact that the second arm link 812 is integrally formed with the second short link 213 results in the rotation of the second short link 213 around the rotation axis 123 . The rotation of the second long link 224 and the rotation of the second short link 213 can result in the rotation of the first long link 212 around the rotation axis 123 . This results in the rotation of the center line 201 . The rotation of the center line 201 around the rotation axis 123 results in the rotation of the robot arm mechanism 101 around the rotation axis 123 .
When the first arm link 811 rotated by the first driving shaft 121 rotates with respect to the second arm link 812 rotated by the second driving shaft 122 , the robot arm mechanism 101 can be contracted and extended.
According to the present invention, the first and second driving shafts 121 and 122 may be replaced by each other about the connection with the first arm link 811 , the second arm link 812 , or the first long link 212 .
According to the present invention, the fact that the fourth link 144 is integrally connected with the first long link 212 results in the fact that the fourth link 144 is at all times at a same angle to the center line 201 . This results in the fact that the second link 142 in parallel relation with the fourth link 144 is at all times at a same angle to the center line 201 . This results in the fact that the fourth link 164 integrally connected with the second link 142 is at all times at a same angle to the center line 201 . This results in the fact that the second link 162 in parallel relationship with the fourth link 164 is at all times at a same angle to the center line 201 . This results in the fact that the handling member 125 integrally formed with the second link 162 is at all times at a same angle to the center line 201 .
Referring to FIGS. 5 and 6 of the drawings, there is shown a second preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 102 is shown in FIGS. 5 and 6 as comprising a handling member 125 for supporting and handling an object.
The robot arm mechanism 102 further comprises a robot arm 820 connected to the handling member 125 . The robot arm 820 comprises a first arm link 821 having first and second end portion, a second arm link 822 having first and second end portion, and a link retaining mechanism 200 .
The link retaining mechanism 200 pivotably retains the first and second arm links 821 and 822 respectively at the first end portions of the first and second arm links 821 and 822 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link 821 and the second line being a line symmetrical with respect to the center line 201 with the line passing through the first and second end portions of the second arm link 822 . The first end portion of the first arm link 821 is integrally formed with the second short link 213 . The first end portion of the second arm link 822 is integrally formed with the second long link 224 . The first end portions of the first and second arm links 821 and 822 are positioned on the center line 201 . In fact the first and second arm links 821 and 822 are in symmetrical relationship with each other with respect to the center line 201 .
The robot arm 820 further comprises a third arm link 823 having first and second end portions. The third arm link 823 and the handling member 125 are pivotably connected with each other at the second end portion of the third arm link 823 and the first portion of the handling member 125 .
The robot arm 820 further comprises a fourth arm link 824 having first and second end portions. The fourth arm link 824 and the handling member 125 are pivotably connected with each other at the second end portion of the fourth arm link 824 and the second portion of the handling member 125 . The first and second arm links 821 and 822 are substantially equal in length to each other. The third and fourth arm links 823 and 824 are substantially equal in length to each other.
The robot arm 820 further comprises a first joint mechanism 140 retaining the first and third arm links 821 and 823 respectively at the second end portion of the first arm link 821 and the first end portion of the third arm link 823 under the state that the first arm link 821 is pivotable around the second end portion of the first arm link 821 with respect to the third arm link 823 . The second end portion of the first arm link 821 and the first end portion of the third arm link 823 are connected with each other. The first link 141 of the first joint mechanism 140 is substantially equal in length to the first arm link 821 . The first link 141 is integrally formed with and in coaxial relationship with the first arm link 821 under the state that the first end portion of the first link 141 is connected with the first end portion of the first arm link 821 . The second link 142 of the first joint mechanism 140 is pivotably connected with the first end portion of the third arm link 823 . The second end portion of the fourth link 144 of the first joint mechanism 140 is integrally connected with the first long link 212 .
The robot arm 820 further comprises a second joint mechanism 132 retaining the second and fourth arm links 822 and 824 respectively at the second end portion of the second arm link 822 and the first end portion of the fourth arm link 824 under the state that the second arm link 822 is pivotable around the second end portion of the second arm link 822 with respect to the fourth arm link 824 . The second end portion of the second arm link 822 and the first end portion of the fourth arm link 824 are connected with each other.
The robot arm 820 further comprises a stabilizing mechanism 170 similar to the stabilizing mechanism 160 in the first preferred embodiment of the robot arm mechanism according to the present invention. The stabilizing mechanism 170 includes first, second, third, and fourth links 171 , 172 , 173 , and 174 which are respectively similar to first, second, third, and fourth links 161 , 162 , 163 , and 164 in the first preferred embodiment of the robot arm mechanism according to the present invention. The stabilizing mechanism 170 and the stabilizing mechanism 160 in the first preferred embodiment are different from each other in the fact that the fourth link 174 has a set angle with respect to the second link 142 to prevent the state that the first and third links 171 and 173 are positioned on a straight line while the robot arm driving mechanism 120 drives the robot arm 820 .
The first link 171 is substantially equal in length to the third arm link 823 . The first link 171 is integrally formed with and in coaxial relationship with the third arm link 823 under the state that the first end portion of the first link 171 is connected with the first end portion of the third arm link 823 . The second link 172 is integrally formed with the handling member 125 . The second end portion of the fourth link 174 is integrally connected with the second link 142 .
The robot arm mechanism 102 further comprises a robot arm driving mechanism 120 for driving the robot arm 820 . The second driving shaft 122 of the arm driving mechanism 120 is integrally connected with the first long link 212 and rotates the first long link 212 around the rotation axis 123 . The first driving shaft 121 of the arm driving mechanism 120 is integrally connected with the first arm link 821 and rotates the first arm link 821 around the first end portion of the first arm link 821 .
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 212 and that the first driving shaft 121 is integrally connected with the first arm link 821 , the first driving shaft 121 may be integrally connected with the second arm link 822 instead of the first arm link 821 , according to the present invention.
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 212 and that the first driving shaft 121 is integrally connected with the first arm link 821 , the second driving shaft 122 may be integrally connected with the second arm link 822 instead of the first long link 212 , according to the present invention.
According to the present invention, the first and second driving shafts 121 and 122 may be replaced by each other about the connection with the first arm link 821 , the second arm link 822 , or the first long link 212 .
The operation of the robot arm mechanism 102 in the second preferred embodiment is similar to the operation of the robot arm mechanism 101 in the first preferred embodiment according to the present invention except for the fact that the stabilizing mechanism 170 prevents the state that the first and third links 171 and 173 are positioned on a straight line while the robot arm driving mechanism 120 drives the robot arm 820 .
Referring to FIGS. 7 and 8 of the drawings, there is shown a third preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 103 is shown in FIGS. 7 and 8 as comprising a handling member 125 for supporting and handling an object.
The robot arm mechanism 103 further comprises a robot arm 830 connected to the handling member 125 . The robot arm 830 comprises a first arm link 831 having first and second end portion, a second arm link 832 having first and second end portion, and a link retaining mechanism 300 having a center line 301 .
The link retaining mechanism 300 comprises first and second joint cross linkages 310 and 320 are respectively similar to the first and second joint cross linkages 210 and 220 in the first preferred embodiment of the robot arm mechanism according to the present invention. The first joint cross linkage 310 includes first short and long links 311 and 312 and second short and long links 313 and 314 which are respectively similar to first short and long links 211 and 212 and second short and long links 213 and 214 in the first preferred embodiment of the robot arm mechanism according to the present invention. The second joint cross linkage 320 includes first short and long links 321 and 322 and second short and long links 323 and 324 which are respectively similar to first short and long links 221 and 222 and second short and long links 223 and 224 in the first preferred embodiment of the robot arm mechanism according to the present invention.
The link retaining mechanism 300 similar to the link retaining mechanism 200 in the first preferred embodiment of the robot arm mechanism according to the present invention, except for the fact that the first long link 312 and the first short link 321 are differ in length from each other and the first short link 311 and the first long link 322 are substantially equal in length to each other.
The link retaining mechanism 300 pivotably retains the first and second arm links 831 and 832 respectively at the first end portions of the first and second arm links 831 and 832 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link 831 and the second line a line symmetrical with respect to the center line 301 with the line passing through the first and second end portions of the second arm link 832 .
The first end portion of the second arm link 832 is integrally formed with the second short link 313 . The first end portion of the first arm link 831 is integrally formed with the second long link 324 . The center line 301 passes through the first and second end portions of the first long link 312 . The first end portions of the first and second arm links 831 and 832 are positioned on the center line 301 .
The robot arm 830 further comprises a third arm link 833 having first and second end portions. The third arm link 833 and the handling member 125 are pivotably connected with each other at the second end portion of the third arm link 833 and the first portion of the handling member 125 .
The robot arm 830 further comprises a fourth arm link 834 having first and second end portions. The fourth arm link 834 and the handling member 125 are pivotably connected with each other at the second end portion of the fourth arm link 834 and the second portion of the handling member 125 . The first and second arm links 831 and 832 are substantially equal in length to each other. The third and fourth arm links 833 and 834 are substantially equal in length to each other.
The robot arm 830 further comprises a first joint mechanism 140 retaining the first and third arm links 831 and 833 respectively at the second end portion of the first arm link 831 and the first end portion of the third arm link 833 under the state that the first arm link 831 is pivotable around the second end portion of the first arm link 831 with respect to the third arm link 833 . The first link 141 of the first joint mechanism 140 is substantially equal in length to the first arm link 831 . The first link 141 is integrally formed with and in coaxial relationship with the first arm link 831 under the state that the first end portion of the first link 141 is connected with the first end portion of the first arm link 831 . The second link 142 of the first joint mechanism 140 is pivotably connected with the first end portion of the third arm link 833 . The second end portion of the fourth link 144 of the first joint mechanism 140 is integrally connected with the first long link 212 .
The robot arm 830 further comprises a second joint mechanism 150 similar to the first joint mechanism 140 and retaining the second and fourth arm links 832 and 834 respectively at the second end portion of the second arm link 832 and the first end portion of the fourth arm link 834 under the state that the second arm link 832 is pivotable around the second end portion of the second arm link 832 with respect to the fourth arm link 834 . The second joint mechanism 150 comprises the first, second, third, and fourth links 151 , 152 , 153 , and 154 which are respectively similar to the first, second, third, and fourth links 141 , 142 , 143 , and 144 . The first link 151 of the second joint mechanism 150 is substantially equal in length to the second arm link 832 . The first link 151 is integrally formed with and in coaxial relationship with the second arm link 832 under the state that the first end portion of the first link 151 is connected with the first end portion of the second arm link 832 . The second link 152 of the second joint mechanism 150 is pivotably connected with the first end portion of the fourth arm link 834 . The second end portion of the fourth link 154 of the second joint mechanism 150 is integrally connected with the first long link 212 .
The fourth links 144 and 154 are substantially equal in length to each other. The fourth links 144 and 154 are integrally formed with and in coaxial relationship with each other under the state that the first end portion of the fourth link 144 is connected with the first end portion of the fourth link 154 .
The robot arm 830 further comprises a stabilizing mechanism 160 . The first link 161 of the stabilizing mechanism 160 is substantially equal in length to the third arm link 833 . The first link 161 is integrally formed with and in coaxial relationship with the third arm link 833 under the state that the first end portion of the first link 161 is connected with the first end portion of the third arm link 833 . The second link 162 of the stabilizing mechanism 160 is integrally formed with the handling member 125 . The second end portion of the fourth link 164 of the stabilizing mechanism 160 is integrally connected with the second link 142 .
The robot arm mechanism 103 further comprises a robot arm driving mechanism 120 for driving the robot arm 830 .
The second driving shaft 122 of the robot arm driving mechanism 120 is integrally connected with the first long link 312 and rotates the first long link 312 around the rotation axis 123 . The first driving shaft 121 of the robot arm driving mechanism 120 is integrally connected with the third link 143 of the first joint mechanism 140 and rotates the first arm link 831 around the first end portion of the first arm link 831 through the first joint mechanism 140 .
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 312 and that the first driving shaft 121 is integrally connected with the third link 143 , the first driving shaft 121 may be integrally connected with the second arm link 832 instead of the third link 143 , according to the present invention.
While there have been described in the above about the fact that the second driving shaft 122 is integrally connected with the first long link 312 and that the first driving shaft 121 is integrally connected with the third link 143 , the second driving shaft 122 may be integrally connected with the second arm link 832 instead of the first long link 312 , according to the present invention.
According to the present invention, the first and second driving shafts 121 and 122 may be replaced by each other about the connection with the third link 143 , the second arm link 832 , or the first long link 312 .
The operation of the robot arm mechanism 103 in the third preferred embodiment is similar to the operation of the robot arm mechanism 101 in the first preferred embodiment except for the fact that the first and second joint mechanisms 140 and 150 firmly retains the first and second arm links 831 and 832 respectively, according to the present invention.
Referring to FIGS. 9 to 11 of the drawings, there is shown a fourth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 104 is shown in FIGS. 9 to 11 as comprising a handling member 125 for supporting and handling an object, a robot arm 840 , and a robot arm driving mechanism 120 for driving the robot arm 840 . The robot arm 840 comprises a driving assist parallelogram linkage 190 .
The robot arm 840 further comprises first, second, third, and fourth arm links 841 , 842 , 843 , and 844 which are similar to the first, second, third, and fourth arm links 831 , 832 , 833 , and 834 in the third preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm mechanism 104 is substantially similar to the robot arm mechanism 103 in the third preferred embodiment of the robot arm mechanism according to the present invention, except for the driving assist parallelogram linkage 190 of the robot arm 840 and the position of the robot arm driving mechanism 120 .
The driving assist parallelogram linkage 190 includes a first link 191 having first and second end portions and substantially equal in length to the distance between the rotation axis 123 and the second end portion of the second arm link 842 . The first link 191 is integrally formed with and in parallel relationship with the first long link 312 .
The driving assist parallelogram linkage 190 further includes a second link 192 having first and second end portions. The first and second links 191 and 192 are pivotably connected with each other at the second end portion of the first link 191 and the first end portion of the second link 192 . The second link 192 is integrally formed with and in parallel relationship with the second arm link 842 .
The driving assist parallelogram linkage 190 further includes a third link 193 having first and second end portions and substantially equal in length to the first link 191 . The second and third links 192 and 193 are pivotably connected with each other at the second end portion of the second link 192 and the first end portion of the third link 193 .
The driving assist parallelogram linkage 190 further includes a fourth link 194 having first and second end portions and substantially equal in length to the second link 192 . The third and fourth links 193 and 194 are pivotably connected with each other at the second end portion of the third link 193 and the first end portion of the fourth link 194 . The fourth and first links 194 and 191 are pivotably connected with each other at the second end portion of the fourth link 194 and the first end portion of the first link 191 under the state that the first link 191 is in parallel relationship with the third link 193 and that the second link 192 is in parallel relationship with the fourth link 194 .
The second driving shaft 122 is integrally connected with the fourth link 194 at the second end portion of the fourth link 194 and rotates the second arm link 842 around the first end portion of the second arm link 842 through the driving assist parallelogram linkage 190 . The first driving shaft 121 is integrally connected with the first long link 312 and rotates the first long link 312 around the rotation axis 123 .
According to the present invention, the first and second driving shafts 121 and 122 may be replaced by each other about the connection with the first long link 312 or the fourth link 194 .
The operation of the robot arm mechanism 104 in the fourth preferred embodiment is similar to the operation of the robot arm mechanism 103 in the third preferred embodiment except for the fact that the position of the arm driving mechanism 120 in the fourth preferred embodiment is different from the position of the arm driving mechanism 120 in the third preferred embodiment, according to the present invention.
Referring to FIGS. 12 and 13 of the drawings, there is shown a fifth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 105 is shown in FIGS. 12 and 13 as comprising a handling member 125 for supporting and handling an object, a robot arm 850 , and a robot arm driving mechanism 120 for driving the robot arm 850 . The robot arm 850 comprises a link retaining mechanism 350 .
The robot arm 850 further comprises first, second, third, and fourth arm links 851 , 852 , 853 , and 854 which are similar to the first, second, third, and fourth arm links 841 , 842 , 843 , and 844 in the fourth preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm mechanism 105 is substantially similar to the robot arm mechanism 104 in the fourth preferred embodiment of the robot arm mechanism according to the present invention.
The link retaining mechanism 350 comprises first and second joint cross linkages 360 and 370 which are respectively similar to the first and second joint cross linkages 310 and 320 in the fourth preferred embodiment of the robot arm mechanism according to the present invention. The first joint cross linkage 360 includes first short and long links 361 and 362 and second short and long links 363 and 364 which are respectively similar to first short and long links 311 and 312 and second short and long links 313 and 314 in the fourth preferred embodiment of the robot arm mechanism according to the present invention. The second joint cross linkage 370 includes first short and long links 371 and 372 and second short and long links 373 and 374 which are respectively similar to first short and long links 321 and 322 and second short and long links 323 and 324 in the fourth preferred embodiment of the robot arm mechanism according to the present invention.
The link retaining mechanism 350 similar to the link retaining mechanism 300 in the fourth preferred embodiment of the robot arm mechanism according to the present invention, except for the fact that the first short link 361 and the first long link 372 are not substantially equal in length to each other.
The retaining mechanism 300 pivotably retains the first and second arm links 831 and 832 respectively at the first end portions of the first and second arm links 831 and 832 and keeps parallel a first line and second line, the first line beign a line passing through the first and second end portions of the first arm link 831 and the second line a line symmetrical with respect to the center line 301 with the line passing through the first and second end portions of the second arm link 832 .
The first end portion of the first arm link 851 is integrally formed with the second short link 363 . The first end portion of the second arm link 852 is integrally formed with the second long link 374 . The center line 351 passes through the first and second end portions of the first long link 362 . The first end portions of the first and second arm links 851 and 852 are positioned on the center line 351 .
The second driving shaft 122 is integrally connected with the fourth link 194 at the second end portion of the fourth link 194 and rotates the second arm link 852 around the first end portion of the second arm link 852 through the driving assist parallelogram linkage 190 . The first driving shaft 121 is integrally connected with the first long link 362 and rotates the first long link 362 around the rotation axis 123 .
According to the present invention, the fourth link 194 and the first long link 362 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
The operation of the robot arm mechanism 105 in the fifth preferred embodiment is similar to the operation of the robot arm mechanism 104 in the fourth preferred embodiment, according to the present invention.
Referring to FIGS. 14 and 15 of the drawings, there is shown a sixth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 106 is shown in FIGS. 14 and 15 as comprising a handling member 125 for supporting and handling an object, a robot arm 860 , and a robot arm driving mechanism 120 for driving the robot arm 860 . The robot arm mechanism 106 is substantially similar to the robot arm mechanism 105 in the fifth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm 860 comprises first, second, third, and fourth arm links 861 , 862 , 863 , and 864 .
The stabilizing mechanism 160 in the fifth preferred embodiment of the robot arm mechanism according to the present invention is replaced by the stabilizing mechanism 170 in the present preferred embodiment.
The link retaining mechanism 350 in the fifth preferred embodiment of the robot arm mechanism according to the present invention is replaced by the link retaining mechanism 200 and an additional link retaining mechanism 250 in the present preferred embodiment.
The additional link retaining mechanism 250 comprises first and second joint cross linkages 260 and 270 are respectively similar to the first and second joint cross linkages 210 and 220 . The first joint cross linkage 260 includes first short and long links 261 and 262 and second short and long links 263 and 264 which are respectively similar to first short and long links 211 and, 212 and second short and long links 213 and 214 . The second joint cross linkage 270 includes first short and long links 271 and 272 and second short and long links 273 and 274 which are respectively similar to first short and long links 221 and 222 and second short and long links 223 and 224 .
The second driving shaft 122 is integrally connected with the fourth link 194 at the second end portion of the fourth link 194 and rotates the second arm link 862 around the first end portion of the second arm link 862 through the driving assist parallelogram linkage 190 . The first driving shaft 121 is integrally connected with the first link 191 and rotates the first long link 212 around the rotation axis 123 through the first link 191 .
According to the present invention, the fourth link 194 and the first link 191 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
The operation of the robot arm mechanism 106 in the sixth preferred embodiment is similar to the operation of the robot arm mechanism in the above-mentioned preferred embodiment, according to the present invention.
Referring to FIG. 16 of the drawings, there is shown a seventh preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 107 is shown in FIG. 16 as comprising a handling member 125 for supporting and handling an object, a robot arm 870 , and a robot arm driving mechanism 120 for driving the robot arm 870 . The robot arm mechanism 107 further comprises an additional handling member 126 for supporting and handling an object.
The robot arm 870 comprises first, second, third, and fourth arm links 871 , 872 , 873 , and 874 which are similar to the first, second, third, and fourth arm links 861 , 862 , 863 , and 864 in the sixth preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm 870 further comprises a fifth arm link 875 having first and second end portions. The additional handling member 126 has first and second portions. The fifth arm link 875 and the additional handling member 126 are pivotably connected with each other at the second end portion of the fifth arm link 875 and the first portion of the additional handling member 126 . The fifth arm link 875 is pivotably retained by the first joint mechanism 140 at the first end portion of the fifth arm link 875 .
The robot arm 870 further comprises a sixth arm link 876 having first and second end portions. The sixth arm link 876 and the additional handling member 126 are pivotably connected with each other at the second end portion of the sixth arm link 876 and the second portion of the additional handling member 126 . The fifth and sixth arm links 875 and 876 are substantially equal in length to each other. The sixth arm link 876 is pivotably retained by the second joint mechanism 150 at the first end portion of the sixth arm link 876 .
The robot arm 870 further comprises an additional stabilizing mechanism 180 similar to the stabilizing mechanism 170 .
The robot arm mechanism 107 is similar to the robot arm mechanism 106 in the sixth preferred embodiment of the robot arm mechanism according to the present invention, except for the additional the additional handling member 126 , fifth arm link 875 , sixth arm link 876 , and the additional stabilizing mechanism 180 .
The second driving shaft 122 is integrally connected with the fourth link 194 at the second end portion of the fourth link 194 and rotates the second arm link 872 around the first end portion of the second arm link 872 through the driving assist parallelogram linkage 190 (See FIG. 14 ).
The first driving shaft 121 is integrally connected with the first link 191 and rotates the first long link 212 around the rotation axis 123 through the first link 191 (See FIG. 14 ).
According to the present invention, the fourth link 194 and the first link 191 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
The operation of the robot arm mechanism 107 in the seventh preferred embodiment is similar to the operation of the robot arm mechanism 106 in the sixth preferred embodiment except for the following operation of the robot arm mechanism 107 in the seventh preferred embodiment.
The another handling member 126 approaches the rotation axis 123 when the handling member 125 leave from the rotation axis 123 , resulting from the fact that the robot arm mechanism 107 comprises the handling member 125 and the additional handling member 126 . By the same reason, the handling member 125 approaches the rotation axis 123 when the another handling member 126 leave from the rotation axis 123 .
Referring to FIG. 17 of the drawings, there is shown a eighth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 108 is shown in FIG. 17 as comprising a handling member 125 for supporting and handling an object, a robot arm 880 , and a robot arm driving mechanism 120 for driving the robot arm 880 .
The robot arm 880 comprises first, second, third, and fourth arm links 881 , 882 , 883 , and 884 which are similar to the first, second, third, and fourth arm links 821 , 822 , 823 , and 824 in the second preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm 880 further comprises the second joint mechanism 132 . The robot arm 880 further comprises the first joint mechanism 131 which is similar to the second joint mechanism 132 and retains the first and third arm links 881 and 883 .
The robot arm 880 further comprises a fifth arm link 885 having first and second end portion, a sixth arm link 886 having first and second end portion, and an additional link retaining mechanism 250 having an additional center line 251 . The additional link retaining mechanism 250 pivotably retains the fifth and sixth arm links 885 and 886 respectively at the first end portions of the fifth and sixth arm links 885 and 886 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the fifth arm link 885 and the second line being a line symmetrical with respect to the additional center line 251 with the line passing through the first and second end portions of the sixth arm link 886 . In fact the fifth and sixth arm links 885 and 886 are in symmetrical relationship with each other with respect to the center line 251 .
The first end portion of the sixth arm link 886 is integrally connected with the second short link 263 . The first end portion of the fifth arm link 885 is integrally connected with the second long link 274 .
The additional center line 251 passes through the first and second end portions of the first long link 262 . The first end portions of the fifth and sixth arm links 885 and 886 are positioned on the additional center line 251 .
The second end portion of the first arm link 881 and the first end portion of the third arm link 883 are connected with each other.
The second end portion of the second arm link 882 and the first end portion of the foruth arm link 884 are connected with each other.
The first long link 212 is integrally formed with and in parallel relationship with the first long link 262 under the state that the first end portion of the first long link 212 is connected with the first end portion of the first long link 262 .
The robot arm 880 further comprises a first stabilizing parallelogram linkage 230 comprising a first link 231 having first and second end portions and substantially equal in length to the first arm link 881 . The first link 231 is integrally formed with and in coaxial relationship with the first arm link 881 under the state that the first end portion of the first link 231 is connected with the first end portion of the first arm link 881 .
The first stabilizing parallelogram linkage 230 further comprises a second link 232 having first and second end portions and substantially equal in length to the fifth arm link 885 . The first and second links 231 and 232 are pivotably connected with each other at the second end portion of the first link 231 and the first end portion of the second link 232 . The second link 232 is integrally formed with and in parallel relationship with the third arm link 883 under the state that the first end portion of the second link 232 is connected with the first end portion of the third arm link 883 .
The first stabilizing parallelogram linkage 230 further comprises a third link 233 having first and second end portions and substantially equal in length to the first link 231 . The second and third links 232 and 233 are pivotably connected with each other at the second end portion of the second link 232 and the first end portion of the third link 233 .
The first stabilizing parallelogram linkage 230 further comprises a fourth link 234 having first and second end portions and substantially equal in length to the second link 232 . The third and fourth links 233 and 234 are pivotably connected with each other at the second end portion of the third link 233 and the first end portion of the fourth link 234 . The fourth and first links 234 and 231 are pivotably connected with each other at the second end portion of the fourth link 234 and the first end portion of the first link 231 under the state that the first link 231 is in parallel relationship with the third link 233 and that the second link 232 is in parallel relationship with the fourth link 234 . The fourth link 234 is integrally formed with and in coaxial relationship with the fifth arm link 885 under the state that the second end portion of the fourth link 234 is connected with the first end portion of the fifth arm link 885 .
The robot arm 880 further comprises a second stabilizing parallelogram linkage 240 which is similar to the first stabilizing parallelogram linkage 230 .
The second stabilizing parallelogram linkage 240 comprises first, second, third, and fourth links 241 , 242 , 243 , and 244 which are respectively similar to the first, second, third, and fourth links 231 , 232 , 233 , and 234 .
The first link 241 is substantially equal in length to the second arm link 882 . The first link 241 is integrally formed with and in coaxial relationship with the second arm link 882 under the state that the first end portion of the first link 241 is connected with the first end portion of the second arm link 882 .
The second stabilizing parallelogram linkage 240 further comprises a second link 242 having first and second end portions and substantially equal in length to the sixth arm link 886 . The second link 242 is integrally formed with and in parallel relationship with the fourth arm link 884 under the state that the first end portion of the second link 242 is connected with the first end portion of the fourth arm link 884 .
The third link 243 is substantially equal in length to the first link 241 . The fourth link 244 is substantially equal in length to the second link 242 . The fourth link 244 is integrally formed with and in coaxial relationship with the sixth arm link 886 under the state that the second end portion of the fourth link 244 is connected with the first end portion of the sixth arm link 886 .
The second driving shaft 122 is integrally connected with the first arm link 881 at the first end portion of the first arm link 881 and rotates the first arm link 881 around the rotation axis 123 . The first driving shaft 121 is integrally connected with the second arm link 882 at the first end portion of the second arm link 882 and rotates the second arm link 882 around the rotation axis 123 .
According to the present invention, the first and second arm links 881 and 882 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
The operation of the robot arm mechanism 108 in the eighth preferred embodiment is similar to the operation of the robot arm mechanism 101 in the first preferred embodiment except for the following operation of the robot arm mechanism 108 , according to the present invention.
According to the present invention, the fact that the fifth and sixth arm links 885 and 886 are retained by the additional link retaining member 250 results in the fact that the fifth and sixth arm links 885 and 886 are in symmetrical relationship with each other with respect to the center line 201 . The first stabilizing parallelogram linkage 230 makes the third and fifth arm links 883 and 885 in parallel relationship with each other. The second stabilizing parallelogram linkage 240 makes the fourth and sixth arm links 884 and 886 in parallel relationship with each other. The third and fourth arm links 883 and 884 are in symmetrical relationship with each other with respect to the center line 201 , resulting from the fact that the third and fourth arm links 883 and 884 are respectively in parallel relationship with the fifth and sixth arm links 885 and 886 . The handling member 125 moves parallel to the center line 201 , by the reason that the third and fourth arm links 883 and 884 are in symmetrical relationship with each other with respect to the center line 201 .
Referring to FIGS. 18 and 19 of the drawings, there is shown a ninth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 109 is shown in FIGS. 18 and 19 as comprising a handling member 127 for supporting and handling an object.
The robot arm mechanism 109 further comprises a robot arm 890 connected to the handling member 127 . The robot arm 890 comprises a first arm link 891 having first and second end portion, a second arm link 892 having first and second end portion, and a link retaining mechanism 400 having a center line 401 .
The link retaining mechanism 400 pivotably retains the first and second arm links 891 and 892 respectively at the first end portions of the first and second arm links 891 and 892 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link 891 and the second line being a line symmetrical with respect to the center line 401 with the line passing through the first and second end portions of the second arm link 892 . In fact the first and second arm links 891 and 892 are in symmetrical relationship with each other with respect to the center line 401 .
The link retaining mechanism 400 comprises a first joint cross linkage 410 which includes a first short link 411 having first and second end portions.
The first joint cross linkage 410 further includes a first long link 412 having first and second end portions and longer than the first short link 411 . The first short and long links 411 and 412 are pivotably connected with each other at the second end portion of the first short link 411 and the first end portion of the first long link 412 .
The first joint cross linkage 410 further includes a second short link 413 having first and second end portions and substantially equal in length to the first short link 411 . The first long link 412 and the second short link 413 are pivotably connected with each other at the second end portion of the first long link 412 and the first end portion of the second short link 413 .
The first joint cross linkage 410 further includes a second long 414 link having first and second end portions and substantially equal in length to the first long link 412 . The second short and long links 413 and 414 are pivotably connected with each other at the second end portion of the second short link 413 and the first end portion of the second long link 414 .
The second long link 414 and the first short link 411 are pivotably connected with each other at the second end portion of the second long link 414 and the first end portion of the first short link 411 under the state that the second long link 414 is crossed with the first long link 412 .
The link retaining mechanism 400 comprises a second joint cross linkage 420 which includes a first short link 421 having first and second end portions.
The second joint cross linkage 420 further includes a first long link 422 having first and second end portions and longer than the first short link 421 . The first short and long links 421 and 422 are pivotably connected with each other at the second end portion of the first short link 421 and the first end portion of the first long link 422 .
The second joint cross linkage 420 further includes a second short link 423 having first and second end portions and substantially equal in length to the first short link 421 . The first long link 422 and the second short link 423 are pivotably connected with each other at the second end portion of the first long link 422 and the first end portion of the second short link 423 .
The second joint cross linkage 420 further includes a second long link 424 having first and second end portions and substantially equal in length to the first long link 422 . The second short and long links 423 and 424 are pivotably connected with each other at the second end portion of the second short link 423 and the first end portion of the second long link 424 .
The second long link 424 and the first short link 421 are pivotably connected with each other at the second end portion of the second long link 424 and the first end portion of the first short link 421 under the state that the second long link 424 is crossed with the first long link 422 .
The length ratio of each of the first and second short links 411 and 413 to each of the first and second long links 412 and 414 is substantially equal to the length ratio of each of the first and second short links 421 and 423 to each of the first and second long links 422 and 424 .
The first short link 411 is integrally formed with and in coaxial relationship with the first long link 422 under the state that the second end portion of the first short link 411 is connected with the first end portion of the first long link 422 . The first long link 412 is integrally formed with and in coaxial relationship with the first short link 421 under the state that the first end portion of the first long link 412 is connected with the second end portion of the first short link 421 .
The first end portion of the first arm link 891 is integrally formed with the second short link 413 . The first end portion of the second arm link 892 is integrally formed with the second long link 424 .
The center line 401 is substantially equally spaced apart from the second end portion of the first long link 412 and the first end portion of the first short link 421 and in perpendicular relationship with the first long link 412 . The first end portions of the first and second arm links 891 and 892 are positioned on the line passing through the first and second end portions of the first long link 412 .
The robot arm 890 further comprises a third arm link 893 having first and second end portions.
The robot arm 890 further comprises a fourth arm link 894 having first and second end portions. The first and second arm links 891 and 892 are substantially equal in length to each other. The third and fourth arm links 893 and 894 are substantially equal in length to each other.
The robot arm 890 further comprises a first joint mechanism 131 retaining the first and third arm links 891 and 893 respectively at the second end portion of the first arm link 891 and the first end portion of the third arm link 893 under the state that the first arm link 891 is pivotable around the second end portion of the first arm link 891 with respect to the third arm link 893 . The first and third arm links 811 and 813 are pivotably connected with each other at the second end portion of the first arm link 811 and the first end portion of the third arm link 813 .
The robot arm 890 further comprises a second joint mechanism 132 retaining the second and fourth arm links 892 and 894 respectively at the second end portion of the second arm link 892 and the first end portion of the fourth arm link 894 under the state that the second arm link 892 is pivotable around the second end portion of the second arm link 892 with respect to the fourth arm link 894 . The second and fourth arm links 812 and 814 are pivotably connected with each other at the second end portion of the second arm link 812 and the first end portion of the fourth arm link 814 .
The handling member 127 is integrally connected with the first long link 412 .
The robot arm mechanism 109 further comprises a robot arm driving mechanism 120 for driving the robot arm 890 .
The arm driving mechanism 120 comprises a first driving shaft 121 rotatable around a rotation axis 123 , and a second driving shaft 122 in the form of a hollow shape to rotatably receive therein the first driving shaft 121 and rotatable around the rotation axis 123 . The first driving shaft 121 is integrally connected with the second end portion of the third arm link 893 and rotating the third arm link 893 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fourth arm link 894 and rotating the fourth arm link 894 around the rotation axis 123 .
According to the present invention, the center line 401 passes through the rotation axis 123 at all times, by the reason that the link retaining mechanism 400 retains the first and second arm links 891 and 892 under the state that the first and second arm links 891 and 892 are in symmetrical relationship with each other with respect to the center line 401 , that the first and second arm links 891 and 892 are equal in length to each other, and that the third and fourth arm links 893 and 894 are equal in length to each other. By the reason that the center line 401 passes through the rotation axis 123 at all times, The handling member 127 approaches and leaves from the rotation axis 123 with keeping a direction with respect to the rotation axis 123 fixed.
According to the present invention, the rotation of the third arm link 893 and the rotation of the fourth arm link 894 can result in the rotation of the center line 401 around the rotation axis 123 . The robot arm mechanism 109 is rotated around the rotation axis 123 by the reason that the center line 401 is rotated around the rotation axis 123 .
According to the present invention, the third and fourth arm links 893 and 894 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
Referring to FIGS. 20 to 21 of the drawings, there is shown a tenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 110 is shown in FIGS. 20 to 21 as comprising a handling member 125 for supporting and handling an object.
The construction of the robot arm mechanism 110 in the present preferred embodiment is similar to the construction of the robot arm mechanism 109 in the ninth preferred embodiment except for the following construction of the robot arm mechanism 110 in the present preferred embodiment.
The robot arm mechanism 110 further comprises a robot arm 900 connected to the handling member 125 . The robot arm 900 comprises a first arm link 901 having first and second end portion, a second arm link 902 having first and second end portion, and a link retaining mechanism 500 having a center line 501 .
The link retaining mechanism 500 pivotably retains the first and second arm links 901 and 902 respectively at the first end portions of the first and second arm links 901 and 902 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the first arm link 901 and the second line being a line symmetrical with respect to the center line 501 with the line passing through the first and second end portions of the second arm link 902 . In fact the first and second arm links 901 and 902 are in symmetrical relationship with each other with respect to the center line 501 .
The link retaining mechanism 500 comprises a first joint cross linkage 510 which includes a first short link 511 having first and second end portions.
The first joint cross linkage 510 further includes a first long link 512 having first and second end portions and longer than the first short link 511 . The first short and long links 511 and 512 are pivotably connected with each other at the second end portion of the first short link 511 and the first end portion of the first long link 512 .
The first joint cross linkage 510 further includes a second short link 513 having first and second end portions and substantially equal in length to the first short link 511 . The first long link 512 and the second short link 513 are pivotably connected with each other at the second end portion of the first long link 512 and the first end portion of the second short link 513 .
The first joint cross linkage 510 further includes a second long 514 link having first and second end portions and substantially equal in length to the first long link 512 . The second short and long links 513 and 514 are pivotably connected with each other at the second end portion of the second short link 513 and the first end portion of the second long link 514 .
The second long link 514 and the first short link 511 are pivotably connected with each other at the second end portion of the second long link 514 and the first end portion of the first short link 511 under the state that the second long link 514 is crossed with the first long link 512 .
The link retaining mechanism 500 comprises a second joint cross linkage 520 which includes a first short link 521 having first and second end portions.
The second joint cross linkage 520 further includes a first long link 522 having first and second end portions and longer than the first short link 521 . The first short and long links 521 and 522 are pivotably connected with each other at the second end portion of the first short link 521 and the first end portion of the first long link 522 .
The second joint cross linkage 520 further includes a second short link 523 having first and second end portions and substantially equal in length to the first short link 521 . The first long link 522 and the second short link 523 are pivotably connected with each other at the second end portion of the first long link 522 and the first end portion of the second short link 523 .
The second joint cross linkage 520 further includes a second long link 524 having first and second end portions and substantially equal in length to the first long link 522 . The second short and long links 523 and 524 are pivotably connected with each other at the second end portion of the second short link 523 and the first end portion of the second long link 524 .
The second long link 524 and the first short link 521 are pivotably connected with each other at the second end portion of the second long link 524 and the first end portion of the first short link 521 under the state that the second long link 524 is crossed with the first long link 522 .
The length ratio of each of the first and second short links 511 and 513 to each of the first and second long links 512 and 514 is substantially equal to the length ratio of each of the first and second short links 521 and 523 to each of the first and second long links 522 and 524 .
The first short link 511 is integrally formed with and in axial alignment with the first long link 522 under the state that the second end portion of the first short link 511 is connected with the first end portion of the first long link 522 . The first long link 512 is integrally formed with and in axial alignment with the first short link 521 under the state that the first end portion of the first long link 512 is connected with the second end portion of the first short link 521 .
The first end portion of the first arm link 901 is integrally formed with the second short link 513 . The first end portion of the second arm link 902 is integrally formed with the second long link 524 . The center line 501 is substantially equally spaced apart from the second end portion of the first long link 512 and the first end portion of the first short link 521 and in perpendicular relationship with the first long link 512 . The first end portions of the first and second arm links 901 and 902 are positioned on the line passing through the first and second end portions of the first long link 512 . In prevent preferred embodiment the first and second arm links 901 and 902 are respectively integrally formed with and in coaxial relationship with the second short link 513 and the second long link 524 .
The robot arm further comprises third and fourth arm links 903 and 904 which are similar to the third and fourth arm links 893 and 894 in the ninth preferred embodiment of the robot arm mechanism according to the present invention.
The first driving shaft 121 is integrally connected with the second end portion of the fourth arm link 904 and rotating the fourth arm link 904 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the third arm link 903 and rotating the third arm link 903 around the rotation axis 123 .
According to the present invention, the third and fourth arm links 903 and 904 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 110 in the tenth preferred embodiment is substantially similar to the operation of the robot arm mechanism 109 in the ninth preferred embodiment.
Referring to FIGS. 20 and 22 of the drawings, there is shown a eleventh preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 111 is shown in FIGS. 20 and 22 as comprising a handling member 125 for supporting and handling an object and a robot arm 910 .
The robot arm 910 comprises first, second, third, and fourth arm link 911 , 912 , 913 , and 914 which are similar to the first, second, third, and fourth arm link 901 ,. 902 , 903 , and 904 in the tenth preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm 910 further comprises a fifth arm link 915 having first and second end portions. The robot arm 910 further comprises a sixth arm link 916 having first and second end portions. The fifth and sixth arm link 915 and 916 substantially equal in length to each other.
The robot arm 910 further comprises a first stabilizing mechanism 610 including a first link 611 having first and second end portions. The first link 611 is integrally formed with and in coaxial relationship with the first arm link 911 under the state that the second end portion of the first link 611 is connected with the second end portion of the first arm link 911 .
The first stabilizing mechanism 610 includes a second link 612 having first and second end portions. The first and second links 611 and 612 are pivotably connected with each other at the second end portion of the first link 611 and the first end portion of the second link 612 . The second link 612 is integrally formed with and in axial alignment with the third arm link 913 under the state that the first end portion of the second link 612 is connected with the second end portion of the third arm link 913 .
The first stabilizing mechanism 610 includes a third link 613 having first and second end portions and substantially equal in length to the first link 611 . The second and third links 612 and 613 are pivotably connected with each other at the second end portion of the second link 612 and the first end portion of the third link 613 . The third link 613 is integrally formed with and in parallel relationship with the fifth arm link 915 under the state that the first end portion of the third link 613 is connected with the second end portion of the fifth arm link 915 .
The first stabilizing mechanism 610 includes a fourth link 614 having first and second end portions and substantially equal in length to the second link 612 . The third and fourth links 613 and 614 are pivotably connected with each other at the second end portion of the third link 613 and the first end portion of the fourth link 614 . The fourth and first links 614 and 611 are pivotably connected with each other at the second end portion of the fourth link 614 and the first end portion of the first link 611 under the state that the first link 611 is in parallel relationship with the third link 613 and that the second link 612 is in parallel relationship with the fourth link 614 .
The robot arm 910 further comprises a second stabilizing mechanism 620 which is similar to the first stabilizing mechanism 610 . The first link 621 is integrally formed with and in coaxial relationship with the second arm link 912 under the state that the second end portion of the first link 621 is connected with the second end portion of the second arm link 912 . The second link 622 is integrally formed with and in axial alignment with the fourth arm link 914 under the state that the first end portion of the second link 622 is connected with the second end portion of the fourth arm link 914 . The third link 623 is integrally formed with and in parallel relationship with the sixth arm link 916 under the state that the first end portion of the third link 623 is connected with the second end portion of the sixth arm link 916 .
The handling member 125 has first and second portions. The fifth arm link 915 and the handling member 125 are pivotably connected with each other at the first end portion of the fifth arm link 915 and the first portion of the handling member 125 . The sixth arm link 916 and the handling member 125 are pivotably connected with each other at the first end portion of the sixth arm link 916 and the second portion of the handling member 125 .
The first driving shaft 121 is integrally connected with the second end portion of the third arm link 913 and rotating the third arm link 913 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fourth arm link 914 and rotating the fourth arm link 914 around the rotation axis 123 .
According to the present invention, the third and fourth arm links 913 and 914 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 111 in the eleventh preferred embodiment is similar to the operation of the robot arm mechanism 110 in the tenth preferred embodiment.
Referring to FIGS. 20 and 23 of the drawings, there is shown a twelfth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 111 is shown in FIGS. 20 and 23 as comprising a handling member 125 for supporting and handling an object and a robot arm 920 .
The robot arm 920 comprises first, second, third, and fourth arm link 921 , 922 , 923 , and 924 which are similar to the first, second, third, and fourth arm link 901 , 902 , 903 , and 904 in the tenth preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm 920 further comprises a fifth arm link 925 having first and second end portions. The robot arm 920 further comprises a sixth arm link 926 having first and second end portions. The fifth and sixth arm link 925 and 926 substantially equal in length to each other.
The robot arm 920 further comprises a first stabilizing mechanism 630 including a first link 631 having first and second end portions. The first link 631 is integrally formed with and in axial alignment with the first arm link 921 under the state that the second end portion of the first link 631 is connected with the second end portion of the first arm link 921 .
The first stabilizing mechanism 630 includes a second link 632 having first and second end portions. The first and second links 631 and 632 are pivotably connected with each other at the second end portion of the first link 631 and the first end portion of the second link 632 . The second link 632 is integrally formed with and in axial alignment with the third arm link 923 under the state that the first end portion of the second link 632 is connected with the second end portion of the third arm link 923 .
The first stabilizing mechanism 630 includes a third link 633 having first and second end portions and substantially equal in length to the first link 631 . The second and third links 632 and 633 are pivotably connected with each other at the second end portion of the second link 632 and the first end portion of the third link 633 . The third link 633 is integrally formed with and in parallel relationship with the fifth arm link 925 under the state that the first end portion of the third link 633 is connected with the second end portion of the fifth arm link 925 .
The first stabilizing mechanism 630 includes a fourth link 634 having first and second end portions and substantially equal in length to the second link 632 . The third and fourth links 633 and 634 are pivotably connected with each other at the second end portion of the third link 633 and the first end portion of the fourth link 634 . The fourth and first links 634 and 631 are pivotably connected with each other at the second end portion of the fourth link 634 and the first end portion of the first link 631 under the state that the first link 631 is in parallel relationship with the third link 633 and that the second link 632 is in parallel relationship with the fourth link 634 .
The robot arm 920 further comprises a second stabilizing mechanism 640 which is similar to the first stabilizing mechanism 630 . The first link 641 is integrally formed with and in axial alignment with the second arm link 922 under the state that the second end portion of the first link 641 is connected with the second end portion of the second arm link 922 . The second link 642 is integrally formed with and in axial alignment with the fourth arm link 924 under the state that the first end portion of the second link 642 is connected with the second end portion of the fourth arm link 924 . The third link 643 is integrally formed with and in parallel relationship with the sixth arm link 926 under the state that the first end portion of the third link 643 is connected with the second end portion of the sixth arm link 926 .
The handling member 125 has first and second portions. The fifth arm link 925 and the handling member 125 are pivotably connected with each other at the first end portion of the fifth arm link 925 and the first portion of the handling member 125 . The sixth arm link 926 and the handling member 125 are pivotably connected with each other at the first end portion of the sixth arm link 926 and the second portion of the handling member 125 .
The first driving shaft 121 is integrally connected with the second end portion of the third arm link 923 and rotating the third arm link 923 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fourth arm link 924 and rotating the fourth arm link 924 around the rotation axis 123 .
According to the present invention, the third and fourth arm links 923 and 924 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 112 in the twelfth preferred embodiment is similar to the operation of the robot arm mechanism 110 in the tenth preferred embodiment.
Referring to FIGS. 18 and 24 of the drawings, there is shown a thirteenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 113 is shown in FIGS. 18 and 24 as comprising a handling member 127 and a robot arm 930 .
The construction of the robot arm mechanism 113 in the present preferred embodiment is similar to the construction of the robot arm mechanism 109 in the ninth preferred embodiment except for the following construction of the robot arm mechanism 113 in the present preferred embodiment.
The robot arm 930 comprises first, second, third, and fourth arm links 931 , 932 , 933 , and 934 which are similar to the first, second, third, and fourth arm links 891 , 892 , 893 , and 894 in the ninth preferred embodiment of the robot arm mechanism according to the present invention (See FIG. 19 ).
The robot arm mechanism 113 further comprises an additional handling member 128 . The robot arm 930 further comprises a fifth arm link 935 having first and second end portion and a sixth arm link 936 having first and second end portion. The fifth and sixth arm links 935 and 936 are substantially equal in length to each other.
The robot arm 930 further comprises an additional link retaining mechanism 450 having an additional center line 451 . The additional link retaining mechanism 450 pivotably retainins the fifth and sixth arm links 935 and 936 respectively at the first end portions of the fifth and sixth arm links 935 and 936 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the fifth arm link 935 and the second line being a line symmetrical with respect to the additional center line 451 with the line passing through the first and second end portions of the sixth arm link 936 . In fact the fifth and sixth arm links 935 and 936 are in symmetrical relationship with each other with respect to the additional center line 451 .
The first end portion of the sixth arm link 936 is integrally connected with the second short link 463 . The first end portion of the fifth arm link 935 is integrally connected with the second long link 474 .
The first end portions of the fifth and sixth arm links 935 and 936 are positioned on the line passing through the first and second end portions of the first long link 462 .
The distance between the second end portion of the first long link 412 and the first end portion of the first short link 421 is substantially equal to the distance between the second end portion of the first long link 462 and the first end portion of the first short link 471 .
The first joint mechanism 601 retains the third arm link 933 at the first end portion of the third arm link 933 . The first joint mechanism 601 retains the first and fifth arm links 931 and 935 respectively at the second end portions of the first and fifth arm links 931 and 935 under the state that the first and fifth arm links 931 and 935 are pivotable respectively around the second end portions of the first and fifth arm links 931 and 935 with respect to the third arm link 933 .
The second joint mechanism 602 retains the fourth arm link 934 at the first end portion of the fourth arm link 934 . The second joint mechanism 602 retains the second and sixth arm links 932 and 936 respectively at the second end portions of the second and sixth arm links 932 and 936 under the state that the second and sixth arm links 932 and 936 are pivotable respectively around the second end portions of the second and sixth arm links 932 and 936 with respect to the fourth arm link 934 .
The additional handling member 128 is integrally connected with the first long link 462 .
The first joint mechanism 601 is formed by a link and has first and second end portions. The third arm link 933 is integrally connected with the first joint mechanism 601 at the portion substantially equally spaced apart from the first and second end portions of the first joint mechanism 601 under the state that first joint mechanism 601 and the third arm link 933 are in perpendicular relationship with each other. The first arm link 931 and the first joint mechanism 601 is pivotably connected with each other at the second end portion of the first arm link 931 and the first end portion of the first joint mechanism 601 . The fifth arm link 935 and the first joint mechanism 601 is pivotably connected with each other at the second end portion of the fifth arm link 935 and the second end portion of the first joint mechanism 601 . The second joint mechanism 602 is formed by a link and has first and second end portions. The fourth arm link 934 is integrally connected with the second joint mechanism 602 at the portion substantially equally spaced apart from the first and second end portions of the second joint mechanism 602 under the state that second joint mechanism 602 and the fourth arm link 934 are in perpendicular relationship with each other. The second arm link 932 and the second joint mechanism 602 is pivotably connected with each other at the second end portion of the second arm link 932 and the first end portion of the second joint mechanism 602 . The sixth arm link 936 and the second joint mechanism 602 are pivotably connected with each other at the second end portion of the sixth arm link 936 and the second end portion of the second joint mechanism 602 .
The first driving shaft 121 is integrally connected with the second end portion of the third arm link 933 and rotating the third arm link 933 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fourth arm link 934 and rotating the fourth arm link 934 around the rotation axis 123 .
According to the present invention, the third and fourth arm links 933 and 934 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 113 in the thirteenth preferred embodiment is similar to the operation of the robot arm mechanism 109 in the ninth preferred embodiment except for the following operation of the robot arm mechanism 113 in the thirteenth preferred embodiment.
By the reason that the robot arm mechanism 113 comprises the handling member 127 and the additional handling member 128 , the handling member 127 leaves from the rotation axis 123 when the additional handling member 128 approaches the rotation axis 123 . Similarly, the additional handling member 128 leaves from the rotation axis 123 when the handling member 127 approaches the rotation axis 123 .
Referring to FIGS. 18 and 25 of the drawings, there is shown a fourteenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 114 is shown in FIGS. 18 and 25 as comprising a handling member 127 and a robot arm 940 .
The construction of the robot arm mechanism 114 in the present preferred embodiment is similar to the construction of the robot arm mechanism 109 in the ninth preferred embodiment except for the following construction of the robot arm mechanism 114 in the present preferred embodiment.
The robot arm 940 comprises first, second, third, and fourth arm links 941 , 942 , 943 , and 944 which are similar to first, second, third, and fourth arm links 891 , 892 , 893 , and 894 in the ninth preferred embodiment of the robot arm mechanism according to the present invention (See FIG. 19 ).
The robot arm mechanism 114 further comprises an additional handling member 128 . The robot arm 940 further comprises a fifth arm link 945 having first and second end portion, a sixth arm link 946 having first and second end portion, a seventh arm link 947 having first and second end portion, and a eighth arm link 948 having first and second end portion. The fifth and sixth arm links 945 and 946 are substantially equal in length to each other. The seventh and eighth arm links 947 and 948 are substantially equal in length to each other.
The robot arm 940 further comprises a third joint mechanism 133 retaining the fifth and seventh arm links 945 and 947 respectively at the second end portion of the fifth arm link 945 and the first end portion of the seventh arm link 947 under the state that the fifth arm link 945 is pivotable around the second end portion of the fifth arm link 945 with respect to the seventh arm link 947 . The robot arm 940 further comprises a fourth joint mechanism 134 retaining the sixth and eighth arm links 946 and 948 respectively at the second end portion of the sixth arm link 946 and the first end portion of the eighth arm link 948 under the state that the sixth arm link 946 is pivotable around the second end portion of the sixth arm link 946 with respect to the eighth arm link 948 .
The robot arm 940 further comprises an additional link retaining mechanism 450 having an additional center line 451 . The additional link retaining mechanism 450 pivotably retains the fifth and sixth arm links 945 and 946 respectively at the first end portions of the fifth and sixth arm links 945 and 946 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the fifth arm link 945 and the second line being a line symmetrical with respect to the additional center line 451 with the line passing through the first and second end portions of the sixth arm link 946 . In fact the fifth and sixth arm links 945 and 946 are in symmetrical relationship with each other with respect to the additional center line 451 .
The additional link retaining mechanism 450 are similar to the link retaining mechanism 400 .
The first end portion of the fifth arm link 945 is integrally connected with the second short link 463 (See FIG. 18 ). The first end portion of the sixth arm link 946 is integrally connected with the second long link 474 (See FIG. 18 ). The first end portions of the fifth and sixth arm links 945 and 946 are positioned on the line passing through the first and second end portions of the first long link 462 .
The distance between the second end portion of the first long link 412 and the first end portion of the first short link 421 is substantially equal to the distance between the second end portion of the first long link 462 and the first end portion of the first short link 471 .
The first driving shaft 121 is integrally connected with the second end portion of the third arm link 943 and rotating the third arm link 943 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fourth arm link 944 and rotating the fourth arm link 944 around the rotation axis 123 .
The first driving shaft 121 rotates the eighth arm link 948 around the second end portion of the eighth arm link 948 . The second driving shaft 122 rotates the seventh arm link 947 around the second end portion of the seventh arm link 947 . The second end portions of the eighth and seventh arm links 948 and 947 are positioned on the rotation axis 943 .
In prevent preferred embodiment the third and fourth arm links 943 and 944 are respectively in axial alignment with the eighth and seventh arm links 948 and 947 .
The additional handling member 128 is integrally connected with the first long link 462 .
According to the present invention, the third and fourth arm links 943 and 944 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 . Similarly, the seventh and eighth arm links 947 and 948 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 114 in the fourteenth preferred embodiment is similar to the operation of the robot arm mechanism 109 in the ninth preferred embodiment except for the following operation of the robot arm mechanism 114 .
By the reason that the robot arm mechanism 114 comprises the handling member 127 and the additional handling member 128 , the handling member 127 leaves from the rotation axis 123 when the additional handling member 128 approaches the rotation axis 123 . Similarly, the additional handling member 128 leaves from the rotation axis 123 when the handling member 127 approaches the rotation axis 123 .
Referring to FIGS. 26 and 27 of the drawings, there is shown a fifteenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 115 is shown in FIGS. 26 and 27 as comprising a handling member 125 and a robot arm 950 .
The robot arm 950 comprises first, second, third, and fourth arm links 951 , 952 , 953 , and 954 which are similar to first, second, third, and fourth arm links 901 , 902 , 903 , and 904 in the tenth preferred embodiment of the robot arm mechanism according to the present invention.
The robot arm mechanism 115 further comprises an additional handling member 126 . The robot arm 950 further comprises a third arm link 950 having first and second end portion and a fourth arm link 954 having first and second end portion. The first, second, third, and fourth arm links 951 , 952 , 953 , and 954 are substantially equal in length to each other.
The robot arm 950 further comprises a link retaining mechanism 400 having a center line 400 .
The robot arm 950 further comprises a fifth arm link 955 having first and second end portion and a sixth arm link 956 having first and second end portion. The robot arm 950 further comprises an additional link retaining mechanism 450 having an additional center line 451 . The additional link retaining mechanism 450 pivotably retains the third and fourth arm links 953 and 954 respectively at the first end portions of the third and fourth arm links 953 and 954 and keeps parallel a first line and a second line, the first line being a line passing through the first and second end portions of the third arm link 953 and the second line being a line symmetrical with respect to the additional center line 451 with the line passing through the first and second end portions of the fourth arm link 954 . In fact the third and fourth arm links 953 and 954 are in symmetrical relationship with each other with respect to the additional link retaining mechanism 450 .
The first end portion of the first arm link 951 is integrally connected with the second short link 413 . The first end portion of the second arm link 952 is integrally connected with the second long link 424 . The first end portion of the third arm link 953 is integrally connected with the second short link 463 . The first end portion of the fourth arm link 954 is integrally connected with the second long link 474 .
The distance between the second end portion of the first long link 412 and the first end portion of the first short link 421 is substantially equal to the distance between the second end portion of the first long link 462 and the first end portion of the first short link 471 .
The handling member 125 has a first and second portions. The additional handling member 126 has a first and second portions. The first arm link 951 and the handling member 125 are pivotably connected with each other at the second end portion of the first arm link 951 and the first portion of the handling member 125 . The third arm link 953 and the handling member 125 are pivotably connected with each other at the second end portion of the third arm link 953 and the second portion of the handling member 125 . The fourth arm link 954 and the additional handling member 126 are pivotably connected with each other at the second end portion of the fourth arm link 954 and the first portion of the additional handling member 126 . The second arm link 952 and the additional handling member 126 are pivotably connected with each other at the second end portion of the second arm link 952 and the second portion of the additional handling member 126 . The arm driving mechanism 120 comprises a first driving shaft 121 rotatable around a rotation axis 123 , and a second driving shaft 122 in the form of a hollow shape to rotatably receive therein the first driving shaft 121 and rotatable around the rotation axis 123 . The first driving shaft 121 rotates the fifth arm link 955 around the second end portion of the fifth arm link 955 . The second driving shaft 122 rotates the sixth arm link 956 around the second end portion of the sixth arm link 956 . The second end portions of the fifth and sixth arm links 955 and 956 are positioned on the rotation axis 123 . The fifth arm link 955 is pivotable around the second end portion of the fifth arm link 955 . The sixth arm link 956 is pivotable around the second end portion of the sixth arm link 956 . The first end portion of the fifth arm link 955 is pivotally connected with the first long link 412 under the state that the first end portion of the fifth arm link 955 is substantially equally spaced apart from the second end portion of the first long link 412 and the first end portion of the first short link 421 . The first end portion of the sixth arm link 956 is pivotally connected with the first long link 462 under the state that the first end portion of the sixth arm link 956 is substantially equally spaced apart from the second end portion of the first long link 462 and the first end portion of the first short link 471 .
The robot arm 950 further comprises a stabilizing mechanism 650 which includes a first link 651 having first and second end portions and substantially equal in length to the first arm link 951 . The first link 651 is integrally formed with and in coaxial relationship with the first arm link 951 under the state that the first end portion of the first link 651 is connected with the first end portion of the first arm link 951 .
The stabilizing mechanism 650 further includes a second link 652 having first and second end portions. The first and second links 651 and 652 are pivotably connected with each other at the second end portion of the first link 651 and the first end portion of the second link 652 . The second link 652 is integrally connected with the handling member 125 .
The stabilizing mechanism 650 further includes a third link 653 having first and second end portions and substantially equal in length to the first link 651 . The second and third links 652 and 653 are pivotably connected with each other at the second end portion of the second link 652 and the first end portion of the third link 653 .
The stabilizing mechanism 650 further includes a fourth link 654 having first and second end portions and substantially equal in length to the second link 652 . The third and fourth links 653 and 654 are pivotably connected with each other at the second end portion of the third link 653 and the first end portion of the fourth link 654 . The fourth and first links 654 and 651 are pivotably connected with each other at the second end portion of the fourth link 654 and the first end portion of the first link 651 under the state that the first link 651 is in parallel relationship with the third link 653 and that the second link 652 is in parallel relationship with the fourth link 654 . The second end portion of the fourth link 654 integrally formed with the first long link 412 or the first short link 421 .
The robot arm 950 further comprises an additional stabilizing mechanism 660 . The additional stabilizing mechanism 660 is similar to the stabilizing mechanism 650 and includes a first link 661 having first and second end portions and substantially equal in length to the fourth arm link 954 . The first link 661 is integrally formed with and in coaxial relationship with the fourth arm link 954 under the state that the first end portion of the first link 661 is connected with the first end portion of the fourth arm link 954 .
The additional stabilizing mechanism 660 further includes a second link 662 having first and second end portions. The first and second links 661 and 662 are pivotably connected with each other at the second end portion of the first link 661 and the first end portion of the second link 662 . The second link 662 is integrally connected with the additional handling member 126 .
The additional stabilizing mechanism 660 further includes a third link 663 having first and second end portions and substantially equal in length to the first link 661 . The second and third links 662 and 663 are pivotably connected with each other at the second end portion of the second link 662 and the first end portion of the third link 663 .
The additional stabilizing mechanism 660 further includes a fourth link 664 having first and second end portions and substantially equal in length to the second link 662 . The third and fourth links 663 and 664 are pivotably connected with each other at the second end portion of the third link 663 and the first end portion of the fourth link 664 . The fourth and first links 664 and 661 are pivotably connected with each other at the second end portion of the fourth link 664 and the first end portion of the first link 661 under the state that the first link 661 is in parallel relationship with the third link 663 and that the second link 662 is in parallel relationship with the fourth link 664 . The second end portion of the fourth link 664 integrally formed with the first long link 462 or the first short link 471 .
The first driving shaft 121 is integrally connected with the second end portion of the sixth arm link 956 and rotating the sixth arm link 956 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the fifth arm link 955 and rotating the fifth arm link 955 around the rotation axis 123 .
According to the present invention, the fifth and sixth arm links 955 and 956 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the link retaining mechanism 400 retains the first and second arm links 951 and 952 under the state that the first and second arm links 951 and 952 are in symmetrical relationship with each other with respect to the center line 401 . The additional link retaining mechanism 450 retains the third and fourth arm links 953 and 954 under the state that the third and fourth arm links 953 and 954 are in symmetrical relationship with each other with respect to the center line 451 . By the reason that the first and third arm links 951 and 953 are respectively in symmetrical relationship with the second and fourth arm links 952 and 954 , the handling member 125 leaves from the rotation axis 123 when the additional handling member 126 approaches the rotation axis 123 . By the same reason, the additional handling member 126 leaves from the rotation axis 123 when the handling member 125 approaches the rotation axis 123 .
According to the present invention, the robot arm mechanism 115 can be rotated around the rotation axis 123 by the rotation of the fifth or sixth arm links 955 or 956 around the rotation axis 123 .
Referring to FIGS. 28 and 29 of the drawings, there is shown a sixteenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 116 is shown in FIGS. 28 and 29 as comprising a robot arm 960 .
The construction of the robot arm mechanism 116 in the present preferred embodiment is similar to the construction of the robot arm mechanism 115 in the fifteenth preferred embodiment except for the link retaining mechanism 500 and the additional link retaining mechanism 550 .
The robot arm 960 comprises first, second, third, and fourth arm links 961 , 962 , 963 , and 964 which are similar to first, second, third, and fourth arm links 951 , 952 , 953 , and 954 in the fifth preferred embodiment of the robot arm mechanism according to the present invention.
The first driving shaft 121 is integrally connected with the second end portion of the fifth arm link 965 and rotating the fifth arm link 965 around the rotation axis 123 . The second driving shaft 122 is integrally connected with the second end portion of the sixth arm link 966 and rotating the sixth arm link 966 around the rotation axis 123 .
According to the present invention, the fifth and sixth arm links 965 and 966 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 .
According to the present invention, the operation of the robot arm mechanism 116 in the sixteenth preferred embodiment is similar to the operation of the robot arm mechanism 115 in the fifth preferred embodiment.
Referring to FIGS. 30 to 32 of the drawings, there is shown a seventeenth preferred embodiment of the robot arm mechanism according to the present invention. The robot arm mechanism 117 is shown in FIGS. 30 to 32 as comprising a handling member 125 and a robot arm 970 .
The robot arm 970 comprises first and second arm links 971 and 972 .
The robot arm 970 further comprises a third arm link 973 having first and second end portions and substantially equal in length to the first arm link 971 . The second and third arm links 972 and 973 are pivotably connected with each other at the first end portion of the second arm link 972 and the first end portion of the third arm link 973 .
The robot arm 970 further comprises a fourth arm link 974 having first and second end portions and substantially equal in length to the second arm link 972 . The first and second arm links 971 and 972 are substantially equal in length to each other. The first and fourth arm links 971 and 974 are pivotably connected with each other at the first end portion of the first arm link 971 and the first end portion of the fourth arm link 974 .
The robot arm 970 further comprises a fifth arm link 975 having first and second end portions and substantially equal in length to the distance between the second end portion of the first long link 512 and the first end portion of the first short link 521 . The first and fifth arm links 971 and 975 are pivotably connected with each other at the second end portion of the first arm link 971 and the first end portion of the fifth arm link 975 . The third and fifth arm links 973 and 975 are pivotably connected with each other at the second end portion of the third arm link 973 and the second end portion of the fifth arm link 975 under the state that the first long link 512 and the fifth arm link 975 are in parallel relationship with each other and that the first arm link 971 and the third arm link 973 are in parallel relationship with each other.
The robot arm 970 further comprises a sixth arm link 976 having first and second end portions and substantially equal in length to the distance between the second end portion of the first long link 512 and the first end portion of the first short link 521 . The second and sixth arm links 972 and 976 are pivotably connected with each other at the second end portion of the second arm link 972 and the first end portion of the sixth arm link 976 . The fourth and sixth arm links 974 and 976 are pivotably connected with each other at the second end portion of the fourth arm link 974 and the second end portion of the sixth arm link 976 under the state that the first long link 512 and the sixth arm link 976 are in parallel relationship with each other and that the second arm link 972 and the fourth arm link 974 are in parallel relationship with each other, the handling member 125 and the sixth arm link 976 integrally formed with each other.
The arm driving mechanism 120 comprises a first driving shaft 121 rotatable around a rotation axis 123 , and a second driving shaft 122 in the form of a hollow shape to rotatably receive therein the first driving shaft 121 and rotatable around the rotation axis 123 . The rotation axis 123 is positioned on the line passing through the first and second end portions of the fifth arm link 975 . The robot arm 970 further comprises a driving assist parallelogram linkage 690 including a first link 691 having first and second end portions and substantially equal in length to the distance between the rotation axis 123 and the second end portion of the first arm link 971 . The first link 691 is integrally formed with and in coaxial relationship with the fifth arm link 975 under the state that the second end portion of the first link 691 is connected with the first end portion of the fifth arm link 975 .
The driving assist parallelogram linkage 690 further includes a second link 692 having first and second end portions. The first and second links 691 and 692 are pivotably connected with each other at the second end portion of the first link 691 and the first end portion of the second link 692 . The second link 692 is integrally formed with and in parallel relationship with the first arm link 971 under the state that the first end portion of the second link 692 is connected with the second end portion of the first arm link 971 .
The driving assist parallelogram linkage 690 further includes a third link 693 having first and second end portions and substantially equal in length to the first link 691 . The second and third links 692 and 693 are pivotably connected with each other at the second end portion of the second link 692 and the first end portion of the third link 693 .
The driving assist parallelogram linkage 690 further includes a fourth link 694 having first and second end portions and substantially equal in length to the second link 692 . The third and fourth links 693 and 694 are pivotably connected with each other at the second end portion of the third link 693 and the first end portion of the fourth link 694 . The fourth and first links 694 and 691 are pivotably connected with each other at the second end portion of the fourth link 694 and the first end portion of the first link 691 under the state that the first link 691 is in parallel relationship with the third link 693 and that the second link 692 is in parallel relationship with the fourth link 694 .
The arm driving mechanism 120 comprises a first driving shaft 121 rotatable around a rotation axis 123 , and a second driving shaft 122 in the form of a hollow shape to rotatably receive therein the first driving shaft 121 and rotatable around the rotation axis 123 .
The second driving shaft 122 is integrally connected with the fourth link 694 at the second end portion of the fourth link 694 and rotating the fourth link 694 around the rotation axis 123 . The first driving shaft 121 is integrally connected with the fifth arm link 975 and rotating the fifth arm link 975 around the rotation axis 123 .
According to the present invention, while the second driving shaft 122 rotates the first arm link 971 through the driving assist parallelogram linkage 690 , the second driving shaft 122 may be directly and integrally connected with the first or third arm links 971 or 973 at the second end portions of the first or third arm links 971 or 973 without the driving assist parallelogram linkage 690 .
According to the present invention, the link retaining mechanism 500 retains the first and second arm links 971 and 972 under the state that the first and second arm links 971 and 972 are in symmetrical relationship with each other with respect to the center line 501 . By the reason that the first arm link 971 is in symmetrical relationship with the second arm link 972 , the fifth and sixth arm links 975 and 976 are positioned on a common line. By the reason that the fifth and sixth arm links 975 and 976 are positioned on the common line, the handling member 125 approaches and leaves from the rotation axis 123 with keeping a direction with respect to the rotation axis 123 fixed.
According to the present invention, the robot arm mechanism 117 can be rotated around the rotation axis 123 by the rotation of the first and second driving shafts 121 and 122 around the rotation axis 123 .
According to the present invention, the fifth arm link 975 and the fourth link 694 may be replaced by each other about the connection with the first or second driving shafts 121 or 122 . | A robot arm mechanism includes a handling member for supporting and handling an object, a robot arm made up of at least four arm links, and a robot arm driving mechanism for driving the robot arm to assume its contracted and extended position. The robot arm comprises first and second arm links and a link retaining mechanism pivotably retaining the first and second arm links. The link retaining mechanism comprises first and second joint cross linkages similar in shape and each having two arms crossed to each other. The first joint cross linkage is integrally connected with one of the first and second arm links of the robot arm. The second joint cross linkage is integrally connected with the other one of the first and second arm links of the robot arm. This leads to the advantage of providing a robot arm mechanism exempt from driven gears, belts and pulleys forming part of a synchronous motion mechanism necessitated by conventional robot arm mechanisms to ensure that no dust is produced and fallen in a vacuum working chamber of highly pure air. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation of the pending patent application Ser. No. 573,958, filed June 11, 1986, now U.S. Patent No. 4,640,225, issued Feb. 3, 1987, which application is a continuation-in-part of application Ser. No. 315,307, filed 10/27/81, now U.S. Pat. No. 4,469,046, which is a continuation-in-part of application Ser. No. 909,256, filed May 24, 1978, now abandoned, the subject matter and description of which is incorporated herein by reference thereto, as though set forth herein in detail.
BACKGROUND OF THE INVENTION 1. Field of the Invention
This invention relates to improvements in a unique odor preventing, disposable, absorbent pad-liner for an animal litter unit, and more particularly to an improved combination of mesh screening and absorbent padding with plastic liner to be utilized in combination with the described custom box or independent holders. 2. Brief Description of the Prior Art
Many domestic animals frequently use litter boxes for the elimination of body wastes. The boxes are usually filled with various kinds of absorbent granular materials such as sand, cat litter and the like, and must be periodically emptied and cleaned, which are somewhat objectionable tasks, since the absorbent granular material must be replaced and the boxes cleaned each time.
Cats, being the most frequent users of litter boxes, present a further problem in that the urine of the feline contains the highest content of urea which, when allowed to stand for any length of time in any absorbent material, releases an ammonia odor. This odor is one of the more objectionable factors in the ownership of a cat.
In order to eliminate the odor caused by cat urine, the litter box must be changed frequently, this being an expensive, laborious and messy job.
Many patents have issued on devices for the indoor use by cats, such as U.S. Pat. No. 3,233,588. The invention disclosed in this patent employs the use of a screen which is placed on top of the cat litter. This patent does ease the problem of animal excrement, by merely lifting the screen and disposing of the feces lying on top, it does not however, contend with the problem of the odor created by the urine. The unit must be periodically emptied of its absorbent granules and thus only partly contents with the elimination of the mess and labor involved. U.S. Pat. No. 3,809,013 is similar, except that a stack of liners is placed under the litter. When the litter becomes soiled, the liner is lifted, the litter filters through screen covered holes in the center of the liner and the litter is reused with the next liner. Again, the excrement is disposed of neatly, however the odor problem remains.
U.S. Pat. No. 3,284,273 discloses an absorbent pad which can be used in combination with animals. Although this pad does contain absorbent capabilities, the odor from the urine of the animal is trapped, much as in the standard cat litter. The pad is not designed for repetitive, long term use in a cat box but rather to retain the urine in a disposable pad, by mopping up pools of urine left on floors or in cages, etc.
U.S. Pat. No. 3,476,083 discloses the use of deodorizing substances which are placed in the bottom of the receptacle. A screen is placed a short distance above, on which lies the standard kitty litter. The upper compartment receives the solid and liquid excreta, retains the solids and absorbs the bulk of the liquid allowing the excess liquids to drain through to the lower compartment. Although providing some neutralizing of the ammonia odor by deodorizing the urine which cannot be absorbed by the litter, it does not provide an effective means for deodorizing the bulk of the urine which has been trapped in the litter. The disposal of all the litter creates a substantial expense to the owner and the cleaning of the lower compartment would be unpleasantly laborious and rather messy. The spilling of the deodorizing substances (lime is suggested) would be objectionable as well as possibly harmful to the person handling the container if by chance some of the chemical substance was to come in contact with the skin.
While many additional patents could be cited regarding other variations of disposal systems, types of granular litter and containers none of these patents overcome both the problem of odor and easy, economical and convenient disposal and replacement.
SUMMARY OF THE INVENTION
In the instant invention the foregoing problems are overcome and an easy to use, odorless, disposable absorbent pad cntaining animal litter box is provided. The odorless animal litter box includes a box-like container capable of locking in place the absorbent pad structure. The absorbent pad structure includes a protective screening and a moisture impermeable liner. The protective screening is capable of withstanding the clawing action of an animal such as a cat, thus protecting the absorbent pad the moisture impermeable liner. The sheet layer of moisture impermeable material has length and width dimensions at least equal to that of the screen. The sorbent pad is positioned between the screen and the moisture impermeable material. The screen is sealed to moisture impermeable material along at least a substantial part of their peripheral edges. The screen is a flexible member formed of strands bonded at their interstices and is formed of a material which is substantially inert to urine. The strands have a tensile strength of at least 20 in lbs./sq.in. in both the warp and filling direction and a thread size in the range from 30 to 80 denier. The screen has mesh count, in number of squares per per square inch, in the range of between 850 and 175.
BRIEF DESCRIPTION OF THE DRAWINGS
The advantages and objects of the invention will become apparent and the invention will be more fully understood from the following specification, particularly when read in conjunction with the drawings, wherein:
FIG. 1 is a top perspective of the assembled unit in accordance with the present invention;
FIG. 2 is an exploded fragmentary view of the absorbent pad of the instant invention;
FIG. 3 is a perspective view of a locking handle for use with the embodiment of the invention shown in FIG. 7;
FIG. 4 is a perspective view of an assembled unit with the handle in the locked position;
FIG. 5 is a perspective view of an assembled unit with the handle in the initial position prior to being locked;
FIG. 6 is an enlarged fragmentary view of a screen for use with the instant invention; and
FIG. 7 is a fragmentary top perspective view of an embodiment of the instant invention which employs a locking mechanism.
DETAILED DESCRIPTION OF THE INVENTION
In order to provide a clear understanding of the instant invention, the various aspects of the invention are hereinafter described in detail.
GRANULAR MATERIAL 20
The granular material as employed in the instant invention is utilized to satisfy the digging instinct of the animal and therefore need not provide absorptive qualities. Consequently, inexpensive materials, such as clay, can be used in accordance with individual preferences. Unlike the commonly employed systems in which the granular material must be used in quantity to provide the required absorptive qualities and digging qualities, minimal quantities of the granular material can be used, as illustrated in the charts supra. The absorption quality of the layer 24 can provide the total or the predominant desiccation effect.
It is critical that the granular material be in contact with the underlying absorbent material so that the urine can be drawn into the absorptive layers. The particle size distribution of the granular material is such that it contains particles which are small enough to fit through the openings of the screen and provide direct moisture transfer from the granular particles to the lower absorptive layer.
The particle size distribution can range between 5.6 to 1 mm, corresponding to U.S. Series Standard Sieve opening #3 1/2 to #18. Smaller particles exist within the litter down to the size of dust, but do not adversely effect the primary function of the particles or adversely effect the absorptive material. Transport of the liquid across the screen can actually be enhanced by the presence of the small particles which are aesthetically undesirable but functionally acceptable.
ABSORBENT UNIT 12
The sorbtive-desiccant elements can be paper, tissue, pulp, starch, and related polymers, etc. Any material which can disperse the liquid quickly, thus providing a large surface area for evaporation of moisture can be used. It is necessary to evaporate from 5 to 20 ml. of liquid each time the litter is used by the cat.
Examples of materials which absorb liquid and cause a drying of the litter, (hence sorbtive-desiccant materials), are those manufactured by Dow Chemical and marketed under U.S. Pat. No. 4,117,184. The instant patent application incorporates by reference thereto, as though set forth in detail herein the description in U.S. Pat. No. 4,117,184 of a product commonly identified as a super absorbent and sold by Dow Chemical Company under the designation DWAL 35 R. The Dow Chemical product is available as a laminate which includes at least a tissue layer and a polymer film layer. The Dow Chemical laminate has an indicated minimum liquid absorbency capacity of 38 grams per gram of laminate.
Alternatively, the super absorbent can be a material such as the National Starch and Chemical Corporation product sold under the registered trademark PERMASORB. The National Starch product is a hydrophilic polymer which has the ability to absorb and hold urine. There is a significant reduction in urine odor and pH level in the presence of PERMASORB.
A ground paper pulp sorbtive-desiccant material has been found to provide a combination of high absorbency, high surface area and low cost. The large surface area provides for rapid urine evaporation.
Toxic chemicals are not only unnecessary but preferably are to be avoided.
Bacteria from the feces cannot grow in the sorbtive-desiccant layer because they are dried out and die or become dormant. It is bacteria which is capable of breaking down the urea into ammonia causing the strong volatile odor commonly associated with cat litter boxes.
As previously stated, the instant invention requires substantially less granular material for each use and requires fewer changes, saving further on granular use. In the prior art type of litter box, the litter consumption is greater than in accordance with the present invention. SCREEN MATERIALS 19
A flexible, screen like mesh or permeable or semi-permeable membrane is utilized to prevent the animal from clawing through to the absorbent layer. The screen material must, therefore, exhibit sufficient strength to with stand the clawing action of the animal. Some of the preferred materials of construction include nylon, polyester, polypropylene, vinyl coated fiberglas. The mesh-like screen or netting 19 can be formed by weaving, knitting, pressure adhesive, heat sealing or any process capable of providing the required claw rip resistance.
Even though the screen is disposable, it is critical that the screen be made of a material which is relatively inert to urine thereby preventing rapid corrosion of the screen material, resultant odors and chemical activity.
From the stand point of rip resistance, the required tensile strength in lbs./sq.in., must be at least 20 and can be as high as 150 or more in both the warp (length) and filling direction. From the stand point of the manufacture of the screen-absorptive layer combination, a minimum warp strength of 20 is also required. The preferred minimum strength is at least 50. The thread size preferably ranges from 30 to 80 denier.
The mesh count, in number of squares per square inch, can range between 850 and 175. At the upper limit, the hole size is so small as to interfere with liquid transfer. At the lower limit, the hole size is so large that the protective ability becomes inadequate. The lower plastic layer must be protected from the cats claws since even pin holes can cause urine to seep under the liner and causing a severe odor problem. Similarly the absorptive layer must be protected from the tearing action of the claws. For example, the screen of Vander Wall, U.S. Pat. No. 3,476,083, would be totally inoperative to prevent tearing of the absorptive layer or the plastic moisture barrier.
The use of a loose screen-like fabric is unacceptable because the mesh can be varied as a result of the force of the animal's claws. Accordingly, the reference to mesh size is intended to indicate the effective size under the acutal use conditions rather than a temporary size which can be readily altered by the animal.
Structural integrity of the screen can be achieved by any of the known means which yields bonding of the strands at their interstices, As for example, through fusion of strands at the cross-over points or through the weaving or knitting of the strands or any other means which precludes relative movement of the strands.
FIG. 1 illustrates, through a top perspective view, the assembled unit 10 of the instant invention. The outer shell unit 16 is slipped over the inner shell unit 44, shown in FIG. 4, locking the absorbent unit 12 in place. The granular material 20, which can be absorbent or non-absorbent, is placed on top of the absorbent unit 12 to provide the animal with the necessary scratching materials, if so required. The granular material would not be required if the unit was being used for a dog or other animal which did not have the scratching instinct.
In the modification of FIG. 1, the screen 19 is formed as an integral part of the outer shell unit 16. A large number of holes 14 are provided in order to permit the free passage of urine from the region above the screen to the sorbtive-desiccant layer below.
FIG. 2 shows, in exploded form, a cross-section of the layers which form the absorbent unit 12. The outer layer 22 which is a thin plastic sheet of a material such as polypropylene or polyethylene prevents waste from making contact with the box and doubles as a bag when disposing of the soiled litter. The sorbtive-desiccant layer 24 is formed from a super absorbent, rapidly evaporating material as previous stated herein.
The protective layer 26 is made from a durable, non-woven tissue substance. In addition to the protective layer 26, there can be an additional layer of either a hydrophobic or hydrophilic material. If a binder is used for either the fabric of the tissue layer or other layer, it must be of a non-water soluble material. The protective screen 28 is of a flexible, durable substance which prevents the animal from scratching through to the bottom layers. The protective layer 26 is described in greater detail in association with FIG. 6. The granular material 20 is placed on top of the absorbent unit as previously described herein.
FIG. 3 illustrates the locking handle 30, the contour of which should conform to that of the outer shell unit 42, as seen in FIG. 4. The outer shell unit 42 has been placed over the inner shell unit 44, locking the absorbent unit 12 in place. The locking handle 30 bottom edge 46 is inserted through the cut out section 54 and placed under the inner shell unit 44 lip 48. The top edge 50 of the locking handle 30 is then slipped over the outer surface 52 of the outer shell unit unit 42, as illustrated in FIG. 5. This action forces the inner shell unit 44 and the outer shell unit 42 to be locked together, preventing slippage of the absorbent unit 12 and providing convenient handles with which to transport the unit. The essential factor in the locking together of the two sections, is the compression of the sorbent unit 12 between the bottom surface 51 of the inner bottom region 55 of the outer shell 42 and the upper surface 53 of the base 57 of the inner shell unit 44. It should be evident that the top lip 48 of the inner shell 44 must be sufficiently spaced from the lower surface 59 of the upper section of the outer shell 42 so as to permit the locking handle 30 to exhibit its compressive force and lock the sorbent unit 12 in place before the top lip 48 can come into contact with the outer shell 42. Also seen in FIG. 5 is the importance of the matching contours of the locking handle 30 and the outer shell unit 42.
FIG. 6 is an enlarged view of the rip proof screen 60. The screen is formed of strands 63 and 64 which are at right angles to each other as well known in the art. The instinct of cats to scratch at fabrics puts a heavy stress on the screen. The clawing action can separate the strands to the point that the sorbtive-desiccant material 70 which underlies the screen can becomee exposed to the claws and torn apart. It is essential that the urine is free to pass through the screen and any intermediate layers, such as a hydrophobic membrane and one or more layers of tissue paper to the sorbtive-desiccant material. Therefore, neither the screen nor the intermediate layers can offer restriction to the urine flow except as well known for the hydrophobic membrane. For this reason, the screen must have sufficient porosity and or hydrophilicity such that beading of urine does not occur. The interstices of the cross strands are shown in FIG. 6, to be fused, as for example by means of heat. It has been found that this type of structure can withstand intense clawing without separation of strands. Thus the inner layers are protected from the claws of the cat. In this regard it is noted that the openings 14 of the screen 19 of FIG. 1, must represent a very high percent of the solid area 18 of the screen as compared to the area occupied by the solid area of the screen. The desired ratio has been found to be more reliably attainable with screens having strands fused at their interstices than by any other means. It must be understood that the opening cannot be so large that the cat can claw at the underlying layers. It is this later fact which results in the difficulty in attaining the required porosity. | The odorless animal litter box of the instant invention includes a box-like container capable of locking in place an absorbent pad structure, which includes a protective screening and a moisture impermeable liner. The protective screening is flexible and formed of strands bonded at their interstices, is substantially inert to urine and capable of withstanding the clawing action of an animal such as a cat. The sheet layer of moisture impermeable material has length and width dimensions at least equal to that of the screen. A sorbtive-desiccant pad is positioned between the screen and the moisture impermeable material and the screen is sealed to moisture impermeable material along at least a substantial portion of their peripheral edges. | 0 |
PRIORITY INFORMATION
[0001] This application is a divisional application claiming priority from U.S. patent application Ser. No. 12/261247 filed on Oct. 30, 2008.
FIELD OF THE INVENTION
[0002] The invention described herein is directed to a downhole fluid injection dispersion device. This invention may be employed to radially disperse fluid injected downhole in a well bore. This invention comprises a body comprising an inlet port and at least two radial outlet ports.
BACKGROUND OF THE INVENTION
[0003] In hydrocarbon production chemicals are introduced into a well through a capillary tube for mitigating problems, such as scaling, corrosion, or the deposition of organic products. Chemicals are also introduced in this manner to treat well fluids, reduce viscosity, and/or demulsify.
[0004] In prior art downhole chemical injection methods using a single capillary tube, the injected chemicals are not widely dispersed in the radial dimension, resulting in limited mixing of the chemicals and well fluids. This limited mixing can result in chemicals channeling on one side of an electrical submersible pump (“ESP”) located downhole. Such channeling leaves a side or portion of the ESP untreated. Additionally, capillary tubes used with prior art downhole chemical injection devices have been subject to plugging, resulting in a lack of chemical dispersion downhole to protect the ESP.
[0005] Another prior art chemical injection method involves injecting chemicals from the well surface into the well annulus. This method involves the chemicals flowing downward as a countercurrent to the gases that are liberated at the pump separator. In this method, the chemicals flow downhole to mix with production fluids and enter the intake or suction of the ESP. Once the mixture of production fluids and chemicals reach the ESP intake, they are discharged from the ESP, rather than flowing down past the ESP motor. Thus, components below the ESP intake, such as the motor, do not receive the intended treatment benefit of the injected chemicals. Downhole motors are especially susceptible to corrosion due to their high operating temperatures.
[0006] One or more embodiments of the invention described herein provide improved dispersion of fluids injected downhole and protection of the capillary tube against plugging, for various forms of oil production systems.
DESCRIPTION OF THE FIGURES
[0007] FIG. 1 is a cross sectional view of a third preferred embodiment of the invention.
[0008] FIG. 2 is a cross sectional view of a second preferred embodiment of the invention.
[0009] FIG. 3 is a cross sectional view of a first preferred embodiment of the invention.
[0010] FIG. 4 is a side view of a nozzle for use with various embodiments of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0011] A first preferred embodiment of the invention is shown in FIG. 3 . In a first preferred embodiment, the invention comprises a body 10 comprising a first body region 12 , a second body region 14 opposite the first body region, an outer longitudinal surface 16 positioned between the first and second body regions and comprising an indented surface region 20 between the first and second body regions, a first ledge 22 , and an inlet port 24 in the first ledge; and at least two radial outlet ports 26 mounted on opposite sides of the first body region
[0012] This first embodiment further comprises a first mechanical coupling 34 connected to the first body region, and a second mechanical coupling 36 connected to the second body region. In a preferred embodiment the second mechanical coupling comprises female pipe threads. In a preferred embodiment the first mechanical coupling comprises male pipe threads.
[0013] This first embodiment farther comprises an internal flow path 38 in fluid communication with the inlet port, said internal flow path comprising a first segment 40 extending longitudinally through the body, and at least two radial segments 42 , each of which is in fluid communication with one of the radial outlet ports. In a preferred embodiment radial segments extend in an orientation that is substantially perpendicular to the orientation of the first segment.
[0014] Another preferred embodiment comprises the limitations of the first embodiment plus a nozzle 27 connected to each radial outlet port.
[0015] Another preferred embodiment comprises the limitations of the first embodiment plus a check valve 46 installed in the inlet port and positioned to allow fluid flow into the inlet port and body, and to prevent fluid flow out of the inlet port and body.
[0016] A second preferred embodiment of the invention is shown in FIG. 2 . In a second preferred embodiment, the invention comprises a body 10 comprising a first outer surface 11 comprising an inlet port 24 , a second outer surface 13 opposite the first outer surface, an outer longitudinal surface 16 between the first outer surface and second outer surface, an inner longitudinal surface 18 between the first outer surface and second outer surface defining a central longitudinal channel, at least two radial outlet ports 26 mounted on opposite sides of the outer longitudinal surface, each of said outlet ports being in fluid communication with the inlet port.
[0017] This second embodiment further comprises a first tubing member 33 extending out of the central longitudinal channel in a first direction and a second tubing member 35 extending out of the central longitudinal channel in a second direction opposite to the first direction.
[0018] Another preferred embodiment comprises the limitations of the second embodiment plus a check valve 46 installed in the inlet port and positioned to allow fluid flow into the inlet port and body, and to prevent fluid flow out of the inlet port and body.
[0019] In another preferred embodiment, the body comprises at least four radial outlet ports 26 , each of which is mounted on a different quadrant of the inner longitudinal surface and is in fluid communication with the inlet port.
[0020] Another preferred embodiment comprises the limitations of the second embodiment plus a nozzle 27 connected to each radial outlet port.
[0021] A third preferred embodiment of the invention is shown in FIG. 1 . In a third preferred embodiment, the invention comprises a body 10 comprising a first outer surface 11 comprising an inlet port 24 , a second outer surface 13 opposite the first outer surface, an outer longitudinal surface 16 between the first outer surface and second outer surface; an inner longitudinal surface 18 between the first outer surface and second outer surface defining a central longitudinal channel, and at least two radial outlet ports 26 mounted on opposite sides of the inner longitudinal surface, each of said outlet ports being in fluid communication with the inlet port.
[0022] This third embodiment further comprises a first tubing member 33 extending out of the central longitudinal channel in a first direction and a second tubing member 35 extending out of the central longitudinal channel in a second direction opposite to the first direction.
[0023] Another preferred embodiment comprises the limitations of the third embodiment plus a check valve 46 installed in the inlet port and positioned to allow fluid flow into the inlet port and body, and to prevent fluid flow out of the inlet port and body.
[0024] In another preferred embodiment, the body comprises at least four radial outlet ports 26 , each of which is mounted on a different quadrant of the inner longitudinal surface and is in fluid communication with the inlet port.
[0025] Another preferred embodiment comprises the limitations of the third embodiment plus a nozzle 27 connected to each radial outlet port.
[0026] In a fourth preferred embodiment, the invention comprises a body 10 comprising a first outer surface 11 comprising an inlet port 24 , a second outer surface 13 opposite the first outer surface, a longitudinal surface 16 between the first outer surface and second outer surface,
[0027] The fourth preferred embodiment further comprises at least two radial outlet ports 26 mounted on opposite sides of the longitudinal surface, each of said outlet ports being in fluid communication with the inlet port
[0028] Another preferred embodiment comprises the limitations of the fourth embodiment plus a nozzle 27 connected to each radial outlet port.
[0029] The foregoing disclosure and description of the inventions are illustrative and explanatory. Various changes in the size, shape, and materials, as well as in the details of the illustrative construction may be made without departing from the spirit of the invention. | The invention described herein is directed to a downhole fluid injection dispersion device. This invention may be employed to radially disperse fluid injected downhole in a well bore. This invention comprises a body comprising an inlet port and at least two radial outlet ports. | 4 |
BACKGROUND AND OBJECTIVES
The invention relates to devices which use mechanical energy for cooling and heating purposes, and in particular to improvements in reciprocal bellows type evaporative cooling systems and heat pumps. An objective of the present invention is to provide a bellows type cooling and heating system which uses less force and energy than standard bellows temperature changing systems. Another objective of the present invention is to provide a cooling system which can use water instead of freon. Another objective is to provide cooling and heating systems which are adapted to operate under low refrigerant pressures, and low temperature differentials between the heat source and the heat sink. Another objective of the present invention is to provide an expander-compressor which is especially adapted to miniature cooling and heating devices, such as those which can be used in micro-climate cooling and heating systems. Another objective is to provide a force and energy sparing transmission of movement between an air evacuated enclosure and the atmosphere.
All compressor type evaporative temperature systems consist of 1. a low boiling point liquid used as a refrigerant and 2. the components involved in the generation and transmission of mechanical energy to compress and expand the vapors of the refrigerant. Most standard compressor type cooling systems use chlorinated hydrocarbons as low boiling point refrigerants (freons). The freons are hazardous because they damage the atmospheric ozone layer.
The boiling point of water can be lowered to freezing temperatures by an air vacuum. Under an air vacuum the water can, therefore, function as a low boiling point refrigerant. Water has several advantages over freon. It is non-toxic to the environment. it is cheaper than freon, and its latent heat of vaporization is higher than that of freon. In addition to the above, water operates at lower pressures and at lower pressure differentials (between the relatively cold and relatively hot portions of the compression types cooling and heating systems) than freons. They therefore require less force to operate than freon based systems. The main disadvantage of using water as a low boiling point refrigerant is the fact that the lowering of the boiling point of the water requires an air vacuum. This requires the housing of the water in a chamber from which the air has been evacuated. Mechanical force must then be transmitted to the water vapors through the walls of the chamber enclosing the air vacuum. Force transmitting means which pierce the surface of the air evacuated chamber increase the chances of leakage of air into the chamber and cancellation of the air vacuum. The most convenient force transmitting means which do not pierce the surface consist of bellows walls which increase and decrease the volume of the chamber. This requires a moving bellows wall surface which is exposed in its inner side to the vacuum and in its outer side to the atmosphere, This requires an investment of power to overcome atmospheric pressure upon the outside of the moving wall during the expansion phase of the reciprocal movements of the wall. The present invention provides means whereby atmospheric resistance to the movement of the wall is overcome without the investment of man made energy sources.
The invention is based upon the fact that force follows the path of least resistance. The direction of any force can, therefore, be controlled by the regulation of the resistance to the flow of the force. In the present invention an atmospheric force, or a vapor force, which provides a resistance to the movement of the movable wall of a bellows chamber, is balanced and neutralized by an atmospheric force, or a vapor force, which is made to flow in the opposite direction. Electric power is, therefore, not required to overcome the resistances. Since work is equal to force times displacement the present invention uses less electric energy to obtain a given displacement than conventional bellows compressor systems, when the temperatures and the refrigerants in the devices are identical.
In addition to the above, the fact that the position of the movable walls of the compressor expander can be changed by a tipping of a balance of opposing forces, causes the moving walls to be responsive to very small outside forces. The balanced bellows compressor-expander is, therefore, responsive to lower pressure ranges than single standard bellows compressors (see numerical example).
SUMMARY
Two bellows chambers which compress and expand in response to inside and outside pressure act as a compressor-expander. The chambers are positioned relative to each other in a way which causes the movable walls of the chambers to face each other, and to travel in opposite directions. The movable walls of the two chambers are attached to each other so that each movable wall transmits an opposing vector force to the other movable wall. The distance between the chambers is fixed to prevent the movements of the chambers towards and away from each other and to provide space for the movements of the flexible walls between the chambers. When the pressures in the chambers are below atmospheric pressure the movable walls of the chamber exert opposing pulling vector forces on each other. When the pressures in the chambers are above atmospheric pressures the movable walls of the chamber exert opposing pushing vector forces on each other. The walls settle in a position between the chambers which is the result of the balance of the opposing vector forces acting upon the walls. A reciprocal outside vector force upon the movable walls tips the balance between the movable walls and moves the walls in the directions of the applied force. This causes a reciprocal expansion and compression of each chamber. The bellows chambers contain a low pressure refrigerant such as water under a vacuum, or a high pressure refrigerant, such as freons or Forane which respond to the the expansion and compression of the chambers. During the expansion phase the low boiling point liquid evaporates in the evaporator chamber and absorbs heat from its surrounding. During the compression phase the condenser chamber delivers heat to its surroundings. The vapor re-condenses into a liquid in the condenser chamber and accumulates in the bottom of the condenser. When the liquid reaches a predetermined level it activates a float valve, and the water returns to the evaporator chamber by force of gravity to continue the heat exchange cycle. The cooling effects of the expansions of the bellows chambers are separated from the heating effects of the compressions of the bellows chamber by a system of tubes and one way valves.
FIG. 1 is a cross section of a preferred embodiment of the temperature changer.
DETAILED DESCRIPTION
As seen in FIG. 1 there is present a frame 5 with side walls 5a and 5b, top wall 5c, and bottom wall 5d. Extending from side wall 5b is a frame wall branch 7. Present on top of the left side of frame branch V is a bellows chamber 11a. The chamber contains a top wall 13a, a bottom wall 15a, and side walls 17a and 19a. Side wall 17a is immobile and is attached to wall branch 7 through frame wall extension 7a. Top and bottom walls 13a and 15a consist of bellows which allow side wall 19a to move to the left and to the right in a reciprocating manner. When wall 19a moves to the right bellows walls 13a and 15a change from a folded to and extended position, This increases the volume of chamber 11a. When wall 19a moves to the left bellows walls 13a and 15a change from an extended to a folded position. This decreases the volume of chamber 11a. The size and number of the folds in the bellows are such that the bellows allows a sufficient distance of travel of wall 19a. The natural bias of the bellows walls flexibility tends to keeps walls 13a and 15a in a folded position. The wails of chamber 11a are made of good insulating materials such as plastic to prevent an exchange of heat between bellows chamber 11a and the environment. Penetrating chamber 11a through the immovable wall 17a are an outlet tube 12a and an inlet tube 14a.
Present on top of the left side of frame wall 5d is a network of heat exchange tubes 20a. The network functions as an evaporator chamber, as will be explained. The net work consists of a top horizontal tube 21a, a bottom horizontal tube 23a, and vertical tubes 25a. Penetrating the top wall of cylinder 21a is inlet tube 22a. The arrangement is that all vertical tubes 25a communicate with both horizontal tubes 21a and 23a. Network 20a is fixed in a position by frame extensions 26a which extend from the top of wall 5d to the bottom of horizontal tube 23a. The tubes and coils of network 20a are made of good heat conducting materials, such as copper, to allow for a maximal transfer of heat from the walls of the tubes to the outside environment. Means such as surface extensions (not shown) to increase the area of the heat exchange surfaces may be used. Penetrating horizontal tube 21a is an outlet tube 24a. Communicating between inlet tube 14a of chamber 11a and outlet tube 24a of horizontal tube 21a is a tube 27a. A one way valve 29a in tube 14a allows the exit of vapor from tube 21a to chamber 11a, but blocks the entrance of vapor from chamber 11a to tube 21a.
Present on the inside left side of top frame wall 5c is a net work of heat-exchange tubes 31a. The network functions as a condenser chamber, as will be explained. The net work consists of a top horizontal tube 33a, a bottom horizontal tube 35a, and vertical tubes 37a. The arrangement is that all the vertical tubes 37a communicate with both horizontal tubes 33a and 35a. Network 31a is fixed in a position by frame extensions 36a of top frame wall 5c. The extensions 36a extend from the inside surface of wall 5c and are attached to the top surface of 33a. The tubes and coils of network 31a are made of good heat conducting materials, such as copper, to allow for a maximal transfer of heat from the walls of the tubes to the outside environment. Means such as surface extensions (not shown) to increase the area of the heat exchange surfaces may be used. Penetrating horizontal tube 33a is an inlet tube 50a. Communicating between inlet tube 50a of horizontal tube 33a and outlet tube 12a of chamber 11a is a tube 41a. A one way valve 43a in inlet tube 12a allows the entrance of vapor from chamber 11a to cylinder tube 33a, but blocks the entrance of vapor from tube network 31a to chamber 11a. Penetrating the bottom wall of horizontal cylinder 35a is outlet tube 34a.
Communicating between tubes 22a and tube 34a is a tube 51a. A floatation valve 53a, present in the tubes 34a, opens and closes tube 51a. Attached to valve 53a is a float 55a. The arrangement is that the float responds to a liquid level in vertical tubes 37a, so that when the liquid reaches a predetermined level in tubes 37a float 55a rises and opens valve 53a. This allows a transfer of liquid from network 31a to network 20a by force of gravity.
Present inside networks 20a and 31a is an air vacuum and low boiling point liquid, such as water 61a. The air vacuum lowers the boiling point of the water, and enhances the evaporation of the water, as will be described.
Present on top of the right side of wall branch 7 is a chamber 11b. Chamber 11b is a duplicate of chamber 11a and its components have been given similar numbers marked by the subscript b instead of a. As seen in FIG. 1 chamber 11b contains a top wall 13b, a bottom wall 15b, and side walls 17b and 19b. The duplicate chambers 11a and 11b are placed in positions, relative to each other, which cause the movable side walls 19a and 19b to face each other. Side wall 17b is immobile and is attached to branch 7 through frame wall extension 7b.
Top and bottom walls 13b and 15b consist of bellows which allow side wall 19b to move to the left and to the right in a reciprocating manner. When wall 19b moves to the left away from wall 17b, bellows walls 13b and 15b change from a folded to and extended position. This increases the volume of chamber 11b. When wall 19b moves to the right, towards wall 17b, bellows walls 13b and 15b change from an extended to a folded position. This decreases the volume of chamber 11b. The size and number of the folds in the bellows are such that the bellows allows a sufficient distance of travel of side wall 19b. The natural bias of the bellows walls tends to keep the bellows walls in a folded position. The walls of chamber 11b are made of good insulating materials such as plastic to prevent an exchange of heat between bellows chamber 11b and the environment. Penetrating chamber 11b through the immovable wall 19b are an outlet tube 12b and an inlet tube 14b.
Present on the right side of frame wall 5d is a network of heat exchange tubes 20b. The network functions as an evaporator chamber, as will be explained. Network 20b is a duplicate of network 20a and its components have been given similar numbers marked by the subscript b. The net work consists of a top horizontal tube 21b, a bottom horizontal tube 23b, and vertical tubes 25b. The arrangement is that all the vertical tubes 25b communicate with tubes 21b and 23b. Network 20a is fixed in a position by frame extensions 26b which extend from the top of wall 5d to the bottom of horizontal tube 23b. The tubes and coils of network 20b are made of good heat conducting materials, such as copper, to allow for a maximal transfer of heat from the walls of the tubes to the outside environment. Means such as surface extensions (not shown) to increase the area of the heat exchange surfaces may be used. Penetrating the side wall of cylinder 21b is an outlet tube 24b. Communicating between inlet tube 14b of chamber 11b and outlet tube 24b of horizontal tube 21b is a tube 27b. A one way valve 29b in tube 14 b allows the exit of vapor from tube 21b to chamber 11b but blocks the entrance of vapor from chamber 11b to tube 21b. Network 20b functions as an evaporator chamber, as will be described. Penetrating the top wall of horizontal cylinder 21b is inlet tube 22b.
Present on the inside right side of top frame wall 5c is a net work of heat-exchange tubes 31b. The network functions as a condenser chamber, as will be explained. Network 31b is a duplicate of network 31a and its components have been given similar numbers marked by the subscript b. Net work 31b consists of a top horizontal tube 33b, a bottom horizontal tube 35b, and vertical tubes 37b. The arrangement is that all the vertical tubes 37b communicate with both tubes 33b and 35b. Network 31b is fixed in a position by frame extensions 36b of top frame wall 5c. The tubes and coils of network 31b are made of good heat conducting materials, such as copper, to allow for a maximal transfer of heat from the walls of the tubes to the outside environment. Means such as surface extensions (not shown) to increase the area of the heat exchange surfaces may be used. Penetrating horizontal tube 33b is an inlet tube 50b. Communicating between inlet tube 50b of horizontal tube 33b and outlet tube 12b of chamber 11b is a tube 41b. A one way valve 43b in tube 12b allows the entrance of vapor from chamber 11b to tube 33b, but blocks the entrance of vapor from tube 33b to chamber 11b. Penetrating the bottom wall of horizontal cylinder 35b is outlet tube 34b.
Communicating between tubes 22b and tube 34b is a tube 51b. A floatation valve 53b, present in the tube 34b, opens and closes tube 34b. Attached to valve 53b is a float 55b. The arrangement is that the float responds to a liquid level in vertical tubes 37b, so that when the liquid reaches a predetermined level in tubes 37b float 55b rises and opens valve 53b. This allows a transfer of liquid from network 31b to network 20b by force of gravity.
Present inside networks 20b and 31b is an air vacuum and low boiling point liquid, such as water 61b. The air vacuum lowers the boiling point of the water, and enhances the evaporation of the water, as will be described.
Present between movable walls 19a and 19b, at a 90 degree angle to the walls, are horizontal rods 71. The rods are permanently attached to walls 19a and 19b and transmit a vector force from one wall to another, as will be explained. Chambers 11a and 11b are kept at a predetermined fixed distance from each other by the attachments of the bottoms of immovable side 17a and 17b to branch support 7, as previously described. In addition, the distance between chambers 11a and 11b is fixed by rods 54 which are attached to the tops of side walls 17a and 17b of the chambers. The distance between the chambers is such that each of bellows walls 13a, 13b, 15a, and 15b are pulled to about half of their expansion potential. This allows an equal left and right distance of travel by movable walls 19a and 19b between the chambers. The arrangement is such that, when the walls travel to the left and to the right, between chambers 11a and 11b, one bellows chamber expands while the other bellows chamber contracts. Attached to the outer surface of wall 19a is a rod 81. The rod is connected, by standard crank and shaft means 85, to a standard motor (not shown) to reciprocally move walls 19a and 19b to the left and to the right between chambers 11a and 11b, as will be described.
The operation of the engine when low boiling point liquid 61a and 61b consists of water is as follows. The Liquid evaporates in chambers 11a and 11b, and exerts a vapor pressure upon the inside walls of the chamber. Since force follows the path of least resistance the vapors exert a force that moves movable wall 19a to the right and movable wall 19b to the left. In contrast, the atmospheric pressure outside the chambers pushes wall 19a to the left, and wall 19b to the right. When refrigerant 61a consists of water the vapor pressure inside the chamber at ambient temperature is below atmospheric pressure. The net atmospheric force will, therefore, push wall 19a to the left and wall 19b to the right. Movable walls 19a and 19b will transmit these opposing vector forces to each other through rods 71. This will cause the movable walls to exert a pulling vector force upon each other. Thus, each wall will be subjected to a pushing vector force by the outside atmosphere, and a pulling vector force in the opposite direction by the movable wall of its adjacent container. When the temperatures in the chambers are equal to each other, the atmospheric push upon each wall is equal to the opposing pulling force by its adjacent wall. The opposing forces upon the walls will then cancel each other. The positions of walls 19a and 19b will then be determined primarily by the equal inherent flexibility of bellows 19 and 39. The inherent flexibility of the bellows will tend to keep the bellows in a folded position. This, however, is prevented by the fixed distance between the chambers which stretch the bellows to a half folded position. The walls will then rest in a position between the chambers determined by the the balance of the flexible forces upon the walls.
When crank and shaft 85 are activated by an electric motor the rotary force provided by the motor is translated to a reciprocal right and left pressure upon movable walls 19a and 19b. When this occurs the balance of forces upon the walls is tipped and the walls move in the direction of the applied force. For example, when rod 81 pushes walls 19a and 19b to the right the force which moves the walls to the right becomes larger than the force which moves the walls to the left. This will initiate a movement of the walls to the right. This enlarges chamber bellows 11a, and contracts chamber bellows 11b. This increases the volume of the vapor in container 11a and decreases the volume of the vapor in container 11b. The expansion of the vapor in container 11a results in a reduction of the vapor pressure in the container to below the vapor pressures in networks 20a and 31a. A portion of the vapor in network 20a will, therefore, leave network 20a through tube 27a and valve 29a to enter chamber 11a. In contrast to the vapors of network 20a, the vapors of network 31a are not effected when chamber 11a expands, because of one way valve 43a which prevents the exit of vapor from network 31a. The remaining vapor in network 20a then expands to fill the volume of the network. The expansion of the vapor induces a reduction in the temperature of the vapor and an additional evaporation of low boiling point liquid 61a in network 20a. The evaporation of the liquid causes the liquid to lose some of its heat content and to cool the coils of network 20a.
While the right movement of rod 81 increases the volume of chamber bellows 11a, it decreases the volume of chamber bellows 11b. This compresses the vapor in the chamber. The compression of the vapor in container 11b results in a increase of the vapor pressure in the container to above the vapor pressures in networks 20b and 31b. A portion of the vapor in chamber 11b will therefore enter condenser network 31b through tube 41b and valve 43b. In contrast to the vapors of the condenser chamber network 31b, the vapors of network 20b are not effected when chamber 11b contracts, because of one way valve 29b which prevents the entrance of vapor from 11b to network 20b. The entrance of additional vapor into network 31b will compress the vapor in network. This causes a temperature increase of the vapor to above ambient temperature. This causes the vapor to lose some of its heat content to the environment through the walls of the condenser chamber. Some of the vapor in 31b then re-condenses into a liquid. The re-condensed liquid accumulates in the lower portion of network 31b. As the level of the water rises in vertical tubes 25b the water lifts float 55b. When the float reaches a predetermined level it opens valve 53b. When this occurs the re-condensed liquid returns to network 20b through tube 51b by force of gravity.
When rod 81 moves to the left it moves walls 19a and 19b to the left. This enlarges chamber bellows 11b, and contracts chamber bellows 11a. This increases the volume of the vapor in container 11b and decreases the volume of the vapor in container 11a. The expansion of the vapor in container 11b results in a reduction of the vapor pressure in the container to below the vapor pressures in networks 20b and 31b. A portion of the vapor in network 20b will, therefore, leave network 20b through tube 27b and valve 29b to enter chamber 11b. The remaining vapor in network 20b then expands to fill the volume of the network. The expansion of the vapor induces a reduction in the temperature of the vapor and an additional evaporation of the low boiling point liquid in the network. The evaporation of the liquid causes the liquid to lose some of its heat content and to cool the coils of network 20b. In contrast to the vapors of network 20b, the vapors of network 31b are not effected when chamber 11b expands, because of one way valve 43b which prevents the exit of vapor from network 31b.
The decrease in the volume of chamber bellows 11a compresses the vapor in the chamber. The compression of the vapor in container 11a results in a increase of the vapor pressure in the container to above the vapor pressures in networks 20a and 31a. A portion of the vapor in chamber 11a will therefore enter condenser network 31a through tube 41a and valve 43a. The entrance of additional vapor into network 31a will compress the vapor in the network. This causes a temperature increase of the vapor to above ambient temperature. This causes the vapor to lose some of its heat content to the environment through the walls of the condenser chamber. Some of the vapor in 31a then re-condenses into a liquid. The re-condensed liquid accumulates in the lower portion of network 31a. As the water accumulates in vertical tubes 25a it lifts float 55a. When the float reaches a predetermined level it opens valve 53a. When this occurs the recondensed liquid returns to network 20a through tube 51a by force of gravity. In contrast to the vapors of the condenser chamber network 31a, the vapors of network 20a are not effected when chamber 11a contracts, because of one way valve 29a which prevents the entrance of vapor to network 20a.
While the present embodiment of the invention has utilized water under an air vacuum as the refrigerant, it is understood that a variety of other refrigerants such as Forane® 134A (tetrafluroethane) (F3CCH2F), an ozone sparring compound may be used without departing from the essence of the invention. When the vapor pressure of the refrigerant exceeds atmospheric pressure the movable walls of the bellows chambers will exert a pushing force upon each other instead of a pulling force. The balance of forces between the moving walls will result from opposing pushing actions by the movable walls instead of opposing pulling forces. The structures and operation of the invention will be exactly as described for FIG. 1. This may be useful in temperature changing systems which operate through a relatively low pressure differential between expansion and compression pressures, such as those which produce a relatively small change in ambient temperature (numerical example 2).
It is understood that, depending on where the evaporators 20a and 20b and the condensers 31a and 31b, are placed, the invention can be used as either a cooling device or a heating device. When the invention serves as a cooling device the evaporators are placed in an enclosure or area which is to be cooled, while the condensers are placed outside of the enclosure, where the heat of the condenser is dissipated as waste heat. In contrast, when the invention serves as a heating device the evaporators are placed in an enclosure or area which requires an increase in the temperature, while the evaporators are placed outside of the enclosure, where the cooling effects of the evaporators are dissipated. Alternatively, the evaporators may be placed in an enclosure which require a decrease in temperature, while the condensers may be placed in and enclosure which requires an increase in temperature and the invention can serve simultaneously as both a cooling and heating device. Proper heat distributing devices such as fans may be used.
NUMERICAL EXAMPLES
The minimum force required to move the movable walls of the balanced bellows expander-compressor is calculated according to formula (c-ev)×a, where c is equal to the vapor pressure of the condenser chamber, ev is equal to the vapor pressure in the evaporator chamber, and a is equal to the area of the movable wall.
The minimal force required to expand a conventional single air evacuated bellows chamber containing vapor pressures which are below atmospheric pressures is calculated according to the formula (at-ev)×a, where at is equal to atmospheric pressure, ev is equal to the vapor pressure in the evaporator chamber, and a is equal to the area of the movable wall.
The minimal force required to compress a conventional single air evacuated bellows chamber containing vapor pressures which are above atmospheric pressures is calculated according to the formula (c-at)×a, where c is equal to the vapor pressure in the condenser chamber, at is equal to atmospheric pressure, and a is equal to the area of the movable wall.
__________________________________________________________________________EXAMPLE 1FORCE REDUCTION BY BALANCED BELLOWSWITH WATER AS REFRIGERANT Force RequiredTemperature and Kg/10 cm Energy saved byWater Vapor Pressure Balanced Single Balancedin Evaporator in Condenser bellows bellows bellows__________________________________________________________________________A) 70 F., 0.026 Kg/cm 105 F., 0.078 Kg/cm 0.52 10.13 94.91% B) 50 F., 0.0125 Kg/cm 105 F., 0.078 Kg/cm 0.65 10.235 93.65% C) 50 F., 0.0125 Kg/cm 115 F., 0.098 Kg/cm 0.85 10.235 91.7%D) 32 F., 0.006 Kg/cm 105 F., 0.078 Kg/cm 0.72 10.30 93.0%E) 32 F., 0.006 Kg/cm 130 F., 0.078 Kg/cm 1.56 10.30 85.86%__________________________________________________________________________
__________________________________________________________________________EXAMPLE 2FORCE REDUCTION BY BALANCED BELLOWSWITH FORANE AS REFRIGERANT Force RequiredTemperature and Forane Kg/10 cm Energy saved byVapor Pressure Balanced Single Balancedin Evaporator in Condenser bellows bellows bellows__________________________________________________________________________a) 80 F., 7.14 Kg/cm 93 F., 8.81 Kg/cm 16.7 77.7 78.5%b) 70 F., 6.04 Kg/cm 105 F., 10.55 Kg/cm 45.1 95.1 52.6%c) 50 F., 5.64 Kg/cm 105 F., 10.55 Kg/cm 49.1 95.1 49.4%d) 32 F., 1.49 Kg/cm 105 F., 10.55 Kg/cm 90.6 95.1 4.7%e) 32 F., 1.49 Kg/cm 130 F., 15.06 Kg/cm 13.57 140 3.1%__________________________________________________________________________ | The force sparing temperature changer operates through at least two air evacuated bellows. The relative positions of the chambers are such that the moving walls of the chambers face each other and transmit opposing vector forces to each other. This causes the movable walls of the bellows to settle in positions which are the result of the balance of opposing forces upon the walls. An outside reciprocal vector force upon the movable walls tips the balance of the opposing forces upon the movable walls and causes a reciprocal expansion and compression of each chamber. The bellows chambers contain a low boiling point liquid, such as water under a vacuum, which responds to the the expansion and compression of the chambers. The cooling effects of the expansion of the chambers upon the low boiling point liquid are separated from the heating effects of the compression of the chambers, by separate tubings and one way valves. | 5 |
BACKGROUND OF THE INVENTION
This invention relates to a system for joining individual partitioning panels together, in situ, for example to form an office or other indoor partition.
In modern day office spaces and other work areas, it is common practice to divide the work area into separate work stations by means of in situ knockdown partitions, commonly made up of individual connectable free-standing or suitably supported panels and the like.
Among the requirements for partitions of the above kind are, inter alia, that the individual panels should be as simple as possible to connect together when erecting a partition and to disconnect when taking down the partition consistent with maintaining the structural integrity and strength of the partition. Also, for aesthetic reasons, it is preferable to be able to conceal any inter-panel connections in the completed partition and generally enhance its overall appearance. The present invention provides a partition joining system directed toward fulfilling these requirements.
SUMMARY OF THE INVENTION
The invention provides a system for releasably joining together individual partitioning panels, in situ, wherein the top corners of each panel are provided with respective attachment fittings for receiving respective ends of plate-like connector brackets used for joining adjacent panels together by attachment to the respective corner fittings of the adjacent panels. Further, the corner fittings at the top corners of the panels each have a snap-on cover, or cap which conceals the connector bracket when the panels are assembled and which at least visually forms a continuation of the panel edging. In the overall system, different connector brackets are provided for joining adjacent panels in line or at right-angles, in the latter case to form angle, T, or cruciform junctions. In each case, the snap-on covers conceal respective ends of the connector brackets, and for T or cruciform junctions, central portions of the connector brackets may have their own integrally formed covers or caps visually integrated with those on the panel corner fittings.
The corner fittings on each panel may include a stand-up threaded post over which an apertured end of a connector bracket is received and tightened down by a nut. The post may be located in a central slotted or recessed portion of the fitting on opposite sides of which are snap-in connector portions for receiving complimentary snap-in connector portions of the cover.
The bottom corners of each panel conveniently have connector fittings similar to those at the top of the panels for receiving similar, inter-panel, plate like connector brackets, but no covers are required.
A partition according to the invention is simple to erect and take down by use of simple wrench-like hand tools for tightening and loosening the nuts associated with each corner fitting and by snapping and unsnapping the respective covers as applicable.
In case of T-junction, right-angle and cruciform inter-panel connections, vertical beading or filler strips and the like may be provided to conceal the panel edges and enhance the appearance of the inter-panel junctions.
Additional features and advantages of the invention will become apparent from the ensuing description and claims read in conjunction with the attached drawings.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a perspective view of a pair of partitioning panels connected together in line by a joining system according to the invention,
FIG. 2 is an enlarged exploded view of a top corner fitting one of the panels,
FIG. 3 is a view similar to FIG. 2 showing adjacent corners of a pair of inter connected panels,
FIG. 4 is a perspective view, from below of a bottom corner of a panel,
FIG. 5 is a view similar to FIG. 4 showing the bottom corners of a pair of inter-connected panels,
FIG. 6 is a sectional elevational view of the top corner portion of a panel,
FIG. 7 is a sectional view on line 7--7 of FIG. 6,
FIG. 8 is a view similar to FIG. 6 of the bottom corner portion of the panel,
FIG. 9 is an exploded perspective view of a bottom corner fitting for the panel prior to assembly,
FIG. 10 is a front elevational view of a panel, part broken away,
FIG. 11 is an underneath perspective view of a cover for a top corner fitting of a panel,
FIG. 12 is an underneath perspective view of the top corner fitting,
FIG. 13 is a perspective view of a plate-like top connector bracket used for connecting adjacent panels together in line,
FIG. 14 is a view similar to FIG. 13 of a bottom connector bracket,
FIG. 15 is a plan view of a top connector bracket for connecting panels, shown in phantom at right angles,
FIG. 16 is a view similar to FIG. 15 of a top connector bracket for connecting three panels together at a T-junction,
FIG. 17 is a view similar to FIG. 16 of a top connector bracket for connecting four panels together at a
cruciform junction,
FIG. 18 is a perspective view of another connector bracket for connecting three panels together at a T-junction,
FIG. 19 is a perspective view of a top corner connection between three panels using a connector bracket as shown in FIG. 18,
FIG. 20 is a sectional view on line 20--20 of FIG. 19,
FIG. 21 is a perspective view of part of a beading strip used in the arrangement shown in FIGS. 19 and 20,
FIG. 22 is a perspective view of a pair of panels connected at a right angle and showing a beading channel and connector strip (exploded), and
FIG. 23 is a sectional plan view of the connection between panels as shown in FIG. 22.
DESCRIPTION OF PREFERRED EMBODIMENTS
A typical partitioning panel 10 to which the present invention is applicable, is shown, for example, in FIGS. 6-10. The panel comprises a rectangular wooden or chipboard frame 12 around which a metal frame 14 of rectangular section tubing lengths welded together is fastened by screws 16 extending through suitable apertures in the metal tubes. The side tubes 18 of the metal frame are open top and bottom. The panel is faced front and back by wooden or chipboard sheets 20 attached by pins 22 to frame 12, the sheets 20 having fabric coverings 24. The side edges of the panel are also provided with fabric covered chipboard or like sheets 26 pinned or otherwise secured between the outer edges of sheets 20. The top edge of the panel is provided with a plastic edging or beading strip 28 with depending legs 30 which snap fit onto the top metal tube of frame 14 (see FIG. 7). The strip 28 terminates at the inner edges of tubes 18.
Press-fitted into the open top of each tube 18 is a plastic attachment fitting 32, see particularly FIGS. 6 and 12. The fitting has a rectangular outer hub 34 dimensioned to press-fit tightly into tube 18, a hexagonal inner hub 36 and a top flange 38. A bolt 40 is mounted in the inner hub so as to project upwardly somewhat from flange 38, the bolt being secured in place by a lock washer 42. On its upper face, flange 38 is formed with opposed rectangular ribs 44 defining a shallow channel 46 (FIG. 2) therebetween for receiving a plate-like connector bracket 48 as will be described. Within the ribs are circular sockets 50 into which cruciform projections 52 of a plastic cover 54 can be releasably press-fitted. The cover is designed to match beading strip 28 and when fitted on flange 38 forms a visual extension of the beading strip. The cover has a peripheral step 56 at one end to define a slot 58 (FIG. 6) through which connector bracket 48 can extend. To secure the bracket in place, bolt 40 is provided with a nut 60. As shown in FIG. 13, bracket 48 has slots 62 at its opposite ends to fit over the respective bolts 40 at the top corners of two adjacent panels. The width of the bracket substantially conforms to the width of channel 46.
Press-fitted into the bottom of each tube 18 is a metal fitting 63 of known kind having, for example, a base portion 64 of zinc plate and a top 66 of spring steel with gripping projections 68. A levelling glide 70 threads into the fitting in known manner. The threaded stem 72 of the glide is provided with a nut and washer assembly for securing a bottom connector bracket 76 onto the adjacent stems 72 and tightening up the assemblies 74, again by means of a simple hand wrench. To disconnect the panels, this simple procedure is reversed.
FIGS. 15, 22 and 23 show an arrangement in which a pair of panels 10 as previously described are connected at a right angle rather than in line. As shown in FIG. 23, the panels are disposed corner edge to corner edge, and a hollow plastic filler strip 80, covered in fabric 82 to match that on the panels is used to fill the corner gap. To hold the filler strip in place, extruded plastic key strips 84 are inserted between the panels, the key strips having barbed ends 86, 88 which engage behind the panels, and behind the opposed lips 81 of the filler strip. In place of the connector brackets 48 used to connect the panels in line, in this case an angled connector bracket 100 (FIG. 15) is used to connect the top corners of the panels. Bracket 100 has apertures 102 in the respective limbs to engage bolts 40 of the respective panels in like manner to the apertures 62 in bracket 48 as previously described. In this case, the central portion of bracket 100 has an integrally attached plastic cover 104 to match visually with the covers 54 on the adjacent panels. Angled bottom brackets (not shown) are provided to replace the previously described brackets 76, and the panels are connected together and taken apart in like manner to the in-line panels previously described.
FIGS. 16 and 18-21 show an arrangement for connecting together three of the panels 10 at a T-junction. As seen in FIG. 20, the panels are located corner edge to corner edge, leaving a rectangular space 90 therebetween. A fabric covered extruded cover strip 92 is used to enclose the space 90, the strip having resilient end portions with ridges 94 that seat in small gaps defined between the sheets 20 and 26 of the respective panels 10. A T-shaped attachment bracket 96 with apertures 98 in its respective limbs and a central plastic cover 99 is used to attach the top corners of the respective panels in like manner to the brackets 48 and 100 previously described. A similarly shaped bracket (not shown) is used for connecting the bottom corners of the panels. A modified top bracket 96' with enclosed apertures 98' is shown in FIG. 18.
FIG. 17 shows an arrangement of four panels 10 interconnected in a cruciform formation using a top connector bracket 106 with four arms 108, apertures 110 and a central cover 112 which is used in the same way as those previously described in conjunction with a similarly shaped bottom connector bracket, not shown.
In each case, the invention provides an extremely simple to use, connection system for partitioning panels wherein the inter-panel connectors are effectively concealed and wherein the aesthetic appearance of the panels is maintained in the connected assembly.
While only preferred embodiments of the invention have been described in detail, the invention is not limited thereby and modifications can be made within the scope of the attached claims. | A system for joining partitioning panels is simple to assemble and take down while effectively concealing the inter-panel connections and maintaining visual continuity of the panels. Attachment fittings are provided at the top and bottom corners of each panel and plate-like connector brackets are used to connect the fittings and assemble the panels either in line or at an angle. Snap-on covers are provided for the top attachment fittings which conceal the connector brackets and form a visual continuation of finishing strips which extend along the top edges of the panels. | 4 |
TECHNICAL FIELD
This description relates to displaying cooking-related information.
BACKGROUND
Electric resistance or induction heating elements used on cooktops do not always provide visual sues to a user about how hot the elements, cookware, or food may be. On some cooktops, status information about cooking is provided implicitly by the controls used to regulate the heating elements or explicitly by displays related to the controls. United States patent application US0024/0238524A1 proposes to warn users when an element is hot using LEDs arranged under the cooktop.
SUMMARY
In general, in an aspect, light that carried information about cooking is directed in a first direction towards a redirection element, at the redirection element, light is redirected to be visible to a person cooking.
Implementations may include one or more of the following features. The information is represented by a color of the light, or by a pattern, an image, a character, or a symbol. The information is modulated by turning the light on and off, light color, and/or light intensity. The light is directed along the first direction through a material which transmits the entire or only a portion of the visible light spectrum. The redirection element comprises a light dispersing element. The light dispersing element comprises laser marked or grit blasted features. The first direction comprises a controlled incoming angle. The information comprises one or more of the following: an on-and-off status, temperature, a temperature distribution, a rate of temperature change, a rate of power change, a desired target temperature, a presence of food, the existence of an usage temperature. The light is delivered from a light emitting diode (LED) and/or a plasma lamp. The light is viewed as emitting from the vicinity of a heating element. The redirection element is in the vicinity of a heating element. The vicinity is directly over the heating element. The light is not located within a cooktop. The light is directed from openings of a light enclosure. The interior of the light enclosure is coated with a Lambertian light reflector. The cooktop surfaces may be coated with a Lambertian light reflector. The cooktop surfaces may be coated with an optically absorptive coating. The redirection element is located within and/or on the surface of a cooktop. The information is displayed by one or more internal redirection elements and/or one or more surface redirection elements. The heating element comprises an induction coil (or any other heating method).
In general, in an aspect, a cooktop comprises a material which transmits some portion or the entire visible light spectrum, and a light redirecting element in the material. The light redirecting element receives light from a light source located outside the cooktop.
Implementations may include one or more of the following. The light source introduces light into a light enclosure with openings; the light redirecting element receives light escaping from the openings. The interior of the light enclosure is coated with a Lambertian light reflector. The edges of the cooktop are coated with a Lambertian light reflector. The bottom surface of the cooktop is coated with an optically absorptive coating.
In general, in an aspect, an apparatus comprises a cooktop and a plasma lamp to provide light visible at an exposed surface to a person cooking.
Implementations may include one or more of the following. The apparatus further includes an induction heating element. The plasma lamp is over the induction heating element. The plasma lamp comprises a grounded electrode. The plasma lamp is illuminated depends on an induction heated cookware's size. The plasma lamp comprises a multiplicity of concentric annuli of light emitting zones. The light is modulated to display the information. The light modulation is a variation in color. The plasma lamp comprises a multiplicity of phosphor layers with different emitted colors.
In general, in an aspect, information is determined about a changing state of cooking begin done on a cooking surface, and light that has a characteristic that changes based on the changing state of cooking being done, is made visible to a user in the vicinity of the cooking surface.
These and other aspects and features and combinations of them may be expressed as methods, apparatus, systems, program products, in “means for” terminology, and in other ways.
Other advantages will be apparent from the description and from the claims.
DESCRIPTION
FIG. 1 is a top view of a cooktop.
FIGS. 2 , 5 , 6 , and 8 are schematic side views of cooktops.
FIG. 7 is a top view of a plasma display.
FIG. 3 is an example of a light enclosure
FIG. 4A is a plan view of cooktop with reflective coated sides
FIG. 4B is a cross section view of cooktop with reflective coated sides
Referring to FIG. 1 , in some examples, visual cues about cooking information related to use of a heating (induction heating, electric heating, or other heating methods) element 10 , 30 or 40 of a cooktop 12 (or other cooking appliance) can be displayed in a way that enables a user 16 to quickly, accurately, and intuitively understood the state of, for example, the heating element 10 , 30 or 40 , the cooktop 12 , a cooking utensil, or the food being cooked, and decide how to proceed, for example, by turning on a heating element 10 , 30 or 40 or keeping clear of a heating element 10 , 30 or 40 that is hot enough to burn.
One portion of the cooktop 12 , a control area 14 , conveys certain kinds of cooking related information to a user 16 . Located in the control area 14 , control knobs 18 , control panel displays 20 , and control buttons 22 display the status of the cooktop 12 . For example, when a heating element 10 , 30 or 40 of the cooktop 12 has been turned on by turning on a control knob 18 , the position of the control knob 18 indicates something about the cooktop's status.
In the example shown in FIG. 1 , another portion of the cooktop 12 , a cooktop heating area 24 , also conveys cooking-related information to the user 16 . Lighting elements 26 , which emit or redirect lights, located in the heating area 24 provide information that may be more easily and intuitively seen and understood than information provided in the control area 14 . Light emitted from or redirected by the lighting elements 26 is visible to a user 16 standing near the cooktop 12 . In some examples, the light may also be visible to users 16 standing in other locations farther away from the cooktop 12 . In some examples, the lighting elements 26 are illuminated by a light source indirectly from the side, above, or below the cooktop. In some examples, the lighting elements emit light from a light source such as a plasma lamp.
In some examples, multiple lighting elements 26 are arranged at and near each of the heating elements 10 , 30 or 40 to ensure at least a portion of the lighting elements 26 remain visible to the user 16 when a pot or other cookware (not shown) is placed on the heating element 10 , 30 or 40 , even though some of the lighting elements 26 may be blocked.
In some examples, lighting elements 26 are discrete elements, one or more or a pattern or group of the lighting elements 26 are associated with specific one or more of the heating elements 10 , 30 or 40 and convey cooking-related information for the associated heating element or elements 10 , 30 or 40 . Conversely, each of the heating elements 10 , 30 or 40 can be associated with one or more patterns or groups of the lighting elements 26 .
For example, in FIG. 1 , heating element 30 is associated with a group 32 of lighting elements 26 . Cooking-related information conveyed by the lighting elements of group 32 pertains (at least on some occasions) to heating element 30 . Heating element 40 is associated with a group 42 of lighting elements 26 . Some dual role lighting elements 44 can be associated with both heating element 30 and heating element 40 . For example, when the dual role lighting elements 44 are conveying cooking-related information associated with heating elements 30 by being lit in red to indicate that heating element 30 has been turned on, the lighting elements 44 will also be lit in red.
In the examples of FIG. 1 , the groups 32 of lighting elements 26 are in groups and patterns (in radial lines) around the associated heating element 30 . In some examples, the lighting elements 26 can be arranged in any other kind of pattern or group. The arrangements of the lighting elements 26 in groups and patterns may be designed to serve the purpose of conveying cooking-related information by, for example, placement intended to maximize visibility.
The lighting elements 26 can be arranged in a wide variety of shapes and configurations, for example, radially ( 32 ) as shown in FIG. 1 . The lighting elements 26 can be arranged around the heating element in patterns of varying densities (both densely and sparsely). The lighting elements 26 need not be circular. The lighting elements 26 are not limited to discrete geometrics such as 32 and 42 . The lighting elements 26 can be continuous geometrics. They can be square, triangular, or any standard or nonstandard shape including alphanumeric characters, icons, symbols, words and designs such as 26 - 1 to 26 - 5 in FIG. 1 . The lighting elements 26 may be arranged in an annular ring (or other shaped) area.
Arrangements may be chosen to serve aesthetic purposes. For example, in the patterns of lighting elements 26 in FIG. 1 , some lighting elements 26 will remain visible to the user 16 even when some of them are obstructed by pots of different diameters. The arrangement also serves an aesthetic purpose because some users 16 find radial arrangements of light attractive. Other patterns (discrete or continuous) that may be useful include arrays, cluster, lines, circles, other geometric groupings, and random groupings. In some arrangements, the lighting elements 26 need not be in the same location as the heating element with which they are associated.
A wide variety of properties of the light emitted from or redirected by the lighting elements 26 (in fact, any light property that is perceivable by a user) can be used to encode and convey cooking-related information. The light properties may include individual colors (e.g., wavelengths), sequences of or time changing patterns of colors, ranges or groups of colors, intensities, sequences of intensities, ranges or groups of intensities, and other modulations. The different light properties may be applied to all of the lighting elements of a group or pattern, or only to some of them, or only to one at a time.
For example, a bright light or a rapidly flashing light can signify a very hot heating element 10 , 30 or 40 or pot and a dim light or a non-flashing light can signify a cooler cooktop 12 . A green light can signify that the cooktop is set to a high power-level whereas a blue appearing light can signify low power level.
A wide variety of cooking-related information can be conveyed using the lighting elements 26 and groups and patterns of them. The cooking related information could include status information about elements of the cooktop 12 , including about the cooktop 12 as a whole, one or more of the heating elements, one or more pots or other items of cookware that are on one or more of the heating elements, the food that is being prepared in one or more of the items of cookware, and other information. Status information may include a power level of a heating element 10 , 30 or 40 , a temperature of a heating element 10 , 30 or 40 when the heating element gets hot, a desired or intended temperature of a heating element 10 , 30 or 40 , a temperature distribution of the heating element 10 , 30 or 40 , a rate of change of temperature of a heating element, a temperature of a pot or other cookware, a desired or intended temperature of a pot or other cookware, a rat of change of temperature of a pot or other cookware, an elapsed time (count-up timer), a remaining time (count-down timer), a presence of food in one or more pots or other cookware, and a current measurement of mass of food in one or more of the pots or other cookware. This cooking-related information can enhance the user's cooking experience and safety. For example, knowing the heating rat of the cookware can help a chef produce more appetizing food. Knowing the time elapsed (or time remaining) since the heating element 10 , 30 or 40 has been turned on or has reached a desired temperature can assist a busy cook by tracking the time remaining for a dish. Knowing the temperature of the pot can reduce the chance of the user 16 (or the food) being burned. When more than one item of food is being cooked on more than one heating element, the lighting elements 26 can be used to guide the user 16 with respect to the order in which different pots or cookware need attention. The cooking-related information could indicate the stage of cooking with respect to the steps of a recipe.
A wide variety of techniques and device can be used to provide the lighting elements 26 . In some examples, the lighting elements 26 are illuminated by a light source indirectly from the side, above, or below the cooktop. In some examples, the lighting elements 26 are one or more plasma lamps.
In some examples, as shown in FIG. 2 , the lighting elements 26 are light redirecting elements, which may be discrete or continuous, arranged to show certain features or patterns 50 within or on a surface (either the top 52 or bottom 53 surfaces) of a glass layer 54 that forms part of the cooktop. When the features 50 are within the glass 54 , they may be located at any distance from the top or bottom planes 56 , 58 of the glass layer, for example at approximately the midplane of the glass thickness. In the example of FIG. 2 , the light is delivered to the features 50 from a side 64 of the cooktop.
As mentioned earlier, the features 50 can be discrete or continuous and can take on any of a wide variety of forms and shapes, including spheres, teardrops, cubes or concentric rings, squares, radially configured circles or rectangles, or lines. The features 50 can be either directly under (for internal features), or on (for surface features) the surface of the cooktop, and be placed in close proximity to a heating element 10 , 30 or 40 so that the cooking-related information for the heating element 10 , 30 or 40 can be displayed.
The glass layer 54 can be made of glass ceramic material similar to that often used in cooktop 12 which has good resistance to high temperatures, thermal cycling and high fracture resistance. In general, as a glass, glass ceramics have composition Li 2 O—Al 2 O 3 —SiO 2 an other phases in very small percentage additions which are used as nucleating agents. Some examples of nucleating agents are TiO 2 , ZrO 2 and P 2 O 5 Nucleating agents enable the desirable properties of the glass ceramic to be achieved. Some trade names for glass ceramics which may be used for cooktop applications are EuroKera, Neoceram, Robax and Ceran.
The cooktop features can be achieved by laser marking, chemical etching, plasma etching, grit blasting, or in other ways. In addition, the glass 54 can be formed originally to have light dispersing features on its surfaces or internally.
When light from a light source 66 (for example, LEDs or conventional lamps) shines onto the internal or external features or other redirecting lighting elements, the redirecting lighting elements such as the internal features 50 or surfaces features 52 or 53 , redirect the light to give the appearance that the lighting elements 26 themselves are emitting light 63 . Visually attractive displays may be achieved by the arrangement of the redirecting lighting elements 26 . The redirecting lighting element 26 (the internal or surface features) can then be used to emit a light signal for conveying information about cooking. For example, referring again to FIG. 1 , when light is redirected by internal or surface features 26 - 5 to display the characters “ON”, the user 16 will read the work “ON” as it is being projected from the internal or surface features.
Referring again to FIG. 1 , in the case of induction heating element, for example, 30 , the lighting elements 26 can be arranged directly above an induction coil (heating element 30 ) between the induction coil 58 and the portion of the cooktop which bears the pot or cookware. An induction coil 68 uses induction heating to heat food. Typically, a ferromagnetic (or ferromagnetic-coated) pot is placed above the induction coil 68 . An induction current in the induction coil produces a rapidly oscillating magnetic field near the surface of the cooktop 12 . The oscillating magnetic field is converted into heat in the ferromagnetic pot. Magnetic hysteresis enhances the heating effect for ferromagnetic materials. The magnetic field also produced electrical eddy currents in the metal base of the pot to produce resistive heating.
In some examples, the LEDs as light source are placed to the side 64 away from the induction heating element 30 . This arrangement avoids potential damages from heat and the oscillating magnetic field which may affect the LED circuitry and causes LEDs to flicker. Furthermore, LEDs can be maintained and replaced more easily.
As shown in FIG. 2 , a control system for controlling the light 63 that is redirected by the lighting elements 26 accepts information regarding the user's actions from the user power controls 60 . Based on this and possibly other information (for example information about induction coil power, cooktop/pan/food temperature, intended recipes, maximum permissible cooking times, other foods being cooked on other elements), the control system coordinates the illumination of the lighting elements 26 (features 50 ) over time. Through the controlled illumination, information about cooking is conveyed to the user.
For example, to boil a pot of water on induction heating element 30 , the user turns on the heating element 30 using the user power controls 60 . The user's action is sent to an LED controller 76 and to an induction power supply 77 . The induction power supply 77 delivers a corresponding amount of power to the induction heating element 30 to heat the water in the cookware.
The induction power supply 77 also sends a signal to the LED controller 76 which incorporates this information in its control of the light source 66 . As the cookware is heated, the temperature of the cooktop is detected by one or more nearby temperature sensor 79 and the temperature of the pot is inferred from the temperature of the cooktop. The temperature may also be directly sensed within the cookware, or derived from the applied system load or other characteristic properties of the coil/target system. It should be noted that other sensors for providing other cooking information such as presence of food can also be used. The temperature sensor 79 sends a temperature signal to the LED controller 76 . The LED controller 76 , based on cooking information signals from the user power controls 60 , power supply information from the induction power supply 77 , and temperature information from the temperature sensor 79 , generates and sends LED control signals to the lighting source 66 . Light 62 from the light source 66 illuminates one or more lighting elements 26 based on the LED control signal. The lighting elements 26 redirect light 63 (such as through scattering) from the light source 66 and convey information to the user 16 . The light source 66 may be standalone LEDs or LED arrays 80 .
Although FIG. 2 shows the light 62 from the LEDs 80 projected from the side 64 of the cooktop, the light can also be projected from below or above the cooktop.
In some embodiments, the light 62 can be delivered to the cooktop through light pipes, fiber optic cables, mirrors, and other optical elements.
Light 62 from the light source 66 travels through the cooktop glass 54 to the lighting elements 26 by internal reflection 82 . To achieve this, the angle 83 of the light from the light source 66 entering the glass cooktop 54 from the side 64 is controlled. For internal features 50 , the incoming angle 83 of the light leads to total internal reflection (TIR) of the LED light 62 . For surface features 52 the incoming angle 83 of the light can be set to the critical angle relative to the top surface 56 of the glass cooktop 54 to lead to development of a cooktop surface light ray traveling on the top surface 56 of the cooktop. For surface features 53 the incoming angle 83 of the light can be set to the critical angle relative to the bottom surface 58 of the glass cooktop 54 to lead to development of a cooktop surface light ray traveling on the bottom surface 58 of the cooktop. Surface features 52 , 53 could also be illuminated from an indirect source located below the cooktop (see below for more details). In some examples, both internal features and surface features are employed for conveying cooking information. For example, internal features 50 can be used to indicate power on and variant power (by variable intensity), and surface features 52 and/or 53 can be used to indicate temperature variation. Internal features 50 and surface features 52 or 53 can be in different colors and/or patterns.
As in an optical fiber, a portion of the light 62 from the light source stays within the transmission medium (the cooktop glass 54 ). As measured between the light ray 62 and the perpendicular vector to the cooktop glass surface, if the angle of incidence 83 from the light source 66 is larger than the critical angle, the light 62 is internally reflected within the cooktop glass 65 . Achieving an incident angle greater than the critical angle insures that the maximum amount of light is imparted to the glass, thus allowing the maximum amount of light to be available for redirection by the lighting elements. Light 62 traveling within the glass 54 , is largely inconspicuous to the user until it encounters the lighting elements 26 , which redirect the light 62 . In this case, the features 50 effectively scatter the light in a conspicuous manner. Because light traveling within the glass is only evident at the features 50 , the light 63 appears to the user 16 to origins from these features 50 .
The critical angle is based on the index of refraction of the glass and of the air using Snell's Law. Any material that is optically transmissive and can withstand the cooking environment is a suitable candidate as a cooktop substrate. When the light travels in a glass ceramic cooktop 54 , as the glass ceramic material has a general transmission of 90% in the visible spectrum, the light travels mostly unimpaired through the cooktop 54 until it hits the features 50 .
A wide variety of light characteristics can be varied to convey a variety of information can be conveyed to the user. In some examples, the light source 66 can emit light 62 in selected wavelengths and polarities. The light source 66 may be different colored LEDs angled at different directions. The features 50 may be designed to act differently with respect to different polarization states of light, and thus light elements of different polarization states can occupy the same position on the cooktop surface.
The features 50 can be designed to redirect the light 62 from the light source 66 in a variety of different ways. For example, the light 62 can be redirected in a specific number of specific directions or it can be scattered and diffused indiscriminately. The light 62 can be redirected by features within the glass 54 (Or on the glass) that are arranged in places 65 a , 65 b as the light reflects from the different planes 65 a , and 65 b . These planes can be arranged to impart aesthetic or informational features to the redirected light. In the case in which the light 62 is redirected by indiscriminating scattering, the features are not arranged in any specific plane 65 a or 65 b . Rather, the features scatter light to create a fuzzy-looking glow.
An advantage of using features 50 within or on the glass is that the features 50 can be placed near areas of intense heat without fear of damage as they are an integral constituent of the glass itself. This permits placement of the lighting elements in places that would not be suitable for light sources 66 . For example, LEDs do not have the thermal stability to be placed near open gas flames or electric heating coils
The redirecting light elements 26 also permit easy replacing or switching of the light sources 66 that serve them. Among other things, the light sources 65 can be placed in an easily accessible area to enable the user 16 to change the light sources 66 (e.g., to replace a burnt-out light source, change the color, or upgrade to a more energy efficient source). In addition, if the supporting cooktop 54 is damaged, the supporting cooktop 54 can be replaced independently of the light source 66 . The user may change the supporting cooktop 54 for other reasons, for example, to change the features 50 for aesthetic purposes. Because the lighting elements 26 are separate from the light sources 66 , manufacturers can produce different models of cooktops that use a common set of lighting sources while changing the features from model to model to serve a variety of different purposes.
In some examples as shown in FIG. 3 , light is captured within a geometric form light enclosure 46 which is designed for having total internally reflected light. The light will be let out only at openings 48 which have been designed to achieve maximum lighting elements (e.g., features 50 , 52 or 53 of FIG. 2 ) illumination. In some examples, the light enclosure 46 can be placed between a heating element, such as an induction heating element 30 , and cooktop glass. The interior surfaces of the light enclosure 46 can be coated with a material to produce a Lambertian light reflection to ensure that light only escapes at the desired location and with maximum intensity. The openings may be in the form of slits, slots, circles, triangle, wedges, squares, or any other geometry. Light from light source such as LEDs, fiber optic bundles, or conventional light sources can be introduced into the geometric form light enclosure 46 along its outer circumferential wall through openings 47 . These light sources can be arranged at an angle to achieve maximum light intensity at the exit ports. Further, multiple light colors can be contained and redirected toward features ( 50 , 52 or 53 of FIG. 2 ) by using internal dividers 49 within the closed light enclosure 46 . This allows a distinct colors to be independently displayed on the cooktop surface simultaneously.
In some examples as shown in FIGS. 4A and 4B , the top view and cross section view of the sides of the cooktop glass 54 which is coated with a Lambertian light reflector 59 to prevent light from escaping at the edges, and to provide a more uniform and more intense illumination of the features 50 . The edge where the light is initially imparted to the cooktop glass can also be coated with the reflective coating to leave only the areas where light enters the glass uncoated. This will assure that the great majority of the light is trapped within the cooktop glass and is available for features 50 maximum illumination.
In some examples, as shown in FIGS. 4A and 4B , the bottom surface 58 of the cooktop glass 54 is coated with an optically absorptive coating 61 such as a black paint. This assures that any light which is refracted out of the glass ceramic at its bottom surface will be absorbed and thus not produce a diffuse reflection. As needed, areas of the bottom of the glass ceramic cooktop can be masked so as to allow light to escape from the light volume.
In some implementations, the light source 66 may be one or more plasma lamps 90 a , 90 b (collectively 90 ). Referring to FIG. 5 , a plasma lamp (PL) controller 92 accepts information from the user power control 60 , the induction power supply 77 , and temperature sensor 79 . Based on this and possibly other information, the controller 92 coordinates how and when a plasma lamp 90 is illuminated. The controlled illumination conveys information about cooking to the user 16 .
The plasma lamp 90 can be built into a cooktop 54 , (e.g., an induction cooktop) so that a flickering or moving glow appears under or in the vicinity of the pot or other cookware being heated. Although induction heating is invisible the plasma glow from the lamp 90 located under the pot can be used to simulate heating by another type of heat, for example, a gas flame. One type of plasma lamp that can be used is described in U.S. Pat. No. 5,383,295.
The cooing-related information provided to a user 16 of the cooktop using the plasma light 90 could include the amount of heating power applied by the induction power supply based on a color and/or intensity of the plasma light 90 . A change in the amount of power being supplied could be indicated by a change in the color or intensity of the plasma light 90 . In some embodiments, the relationship between the colors and power levels can follow a blackbody curve (red=low, yellow=medium, white=medium high, and blue=high). Other color-to-power level relationships may be selected based on psychological associations of various colors with information, for example blue=low and orange or red=high.
By adjusting the parameters of the plasma discharge or using diffusers, the plasma can appear warm and fuzzy rather than as a dangerous-looking lightning or sparing effect. The plasma lamp 90 contains gases and phosphors in the plasma discharge region. The colors can be produced by changing these gases and/or phosphors. The position of the plasma generation can also be controlled through modifying electrode geometrics.
Power for the plasma stimulation can be from a separate power supply or from an existing power supply. If a separate power supply is used, a conventional high-voltage, high frequency power supply may power the plasma lamp. If an existing power supply used, the existing induction power supply 77 can be modified to produce high frequency components so that an additional power supply is not necessary.
Referring to FIG. 6 , in some embodiments, a plasma lighting system 100 can be designed to use two phosphors by applying each phosphor to opposite sides 102 b , 104 a of a glass plate 103 . Plasma lamp is a sandwiching of five glasses: a top glass 101 , a top spacer glass 102 , a middle glass 103 , a bottom space glass 104 , and a bottom glass 105 . A cavity 106 is formed by the middle glass 103 , a spacer glass 102 , 104 , and either the top 101 or bottom 105 glasses. Xenon gas fills the cavity 106 and various combinations of phosphor line a portion of the cavity's walls.
In some examples, orange phosphor lines a portion 108 of the cavity 106 formed by the top side of the middle glass 102 b and blue phosphor lines a portion 110 of the cavity 106 formed by the bottom side of the middle glass 104 a . Each side is energized separately by a low frequency power supply (typically 60 Hz) 112 , 114 . The low frequency prevents the electricity from energizing the opposite side. By continuously varying the electrical stimulation of each side, a full range of colors is produced that varies from blue to orange. The intermediate colors include shade of magenta. The intensity of the light (brightness) can also vary at the same time the color goes from blue to orange. For example, the intensity may gradually increase during the blue to orange transition. In come embodiments, the blue phosphor is placed on the side opposite the view, the bottom side of the middle glass 104 a , because the blue is brighter than the orange.
To avoid electrically charging the cookware and giving the user a shock or tingling sensation when the user that touches the pot, the plasma could be adequately grounded to remove the electrical charge. Referring to FIG. 6 , in some embodiments, electrodes 116 , 118 , 120 , 122 are included in plasma light were electrodes 118 , 122 are grounded. This effectively prevents electrical charges from being induced in the pot.
Referring to FIG. 7 , various plasma geometries can be used. One example uses concentric circles 124 . The plasma is trapped within a circular annulus that is approximately ¼ side. This arrangement makes the flickering plasma light appear alive. The width of the circular annulus may be sized to the user's desires. The circular annulus does not extend completely around the circle. This forces the low frequency current to travel uniformly from one electrode to the other.
Referring to FIG. 8 , the plasma lighting 90 a , 90 b an be combined with LEDs 80 to produce a variety of effects such as the ability to independently signal when the cooktop 54 is hot (temperature) and when the induction coil 68 is energized (power). For example, red LED's can signal hot cooktop 54 and blue plasma can signal energized induction coil 68 . Electrodes or coil pickups can be used to couple the LED with the plasma.
Other embodiments are within the scope of the following claims. | Among other things, light that carries information about cooking is directed in a first direction towards a redirection element and, at the redirection element, the light is redirected to be visible to a person cooking. | 5 |
[0001] This application claims the benefit of the Korean Application No. P2004-26914 filed on Apr. 20, 2004, which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a combined drying and washing machine, and more particularly, to a radiation structure of a washing machine.
[0004] 2. Discussion of the Related Art
[0005] Generally, a washing machine is an apparatus to get laundry such as clothes clean by rotating a drum receiving therein detergent, washing water and laundry using a driving force of a motor. In such a washing machine, laundry is less worn and tangle-free. In recent years, a washing machine having drying function has been developed.
[0006] The washing machine includes a tub installed inside a housing, and a drum installed rotatably inside the tub. To dry laundry, the washing machine further includes a drying duct and a condensation duct. The drying duct is connected to the tub and receives therein a heater and a blower fan. Also, the condensation duct feeds hot air to the drum disposed inside the tub via the tub. The fed hot air dries the laundry and is exhausted to the condensation duct via the drum and the tub. The condensation duct removes moisture from the exhausted air and returns the moisture-removed air to the drying duct such that the moisture-removed air is again heated. The air inside the washing machine dries the laundry while it circulates via the tub, the drum, the condensation duct and the drying duct.
[0007] However, in the related art washing machine, the drying duct is connected to a gasket provided at the tub and an entrance of the housing and hot air fed through such a contact portion is discharged through a side portion of the tub. To this end, the related art washing machine having a typical drying function has the following drawbacks.
[0008] First, hot air is discharged from the drum through a side portion of the tub without deeply permeating an inside of the drum. To this end, the laundry received in a deep inside of the drum is not properly dried.
[0009] Secondly, the drying duct is stationary but the gasket is shaken together with the tub. To this end, the gasket may be worn or torn.
[0010] Thirdly, the hot air discharged from the drying duct collides with a door around the gasket to cause a serious flow resistance of air, which is one of reasons that the hot air does not reach the deep inside of the drum.
[0011] Fourthly, the drying duct may be overheated or deformed due to hot air flowing therethrough. Also, an adjacent part, in particular, the tub may be deformed due to the heated drying duct.
SUMMARY OF THE INVENTION
[0012] 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.
[0013] An object of the present invention is to provide a washing machine having an enhanced drying efficiency and performance.
[0014] 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.
[0015] To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a washing machine including: a housing; a tub installed inside the housing, for storing washing water; a drum rotatably installed inside the tub and configured to wash laundry; a drying duct connected to the tub, for generating hot air and feeding the generated hot air to an inside of the drum; a condensation duct connected to the tub and the drying duct, for removing moisture from an air discharged from the tub to guide the moisture-removed air to the drying duct and allowing the hot air to cross the inside of the drum together with the drying duct; and a radiation mechanism disposed at the drying duct, for radiating heat of the drying duct.
[0016] The drying duct and the condensation duct are configured to allow the hot air to fully and completely cross the inside of the drum in an axial direction thereof and are accurately configured to flow the hot air from a front side of the drum to a rear side of the drum.
[0017] The drying duct and the condensation duct are configured to flow the hot air in a diagonal direction inside the drum. Substantially, the drying duct and the condensation duct are configured to flow the hot air from a front upper side of the drum to a rear lower side of the drum.
[0018] The drying duct is preferably connected to a front upper portion of the tub. Also, the tub comprises an inlet formed at a front upper portion thereof and communicating with the drying duct, and the drum comprises an inlet formed at a front upper portion thereof and communicating with the drying duct.
[0019] The drying duct closely contacts an outer circumference of the tub and comprises an upper cover and a lower cover coupled to each other. The upper cover of the drying duct is made of steel and the lower cover of the drying duct is made of aluminum alloy.
[0020] The condensation duct is connected to a rear portion of the tub and is accurately connected to a rear lower portion of the tub.
[0021] The radiation mechanism is provided at an upper portion of the drying duct. The radiation mechanism comprises at least one radiation fin provided in the drying duct or at least one radiation groove formed at the drying duct. Also, the radiation mechanism comprises at least one radiation fin and at least one radiation groove provided in the drying duct. In this case, the radiation mechanism comprises a plurality of radiation fins and a plurality of radiation grooves, and the radiation fins and the radiation grooves are alternatively arranged.
[0022] According to the present invention, the drying performance and efficiency are greatly enhanced.
[0023] 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
[0024] 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:
[0025] FIG. 1 is a side sectional view of a washing machine according to the present invention;
[0026] FIG. 2 is a perspective view of an upper cover having a radiation mechanism according to the present invention;
[0027] FIG. 3 is a perspective view of an upper cover having a modified radiation mechanism according to the present invention; and
[0028] FIG. 4 is a perspective of an upper cover having another modified radiation mechanism according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0029] Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings.
[0030] FIG. 1 is a side sectional view of a washing machine according to the present invention.
[0031] Referring to FIG. 1 , the washing machine macroscopically includes a housing 10 , a tub 30 , a drum 40 , a drying duct 100 , a radiation mechanism 200 , and a condensation duct 300 .
[0032] The housing 10 has a laundry inlet formed at a front portion thereof. A door 20 is openably and closably installed at the laundry inlet of the housing 10 . The door 20 is provided with a door glass 21 protruded toward an opening of the tub 30 . A gasket 80 is disposed between the laundry inlet and the opening of the tub 30 . The tub 30 is installed to store washing water inside the housing 10 , and the drum 40 is rotatably installed inside the tub 30 . To save the material cost and reduce the weight, the tub 30 may be formed of plastic material. The drum 40 has a plurality of holes 40 a through which washing water received in the tub 30 is introduced. Also, a power unit connected with the drum 40 is disposed around the tub 30 , and the drum 40 is driven by the power unit.
[0033] Meanwhile, a drying duct 100 is installed inside the housing 10 and is connected with the tub 30 . The drying duct 100 is provided therein with a blower fan 62 and a heater 61 to thereby feed hot air to the drum 40 through the tub 30 . The condensation duct 300 is connected with the drying duct 100 and the tub 30 , respectively. The condensation duct 300 is provided with a water feeder 310 for feeding cooling water so as to condense moisture contained in the air and remove the moisture. Accordingly, the hot air is discharged to the condensation duct 300 from the drum 40 through the tub 30 , is converted into dry air, and is then guided to the drying duct 100 for reheating.
[0034] In more detail, the drying duct 100 is connected to a front upper portion of the tub 30 . The tub 30 has an inlet 31 communicating with the drying duct 100 and the drum 40 has an inlet 41 communicating with the drying duct 100 through the inlet 31 of the tub 30 . Also, the condensation duct 300 is connected to a rear lower portion of the tub 30 , and a discharge hole 32 is also formed at a rear lower portion of the tub 30 so as to communicate with the condensation duct 300 . Due to the positions of the connection portions between the drying duct 100 and the tub 30 and between the condensation duct 300 and the tub 30 , the hot air flows from the inside of the drum 40 to the front of the drum 40 and the back of the drum 40 as indicated by arrow. In accuracy, the hot air flows from the front upper portion of the drum 40 to the rear lower portion of the drum 40 . In other words, the hot air flows in a diagonal direction of an inside of the drum 40 . Resultantly, the drying duct 100 and the condensation duct 300 are configured to allow the hot air to fully and completely cross the inner space of the drum 40 in the axial direction of the drum 40 due to their proper installation positions. Accordingly, the hot air is uniformly distributed into the whole inner space of the drum 40 , so that drying efficiency and performance are greatly enhanced.
[0035] Also, the drying duct 100 includes an upper cover 110 and a lower cover coupled with each other. In addition, the drying duct 100 closely contacts the outer circumferential surface of the tub 30 so as to reduce an overall height of the washing machine. In accuracy, the lower cover 120 of the drying duct 100 closely contacts the upper outer circumferential surface of the tub 30 as shown in FIG. 1 . The upper cover 110 of the drying duct 100 is made of steel. Meanwhile, in order to prevent the tub 30 made of plastic material from being deformed due to the heat transferred from the lower cover 120 , the lower cover 120 is preferably made of aluminum alloy having better heat conductivity, corrosion-resistant property and heat-resistant property. Thus, the lower cover 120 is manufactured by a die-casting. Accordingly, by manufacturing only the lower cover 120 of aluminum alloy, the tub 30 can be prevented from being deformed and at the same time the manufacturing costs of the drying duct 100 can be saved.
[0036] The radiation mechanism 200 is disposed at the upper side of the drying duct 100 to radiate the heat of the drying duct 100 .
[0037] As shown in FIG. 2 , the radiation mechanism 200 includes at least one radiation fin, preferably, a plurality of radiation fins 210 . The radiation fins 210 are arranged at a predetermined interval to be normal to a length direction of the drying duct 100 . Of course, the radiation fins 210 may be arranged in the length direction of the drying duct 100 . These fins 210 as applied in a combined drum type drying and washing machine increases a radiation area for radiating heat of the drying duct 100 in the course of drying cycle. In more detail, when the drying duct 100 is heated by a drying operation, some of heat is transferred to the lower cover 120 and is radiated and the others of the heat are transferred to the upper cover 110 and are radiated from the upper cover 110 . At this time, the upper cover 110 having the increased radiation area due to the radiation fins 210 can radiate a large amount of heat. As a consequence, a very small amount of heat is transferred to the lower cover 120 and the tub, thereby preventing the tub 30 from being deformed. Alternatively, the radiation fin 210 may be attached on the upper cover 110 as an independent member or be formed integrally with the upper cover 110 .
[0038] Referring to FIG. 3 , the radiation mechanism 200 includes at least one, preferably, a plurality of radiation grooves 220 formed at the upper cover 110 . The radiation grooves 220 increase the radiation area of the upper cover 110 like the radiation fins 210 . Due to the increase of the radiation area, the radiation efficiency in the drying cycle of the combined drum type drying and washing machine is enhanced. Accordingly, a very small amount of heat is transferred to the tub 30 , thereby preventing the tub 30 from being deformed.
[0039] In addition, as shown in FIG. 4 , the radiation mechanism 200 may include at least one radiation fin 210 and at least one radiation groove 220 , preferably, a plurality of radiation fins 210 and a plurality of radiation grooves 220 . In the latter case, the radiation fins 210 are first formed at a predetermined interval and the radiation grooves 220 are formed between the radiation fins 210 . In other words, the radiation fins 210 and the radiation grooves 220 are alternatively arranged, which is very advantageous for the radiation. Thus, the combination of the radiation fins 210 and the radiation grooves 220 increases the radiation area, so that more efficient radiation is performed.
[0040] As described above, the washing machine according to the present invention has the following advantages.
[0041] First, since the air fed to an inside of the drum permeates to a deep place of the drum to uniformly dry all laundries, drying efficiency and performance are enhanced.
[0042] Secondly, since the drying duct is connected to the tub unlike in the typical washing machine, wearing and tearing of the gasket are solved.
[0043] Thirdly, the radiation mechanism provided in the upper cover of the drying duct effectively discharges a large amount of heat from the drying duct. To this end, a very small amount of heat is transferred to the tub, thereby preventing the tub from being deformed.
[0044] It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention. 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. | Provided is a washing machine having an enhanced drying performance. The washing machine includes: a housing; a tub installed inside the housing, for storing washing water; a drum rotatably installed inside the tub and configured to wash laundry; a drying duct connected to the tub, for generating hot air and feeding the generated hot air to an inside of the drum; a condensation duct connected to the tub and the drying duct, for removing moisture from an air discharged from the tub to guide the moisture-removed air to the drying duct and allowing the hot air to cross the inside of the drum together with the drying duct; and a radiation mechanism disposed at the drying duct, for radiating heat of the drying duct. | 3 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention generally concerns gaming tokens such as disks or flat plaques integrating an electronic chip or an electronic identifier (indifferently called hereafter electronic identification device). The applications for this invention are to be found, amongst others, in the contactless identification of persons and objects also called electronic labelling and in the authentication, the identification and management (in particular the tracing and counting) of gaming tokens also called casino chips. The expression “gaming token” covers any token that can be used in a gaming room and representing a value that is predetermined or not. Gaming token are usually made of a rigid plastic material to obtain a structure that is solid enough to resist conditions of use in casinos which are often very tough.
2. Description of Background and Relevant Information
The patent application EP-A-0694872 in the name of the Applicant describes a gaming token or plaque the body of which integrating an electronic chip is made from laminated sheets of rolled plastic material. The electronic chip or electronic identifier includes an electronic circuit with a memory bearing identification and/or coding information concerning the person or object associated with the token (electronic label) or the token itself (gaming token or payment token), the electronic circuit generally being associated with an emitter-receiver connected to an antenna and adapted to be supplied by inductive coupling. The electronic chip is placed in the centre of an opening provided in the body of the plaque, protected and held on either side by two rigid pellets and finally made one and integrated into the body of the plaque by a lamination of top sheets of transparent cellulose acetate followed by the thermoforming of the whole.
The manufacturing process for the body of the plaque incorporating the electronic chip by laminating thin sheets of plastic material described in the above mentioned patent application is well adapted to highly decorated plaques and representing a high nominal value, usually manufactured in small or medium sized series. However, a good protection of the electronic chip when it is integrated into the body of the plaque requires a certain thickness (usually between 4 and 6 mm) so gaming tokens or plaques with a thickness of about 3 mm and equipped with an electronic chip are difficult to manufacture using this method with an excessive number of rejects resulting from the destruction of the chip.
Among the less expensive manufacturing methods for gaming plaques and tokens, the thermocompression method of a plastic compound in a mould giving the final shape of the token is known from the U.S. Pat. No. 3,968,582. As a variant, peripheral inserts of various colours are obtained by the partial elimination of the plastic compound around the token preform and replacement by inserts of a coloured material before the thermocompression operation. The tokens thus obtained, however, offer a poor visual quality decoration and do not include any electronic identifier.
SUMMARY OF THE INVENTION
One object of the invention is to propose a new manufacturing method for tokens with an electronic identifier, simple in structure, compact and robust, particularly for namely thin tokens, allowing easy and inexpensive manufacture suitable for mass production.
For this purpose, the invention proposes a gaming token or plaque or similar device, including a flat body with approximately parallel surfaces, made of plastic with a cavity in which an electronic identification device is placed, characterised in that the cavity offers at least one face opening closed by a plastic plug inserted into the cavity and made one directly with the flat body.
The structure of the gaming token or plaque according to the invention and in which the plastic plug is inserted into the cavity and made one directly with the plastic of the token makes the token very robust while reducing its thickness (by eliminating any superfluous layer of plastic). Furthermore, the simplification of their structure makes the tokens in accordance with the invention much more easy to manufacture. Preferably, in variants of the realisation of the invention plugs are used inserted with a minimum clearance in the face openings of the cavities having matching shapes and directly made one with the body of the token or plaque by gluing, welding (fusion/welding or ultrasonic welding) and/or mechanical interlocking, for example by deformation by heating and/or compression of the token body at and around the area of the surface opening of the cavity and fold down plastic material around the plug, preferably previously bevelled.
According to a one, embodiment of the invention, the plug, inserted into the cavity in a solid state, possibly softened or pasty, is deformed and welded to the body of the token by combined heating and pressure. As it is described in the rest of the disclosure, the heating of the body and/or token may take place before the pressure is applied and/or simultaneously with the application of the pressure depending on the plastics used, on the shapes of the items to be welded and the heating and press devices used.
Thus, the deformation capacity of the plug reduces the risks of deterioration of the electronic identifier while ensuring a very robust weld, most often with interlocking, at the level of the side wall of the cavity and a good cohesion between the token body thus completed and the electronic identifier. Preferably, the combined application of heating and pressure extends over the plug and over the two entire faces of the body, which generally allows a good surface aspect to be obtained at once on both faces of the token or plaque.
According to a first variant, the body has a through cavity closed by two plugs placed on either sides of the electronic identification device. This arrangement allows a better distribution of the stresses on the electronic identification device when the welding operation by combined heat and pressure is carried out.
According to another variant, the body offers a non-through cavity with a flat or stepped bottom intended to receive all or part of the electronic identification device and closed by a plug.
Preferably, the electronic identification device includes an electronic circuit having a memory containing information concerning the token, for example an identification code and an emitter-receiver with a peripheral antenna adapted to be supplied by inductive coupling, the whole being placed in a protective enclosure such as a thin film flat envelope, a protective shell made of rigid plastic or a hardened coating resin pellet, especially of the epoxy type. Preferably, the electronic identification device and the protective enclosure are in the form of a flat disk with a smaller diameter than the diameter of the cavity so that it can be fitted at least partly into the housing formed by the stepped bottom of the cavity.
According to another embodiment of the invention, the body and or the plug are each made of an identical or different thermoplastic material, loaded or not, and showing a vitreous transition temperature of between 40° C. and 130° C., preferably between 50° C. and 100° C.
As various variants of embodiments of the invention using bodies and plugs of thermoplastic material in general, the bodies and plugs are each made of a thermoplastic material, loaded or not, and belonging to one of the following families:
the styrenes and their copolymers, in particular PBS and ABS, the methacrylics, in particular PMMA, the vinyls in particular PVC and their copolymers, the celluloses, in particular cellulose acetate, the saturated polyesters, in particular PBT and the polyolefins, in particular PE hd and their copolymers.
According to yet another embodiment of the invention, the body and the plug are made of identical or different thermosetting plastic, loaded or not, namely a material belonging to the family of non-saturated polyesters.
Preferably, but as an option, the body and the plug for the last two embodiments of the invention presented above are made of plastic materials having the same basic polymer, so as to facilitate in particular the welding between the body and the plug, or of plastic material compatible with the welding.
The invention also concerns a method of manufacturing a gaming token or plaque or similar device, hereinafter indifferently called token, with a thermoplastic body, including the following operations:
manufacturing by groups or by unit, of the thermoplastic token body,
making of a cavity in the body having at least one face opening,
making in the cavity of the electronic identification device and insertion of a plug, in each face opening,
closing of the cavity by welding of the plug(s) with the token body previously heated, in particular and around the area of each opening by applying pressure to the heated area(s),
as an option, cutting of the contour of the token body and/or finishing of the edge of the token if necessary.
The invention also concerns a method of manufacturing a gaming token or plaque or similar device, hereinafter indifferently called token, with a thermosetting body, characterised in that it includes the following operations:
manufacturing of a preform of the token body in a thermosetting plastic material,
making of a cavity in the preform having at least one face opening,
placing of the electronic identification device in the cavity and insertion of a plug, in each face opening,
placing in a mould of the whole composed of the preform of the token body equipped with the electronic identification device and plug(s),
making of the token body by thermocompression of the whole and closing of the cavity in the token body.
It should also be noted that the invention is not limited to gaming tokens and plaques, but also concerns similar devices equipped with an electronic chip and having similar shapes and structures, in particular fixed amount prepaid tokens and electronic payment tokens, electronic labels, plaques or electronic identification cards and it should also be noted that electronic identification may sometimes be limited to a simple authentication of the electronic chip, i.e. the recognition of the presence of the chip by the associated contactless reader (radio-frequency reader also called RFID reader) for electronic transaction (read and/or write).
Other objects, characteristics and advantages of the present invention will appear on reading the following description of various embodiments of the invention including methods of manufacturing therefor and given as non restricting examples in reference to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a perspective view of a gaming plaque made of thermoplastic material with a through cavity in accordance with a first embodiment of the invention;
FIG. 2 shows a longitudinal sectional view in a plane perpendicular to the plaque and passing through the line AA, of the plaque body of FIG. 1 equipped with the electronic identifier before fixation of the plugs;
FIG. 3 shows a longitudinal sectional view in a plane perpendicular to the plaque and passing through the line AA, of the plaque of FIG. 1 after fixation of the plugs;
FIG. 4 shows a longitudinal sectional view similar to FIG. 2 concerning a variant of the plaque of FIG. 1 with a non through cavity before fixation of the plug;
FIG. 5 shows a longitudinal sectional view similar to FIG. 3 concerning the variant of the plaque of FIG. 1 with a non through cavity shown in FIG. 4 after fixation of the plug;
FIG. 6 shows a perspective view of a gaming token made of thermosetting material with a non-through cavity in accordance with a second embodiment of the invention;
FIG. 7 shows a diametral sectional view, in a plane perpendicular to the token and passing through line BB, of the preform of the body of the token in FIG. 6, equipped with the electronic identifier and the plug before the thermocompression operation;
FIG. 8 shows a diametral sectional view, in a plane perpendicular to the token and passing through line BB of the token of FIG. 6, after the thermocompression operation;
FIG. 9 shows a diametral sectional view of the electronic identification device integrated into the plaques and tokens in accordance with the invention; and
FIGS. 10 a and 10 b illustrate the technique used to interlock the plug into the token body and each shows a sectional view respectively before and after compression on the token body.
It should be noted that the plaques and tokens illustrated in the drawings presented above are shown to a scale that is larger in thickness to facilitate the understanding of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
FIGS. 1 to 3 concern a first embodiment the token or plaque in accordance with the invention with a deformable plug and according to which the body of the token or plaque is composed of a thermoplastic material, in the present case a gaming plaque 10 approximately rectangular shown in perspective, the flat body 12 of which shows two approximately parallel faces 13 and 14 . The plaque integrates a chip or electronic identifier 16 placed in a cavity 15 crossing through the body 12 perpendicular to the faces 13 and 14 as seen in FIG. 2 (and represented in FIG. 1 by dashes). Of course the description of this embodiment of the invention also applies to disk shaped token with a circular contour and to flat tokens or plaques with various contours, namely elliptic.
Generally, the electronic identification device 16 (shown as a cross-section in FIG. 9) includes an electronic circuit 25 with a PROM memory containing information on the token and or the person or object associated with the token, for example a fixed digital or alphanumerical identification code of 64 bytes (including one or several fields such as: the serial number, the identification of a product, batch or place, a digital value associated with the token, etc.), and an emitter-receiver 26 with a peripheral circular antenna 27 adapted to be fed by inductive coupling from the modulated waves of the reader station (not shown). Practically, the emitter-receiver is capable of exchanging data without contact by modulated waves with a remote reader station (for example, between 15 cm and 2 m), the working frequency lying being 10 kHz and 20 MHz. The electronic device containing a memory for example can be used as a protection against theft and/or to facilitate the management and inventory of a batch of objects in a defined space (storage areas, warehouses, stores). Of course, without going beyond the scope of the invention, the electronic device 16 equipped with a memory of a non-reprogrammable type (read-only) can be replaced by a changing code reprogrammable device with possibility of reading and writing to the memory.
The electronic identification device 16 including the emitter-receiver 26 and the peripheral antenna 27 is placed between two thin and resistant plastic films 28 welded on the periphery to form a protective envelope, the whole being in the form of a thin pellet 29 of a maximum thickness of around one millimetre and a diameter of between 10 and 20 mm. As a result, the cavity 15 has a cylindrical shape with a circular base of a diameter slightly greater by a few millimetres (see FIG. 2) thus avoiding a premature deterioration of the electronic chip when the electronic identifier is placed in the cavity. Furthermore, without going beyond the scope of the invention, cavities with various sections (namely rectangular) are used to house the electronic identifiers the antennas of which have matching contours (namely rectangular).
It should be noted that the invention is not limited to this type of thin film protection of the electronic identifier, but also concerns the integration of any electronic identifier in its protective enclosure, namely identifiers enclosed in a rigid plastic shell, for example a shell made of injected plastic for an electronic label such as described in the patent application WO-A-98/39989 in the name of the Applicant, or embedded in a hardened resin in particular of the epoxy type. Practically, the choice of the protective enclosure depends on the level of protection required for the electronic chip itself and necessary to allow the chip to resist the rise in temperature and pressure when the cavity is closed and the plug welded.
The body 12 of the plaque can be realised indifferently either by the unit, for example by injection moulding, the cavity, whether crossing through the body or not, being obtained directly during moulding, or in group from thick sheets or strips (monobloc or welded, glued or laminated multiple layers) of predimensioned thermoplastic material either having the final thickness of the plaque or token, for example 3 mm (in the event of limited surface compression) or a slightly greater thickness, for example 4 mm for 3 mm (in the event of compression over the whole face of the plaque or token such as illustrated in FIGS. 3 and 5 ), the other dimensions possibly reaching one meter.
According to a first variant with a through cavity illustrated in FIG. 2 the thick sheet or strip is pierced with the number of holes corresponding to the number of plaques or tokens to be produced, the degrouping of the plaques or tokens obtained by cutting and punching or by milling the contour of the plaque or token, cut also called trimming, being carried out at the end of manufacture after integration of the electronic identifier 16 and closing of the cavity.
According to another variant, the thick sheet or strip is softened by heating (between 50° C. and 150° C.) and punched to obtain individually the body 12 , 12 ′ of the token or plaque. Simultaneously, the cavity intended to be used as housing recess for the electronic identifier is realised:
either as a through hole 15 by punching or cutting out,
or as a blind hole, non-through cavity 15 ′ with a flat bottom 24 ′ or a stepped bottom, either by die stamping on a part that is still hot or by non-opening spot facing with a milling cutter on a harder cooled part. For example, the cavity has a depth of approximately 2 mm.
The plugs 19 , 20 , 19 ′ are obtained for example by punching (cold or hot if necessary) from plates or strips with a thickness of between 1 and 1.5 mm.
As shown in FIG. 2, the through cavity 15 has two face openings 17 and 18 . The integration of the electronic identifier 16 starts by placing it between the two plugs 19 and 20 .
The plugs 19 and 20 are inserted (with the electronic identifier 16 ′) in the cavity 15 preferably with a minimum clearance in solid state, sometimes softened or pasty, deformable during the later stage of compression or welding. The plugs 19 and 20 have a contour that matched that of the cavity 15 , e.g. a circular contour, and have a thickness that makes their two external faces slightly overlap that of the faces 13 and 14 of the body 12 so as to ensure the complete filling of the cavity 15 and a solid weld with mechanical interlocking more or less undulated 25 (see FIG. 3 ), in the side wall 23 of the cavity when the face openings 17 and 18 are closed.
As a non restricting example, the body 12 and the plugs 19 and 20 are made of the same thermoplastic material, in this case loaded between 50% and 70% with barite or barium sulphate, chosen from among one of the following polymer families:
the styrenes and their copolymers,namely polybutadienestyrene (PBS) and acrylonitrile-butadiene styrene (ABS),
the methacrylics, namely polymethylmethacrylate (PMMA),
the vinyls, namely polyvinyl chloride (PVC) and their copolymers,
the celluloses, namely cellulose acetate,
the saturated polyesters, namely polybutyleneterphtalate (PBT),
and the polyolefines, namely high density polyethylene (PE hd) and their copolymers.
Still within the scope of the present invention, it should be noted that good weld joints can also be obtained by using for the body and plugs couples of different polymer based thermoplastic materials offering a good compatibility to be welded together, for example the couples ABS/PMMA, ABS/PBT and PVC/PBT. In any case, the undulated mechanical interlocking at joint level reinforces the weld.
The integration of the electronic identifier ends with the heating and compression (respectively shown in FIG. 3 by the straight arrows P and the curved arrows C) of the plugs 19 and 20 and the body 12 using a press, the hot plates 21 and 22 of which are arranged opposite each plug 19 and 20 on either side of the body of the plaque 12 . These hot plates 21 and 22 which cover the whole surface of the faces 13 and 14 of the body of the plaque or token are mobile by bringing one close to the other by any known arrangement (not described) so as to push sufficiently, but not in excess, the plugs 19 and 20 towards the inside of the cavity 15 so as to embed the thin pellet or protective envelope 29 of the identifier 16 and to hold the latter in position. The controlled movement of the press with plates 21 and 22 enables the body of the plaque or token to be obtained directly at the required final thickness (for example 3 mm) the excess material being pushed to the edge of the token, the body in addition undergoing a slight optional reduction of its thickness (for example, approximately one millimetre).
In special situations, and in particular depending on then types of thermoplastic materials used for the bodies and plugs, the heating temperature is generally between 100° C. and 160° C. and the pressure applied generally between 1 and 10 Mpa (10 to 100 bars). Furthermore, it may be preferable to start heating the body and/or plug before applying the pressure on the plugs and/or body.
As shown in FIG. 3, the plugs 19 and 20 , under the combined action of the heat and the pressure applied to each face 13 and 14 , are deformed to become welded to the side wall 23 of the cavity 15 and most often form fitting and interlocking undulations 15 when the face openings 17 and 18 are closed, the limit of the welding area disappearing (at least on the surface), when using identical or almost identical thermoplastic material of the same colour for the plugs 19 and 20 and the body of the plaque 12 . Thus, the creation of a real mechanical interlocking between the plug and the side of the cavity reinforces the weld joint. This interlocking is obtained more easily when heat and pressure are applied on the whole of the token face (the plastic flow being facilitated) rather than within an area limited to the plug and immediate surroundings of the face openings for the body.
In some cases, it is possible for the volume of the two plugs 19 and 20 to be slightly greater than the volume required to completely fill the cavity 15 once the identifier 16 has been installed, the excess material on the faces 13 and 14 after closing of the cavity 15 being caused to creep towards the edge of the body of the token or plaque.
The manufacture of the plaque (or token) continues with the cutting of the contour of the body in the event of group production from a thick sheet and/or the finishing of the edge, if necessary. As an option, it is possible to create a sunk decoration or a new hollow cavity (1 to 2 mm) by die punching and/or the placing of a surface decoration on the faces of the plaque (or token), for example by pad printing, hot punching or screen printed and heat bonded covering labels on the faces of the plaque (or token), etc.
FIGS. 4 and 5 concern a plaque 10 ′ variant of the plaque 10 (or token) described above and distinguished from the latter by a non through cavity 15 ′. Of generally similar structure, plaques 10 and 10 ′ have a large number of identical or similar technical characteristics, the description of which will not be repeated in detail below and which have the same numerical references accompanied by the sign′.
As shown in FIG. 4, the cavity 15 ′ of the plaque 10 ′ has a flat bottom 24 ′ approximately parallel to the faces 13 ′ and 14 ′ and distant from the sole face opening 17 ′ so as to place the electronic identifier 16 ′ in median position in the thickness of the body 12 ′ with its circular peripheral antenna in parallel position with the faces 13 ′ and 14 ′ of the plaque 10 ′. As with the plaque 10 , a solid but deformable thermoplastic plug 19 ′ is first of all inserted into the face opening 17 ′ after placing the identifier 16 ′ in the cavity 15 ′ then welded with undulated mechanical interlocking 25 ′ to the side wall 23 ′ of the cavity 15 ′ by heating and compression. Here again, the plug 19 ′ slightly extends beyond the face 13 ′ and has a sufficient volume to fill the cavity, extending around the periphery of the electronic identifier. It should be noted that it may be practical to heat the bottom 24 ′ of the cavity 15 ′ through the bottom heating plate 22 ′ to ensure a good support between the electronic identifier 16 ′and the wall of the bottom 24 ′. In some cases, a spot of glue can be placed between the bottom 24 ′ and the identifier 16 ′.
The invention is not limited to the ways, of heating and compression or thermocompression described herein, but concerns the use of technically equivalent ways known to specialists. In particular, the expression “heating” is used in a wide sense and covers more especially heating by electrical resistances, high frequency, micro-wave or infrared heating. Within the scope of the invention it is also possible to physically separate the ways of heating from the ways of compression (plate press). Finally, in certain variants of the realisation of the invention, the plug(s) are preheated before being inserted into the cavity. It is also possible to preheat or to heat during final compression the whole body of the token or plaque. In the same way, the pressing ways can be limited in surface for the thermoplastic material or cover the whole face of the token or plaque for both the thermoplastic material and thermosetting material (as described below), thus allowing a token or a plaque to be obtained with a good surface condition and a high quality visual aspect.
FIGS. 6, 7 and 8 concern a second embodiment of the token or plaque according to the invention and according to which the body of the token or plaque is made of a thermosetting plastic material, in this case a gaming token 30 shown in perspective the flat body 32 of which has two approximately parallel faces 33 and 34 .
Generally, the structure of the token 30 is similar to that of the plaque 10 ′ and its description will not be repeated in detail, especially for the same elements.
The token 30 integrates an electronic identifier 36 , identical to the electronic identifier 16 described above, placed in a cavity 35 made in the body 32 , the antenna of the identifier 36 being placed approximately parallel to faces 33 and 34 . Practically, the body 32 is realised from a preform made of thermosetting material including a non-through cavity 35 entering into the body 32 at right angles to faces 33 and 34 visible in FIG. 7 . The cavity 35 is obtained either directly when the preform is realised (cold premoulding), or by removing material. As an option, the bottom 40 of the cavity has a central step to determine a housing recess 44 for the electronic identifier 36 .
As shown in FIG. 7, the cavity 35 with a central stepped bottom 40 forming a housing 44 includes a face opening 37 . The integration of the electronic identifier 16 begins with its placing inside the housing 44 of the cavity 35 approximately at half height followed by the insertion of a plug 39 in the face opening 37 of the cavity 35 . The preform of the body of the token is placed in a heating mould 41 , 42 of which only the bottom part 42 is shown in FIG. 7 .
The plug 39 is inserted in the cavity 35 , preferably with a minimum clearance in a solid but deformable state during the later welding stage and offers a sufficient volume to completely fill the cavity 35 and a good weld with the side 43 of the latter when the face opening 37 is closed.
The plug 39 (as well as the body) is made of a thermosetting material, loaded or not; for example a polymer chosen from among the non saturated polyesters loaded between 50% and 70% in weight with barite or barium sulphate.
The integration of the electronic identifier ends with a thermocompression operation with the combined action of heat and pressure in the mould 41 , 42 , with a temperature of between 120° C. and 160° C. and an applied pressure of between 0.2 and 1 Mpa (between 2 and 10 bars).
As shown in FIG. 8, the plug 39 and 20 under the combined action of heat and pressure applied to each heated area looses its shape and welds with undulated mechanical interlocking 43 to the side wall of the cavity 35 and closes the face openings 37 , the limit of the welding area disappearing (at least on the surface) in the event of identical or almost identical thermosetting materials for the plug 39 and the body or the token 32 .
Of course, the description of this second embodiment of the invention also applies to rectangular plaques and flat token or plaques with various contours, especially elliptic, as well as to plaques and tokens with through cavities closed by two plugs.
Thus, thanks to the invention described herein, especially in its two preferred embodiments, it is possible to obtain gaming plaques and tokens with electronic identifiers, or similar devices approximately 3 mm thick, of good quality and at a low cost.
The invention is not limited to the use of deformable plugs to close the cavities of the tokens and plaques. Within the scope of the invention, in the variants not described plugs are used that are inserted with a preferably minimum clearance into the face openings of the cavities with a matching shape and directly made one with the body of the token or plaque by gluing or welding (fusion welding or ultrasonic welding) or mechanical interlocking. In one variant of the invention shown in FIGS. 10 a and 10 b , the mechanical interlocking is realised after placing the electronic identifier 46 in the cavity 45 by deformation by heating and/or compression of the token body 48 at the level of the surface opening 47 of the cavity 45 and fold down plastic material 53 around the plug 49 , preferably previously bevelled (bevel 52 ). | A device and method making the device. The device includes a flat body made of a plastic material. The flat body has at least two parallel faces and a cavity which opens to at least one of the at least two parallel faces. The cavity is adapted to receive an electronic identification device. At least one plug made of a plastic material is included. The at least one plug is adapted to be inserted into the cavity. The electronic identification is retained in the flat body when the at least one plug is inserted into the cavity. The method includes making the flat body, forming the cavity in the flat body, placing the electronic identification device in the cavity, inserting the at least one plug in the cavity, and fixing the at least one plug to the flat body. | 0 |
FIELD OF THE INVENTION
[0001] The present invention relates to the field of nonwoven fabrics such as those produced by the meltblown and spunbonding processes. Such fabrics are used in a myriad of different products, e.g., garments, personal care products, infection control products, outdoor fabrics, and protective covers.
BACKGROUND OF THE INVENTION
[0002] Bicomponent fibers are fibers produced by extruding two polymers from the same spinneret with both polymers contained within the same filament. The advantage of the bicomponent fibers is that it possesses capabilities that can not be found in either of the polymers alone. Depending on the arrangement and relative quantities of the two polymers, the structure of bicomponent fibers can be classified as core and sheath, side by side, tipped, microdenier, mixed fibers, etc.
[0003] Sheath-core bicomponent fibers are those fibers where one of the components (core) is fully surrounded by the second component (sheath). The core can be concentric or eccentric relative to the sheath and possessing the same or different shape compared to the sheath. Adhesion between the core and sheath is not always essential for fiber integrity. The sheath-core structure is employed when it is desirable for the surface of the fiber to have the property of the sheath such as luster, dyeability or stability, while the core may contribute to strength, reduced cost and the like. A highly contoured interface between sheath and core can lead to mechanical interlocking that may be desirable in the absence of good adhesion.
[0004] Generally, composite bicomponent sheath-core fibers have been used in the manufacture of non-woven webs, wherein a subsequent heat and pressure treatment to the non-woven web causes point-to-point bonding of the sheath components, which is of a lower melting point than the core, within the web matrix to enhance strength or other such desirable properties in the finished web or fabric product.
[0005] Poor abrasion resistance of Polyethylene/Polyethylene Terephthalate (PE/PET) sheath/core bicomponent spunbond has been an industry recognized problem since the last 10-15 years. Various approaches have been devised attempting to solve this problem. Similar problems also affect many other frequently used sheath/core structures such as PE/Polyesters (for example, Polybutylene Terephthalate (PBT), Polytrimethylene Terephthalate (PTT), Polylactide (PLA)), PE/Polyolefins, PE/Polyamide, PE/Polyurethanes.
[0006] A first method is directed to the modification of fiber structure to improve adhesion between the sheath and core component. For example, a mixture of EVA (ethyl vinyl acetate) and PE was suggested for a sheath component in U.S. Pat. No. 4,234,655, U.S. Pat. No. 5,372,885 teaches the use of a blend of maleic anhydride grafted HDPE and un-grafted LLDPE (linear low density polyethylene). A mixture of PE and acrylic acid copolymer was suggested in U.S. Pat. No. 5,277,974 and a blend of HDPE (high density polyethylene) with LLDPE was claimed in WO 2004/003278A1 as a sheath component.
[0007] An approach for improving abrasion resistance proposed is by increasing the bond area of the spunbond, for example, U.S. Pat. Appl. Publ. No. 20020144384 teaches a non-woven fabric with a bond area of at least about 16%, 20% or 24%. However, higher bond area samples results in loss of softness and drapeability of bicomponent spunbond, which is not desirable for many applications especially for medical apparel such as surgical gowns. At the other extreme, nonwovens with small bond areas tend to make soft feeling but very weak fabric.
[0008] Another approach involves the use of a number of treatments, such as multiple washings and chemical treatments.
[0009] Yet another approach, which is of particular relevance to the subject matter of this application, is directed to adopting a specific thermal bonding pattern for nonwoven fabric comprising a pattern having an element aspect ratio between about 2 and about 20 and unbonded fiber aspect ratio of between about 3 and about 10, as disclosed in U.S. Pat. No. 5,964,742. Such a pattern has been found to possess a higher abrasion resistance and strength than a similar fabric bonded with different bond patterns of similar bond area.
[0010] There remains a need for a nonwoven fabric without resort to chemical treatments having good bonding strength (i.e. tensile strength and abrasion resistance) yet also having good fabric softness, particularly at relatively high bonding area.
[0011] Accordingly, it is an object of this invention to provide a nonwoven fabric with a high bonding area while retaining softness and comparable or better tensile strength and abrasion resistance compared to fabrics bonded with other known patterns.
[0012] It is another object of this invention to provide a method of preparing a nonwoven fabric with a high bonding area while retaining softness and comparable or better tensile strength and abrasion resistance.
SUMMARY OF THE INVENTION
[0013] The objects of the present invention are met by a thermal bonding pattern for nonwoven fabric comprising a basket-weave pattern having a transition area ( 2 ) equal to at least 10% of bond spot area ( 1 ) in FIG. 1 , more preferably a transition area ( 2 ) equal to at least 50% of bond spot area ( 1 ), and most preferably a transition area ( 2 ) equal to at least 100% of bond spot area ( 1 ). It has been unexpectedly found that such a fabric has a higher abrasion resistance and strength than a similar fabric bonded with different bond patterns without the attendant loss of softness. The nonwoven fabric of this invention can be prepared using calendering and embossing processes. Although single pass, double pass, s wrap and 3 stack with idler can all be used, double pass is most preferred.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a drawing of a bond spot and a transition area.
[0015] FIG. 2 is a drawing of a bonding pattern satisfying the requirements of this invention and called the basket-weave pattern.
[0016] FIG. 3 is a drawing of a bonding pattern termed cross-hatch pattern.
[0017] FIG. 4 is a top view of a basket-weave pattern.
[0018] FIG. 5 is a cross-section of a nonwoven bonded using a basket weave pattern showing transition area “b” and bond spot area “a”.
[0019] FIG. 6 is an SEM cross-sectional image of a nonwoven web made by using a cross-hatch pattern which does not have a transition area.
[0020] FIG. 7 . is a drawing of the dimension of basket-weave pattern.
[0021] FIG. 8 is a drawing of the dimension of cross-hatch pattern.
DEFINITIONS
[0022] The term “spunbond” filaments as used herein means filaments which are formed by extruding molten thermoplastic polymer material as filaments from a plurality of fine capillaries of a spinneret with the diameter of the extruded filaments then being rapidly reduced by drawing. Spunbond filaments are generally continuous and usually have an average diameter of greater than about 5 microns. The spunbond filaments of the current invention preferably have an average diameter between about 5 to 60 microns, more preferably between about 10 to 20 microns. Spunbond nonwoven fabrics or webs are formed by laying spunbond filaments randomly on a collecting surface such as a foraminous screen or belt. Spunbond webs can be bonded by methods known in the art such as hot-roll calendering, through air bonding (generally applicable to multiple component spunbond webs), or by passing the web through a saturated-steam chamber at an elevated pressure. For example, the web can be thermally point bonded at a plurality of thermal bond points located across the spunbond fabric.
[0023] The term “nonwoven fabric, sheet or web” as used herein means a structure of individual fibers, filaments, or threads that are positioned in a random manner to form a planar material without an identifiable pattern, as opposed to a knitted or woven fabric.
[0024] The term “filament” is used herein to refer to continuous filaments whereas the term “fiber” is used herein to refer to either continuous or discontinuous fibers.
[0025] The term “multiple component filament” and “multiple component fiber” as used herein refer to any filament or fiber that is composed of at least two distinct polymers which have been spun together to form a single filament or fiber. Preferably the multiple component fibers or filaments of this invention are bicomponent fibers or filaments which are made from two distinct polymers arranged in distinct substantially constantly positioned zones across the cross-section of the multiple component fibers and extending substantially continuously along the length of the fibers. Multiple component fibers and filaments useful in this invention include sheath-core and island-in-the-sea fibers.
[0026] As used herein “thermal point bonding” involves passing a fabric or web of fibers to be bonded between a heated calender roll and an anvil roll. The calender roll is usually, though not always, patterned in some way so that the entire fabric is not bonded across its entire surface, and the anvil roll is usually flat. As a result, various patterns for calender rolls have been developed for functional as well as aesthetic reasons. One example of a pattern has points and is the Hansen-Pennings or “H&P” pattern with about a 30% bond area with about 200 pins/square inch as taught in U.S. Pat. No. 3,855,046 to Hansen and Pennings. The H&P pattern has square point or pin bonding areas. Another typical point bonding pattern is the expanded Hansen-Pennings or “EHP” bond pattern which produces a 15% bond area. Another typical point bonding pattern designated “714” has square pin bonding areas where in the resulting pattern has a bonded area of about 15%. Other common patterns include a diamond pattern with repeating and slightly offset diamonds with about a 16% bond area and wire weave pattern looking as the name suggests, e.g. like a window screen, with about an 18% bond area. Typically, the percent bonding area varies from around 10% to 30% of the area of the fabric laminate web. As is well known in the art, the spot bonding holds the laminate layers together as well as imparts integrity to each individual layer by bonding filaments and/or fibers within each layer.
[0027] As used herein, the term “garment” means any type of non-medically oriented apparel which may be worn. This includes industrial work wear and coveralls, undergarments, pants, shirts, jackets, gloves, socks, and the like.
[0028] As used herein, the term “infection control product” means medically oriented items such as surgical gowns and drapes, face masks, head coverings like bouffant caps, surgical caps and hoods, footwear like shoe coverings, boot covers and slippers, wound dressings, bandages, sterilization wraps, wipers, garments like lab coats, coveralls, aprons and jackets, patient bedding, stretcher and bassinet sheets, and the like.
[0029] As used herein, the term “personal care product” means diapers, training pants, absorbent underpants, adult incontinence products, and feminine hygiene products.
[0030] As used herein, the term “protective cover” means a cover for vehicles such as cars, trucks, boats, airplanes, motorcycles, bicycles, golf carts, etc., covers for equipment often left outdoors like grills, yard and garden equipment (mowers, roto-tillers, etc.) and lawn furniture, as well as floor coverings, table cloths and picnic area covers.
[0031] As used herein, the term “outdoor fabric” means a fabric which is primarily, though not exclusively, used outdoors. Outdoor fabric includes fabric used in protective covers, camper/trailer fabric, tarpaulins, awnings, canopies, tents, agricultural fabrics, and outdoor apparel such as head coverings, industrial work wear and coveralls, pants, shirts, jackets, gloves, socks, shoe coverings, and the like.
[0032] As used herein, the term “transition area” refers to an area in substrate surrounding the bond point area, where the fibers are sufficiently heated and compressed to exhibit some amount of bonding.
Test Methods
[0033] Stoll Abrasion Test was used for measuring the relative resistance to abrasion of a fabric in the examples presented hereinafter. The test results are reported on a scale of 0 to 5 with 5 being the most wear and 0 the least, after 100 cycles with a weight of 2.5 lbs. The test is carried out with a Stoll Quatermaster Abrasion tester such as model no. CS-22C-576 available from SDL Inc. or Testing Fabrics Inc. The abradant cloth used is a 3 inch by 24 inch with the longer dimension in the wrap direction. The test specimen size is a 4 inch by 4 inch.
[0034] The softness of a nonwoven fabric was measured according to the “Handle-O-Meter” test. The test used here is: 1) the specimen size was 4 inches by 4 inches and 2) five specimens were tested. The test was carried out on Handle-O-Meter model number 211-5 from Thwing Albert Instrument Co., 10960 Dutton Road, Philadelphia, Pa. 19154.
DETAILED DESCRIPTION OF THE INVENTION
[0035] In order to avoid the trade-off between the abrasion resistance and softness seen in most conventional patterns, the inventors have discovered a pattern termed basket-weave pattern which comprises a large transition area interconnecting bonded and non-bonded area. Such a pattern results in a soft nonwoven web with high abrasion resistance with a bond area as high as 50%, typically in the range of 5 to 50%.
[0036] FIGS. 7 and 8 show the dimension of patterns of basket-weave and cross-hatch, respectively. The roundness of basket-weave pattern contribute to the existence of noticeable transition areas.
[0037] The transition area works as a connection for both bonded and non-bonded area, and contributes to building-up the network structure, which strengthens the resistance of the fibers against the applied shear or normal stress during the abrasion process, without compromising softness and drapeability. It is also found that the integrity and amount of the transition area is critical for both abrasion resistance and softness, as basket weave with relatively large transition area gives this effect but other patterns with negligible transition area compromise softness greatly for similar improvement in abrasion resistance.
[0038] While not to be bound by theory, it is hypothesized that abrasion resistance is improved by the basket-weave pattern because more fibers are tied down by the existence of the transition area. However, since in the transition area, fibers are not fully melted and fixed, they have enough freedom to move, and because of the flexibility of the fibers softness does not deteriorate.
[0039] The method of conducting the thermal point bonding is also shown to affect the properties of the products. Examples of suitable calendering methods include single pass, double pass, S wrap etc. In most occasions, it was found that double pass calendering is preferred and especially suited for generating desirable combination of properties.
[0040] Tests of fabrics bonded with an example of the inventive pattern (basket weave pattern) and with representative conventional patterns are presented herewith showing the advantageous properties of the inventive pattern.
EXAMPLE 1
[0041] A nonwoven base material was produced using 40/60 PE/PET sheath/core bicomponent spunbond fibers through pressure bonding with cold calender rolls at room temperature at a nip pressure of 400 pli. The base material has a basis weight of 40 gsm.
[0042] For the test samples, the base material was thermally point bonded using basket-weave pattern with 30% bond area or using a diamond pattern with 40% bond area. Both bonding experiments were conducted at various calender temperatures (239-266° F. of both top and bottom rolls), and speeds (10-200 ft/min), and range of nip pressures (75-1500 pli).
[0043] The thermal point bonding was performed using an embossed roll and a smooth roll in a single pass. Both the test samples and control samples have a basis weight of 40 gsm.
[0044] The test data are summarized in Table 1.
[0000]
TABLE 1
Result
Additional Treatment Step
Bond
Temp.
Pressure
Abrasion
Material
Top Roll
Bottom Roll
Area (%)
(° F.)
(pli)
Resistance
Softness
Test BW1
Smooth
B-W
30
252
350
0.8
39.3
Test Dia1
Smooth
Diamond
40
266
75
1.3
23.9
Control 1
NA
NA
18
265
600
2.5
43.3
[0045] In Table 1, results are presented for two test samples against a control sample, i.e., a first test sample BW1 processed through a top roll of steel with smooth surface and a bottom roll of steel with basket-weave patterns and a second test sample Dial processed through a top roll of steel with smooth surface and a bottom roll of steel with diamond pattern.
[0046] It can be concluded that when the samples are bonded at single bonding step, basket-weave pattern at 30% bonding area not only showed better abrasion resistance than standard bonding pattern (oval, 18%), but also better than a diamond bonding pattern with 40% bonding area. As a surprising side effect, samples acquired a texture and bulkiness when embossed with basket-weave pattern with single pass (29% increase of thickness from 245 to 316 μm).
EXAMPLE 2
[0047] A nonwoven base material was produced using 40/60 PE/PET sheath/core bicomponent spunbond fibers through thermal bonding on a calender roll with an oval pattern with 18% bonding area at 265° F. and at a nip pressure of 600 pli. The base material has a basis weight of 40 gsm.
[0048] For the test samples, the base material was thermally point bonded using basket-weave pattern with 30% bond area. The bonding was conducted at various calender temperatures (239-266° F. of both top and bottom rolls), and a fixed speed of 10 ft/min and a nip pressure of 750 pli.
[0049] The thermal point bonding was performed using an embossed roll and a smooth roll in a double pass for the test sample.
[0050] The control sample was prepared in a single pass under the conditions specified in Example 1. Both the test and the control samples have a basis weight of 35 gsm.
[0051] The test data are summarized in Table 2.
[0000]
TABLE 2
Result
Additional Treatment Step
Bond
Temp.
Pressure
Abrasion
Material
Top Roll
Bottom Roll
Area (%)
(° F.)
(pli)
Resistance
Softness
Test BW2
Smooth
B-W
30
250
750
0.0
28.6
Control 2
NA
NA
18
265
600
2.3
30.6
[0052] In Table 2, results are presented for the test sample BW2 processed through a top roll of steel with smooth surface and a bottom roll of steel with basket-weave patterns and a control sample.
[0053] It can be concluded that when the basket weave pattern was used in the second bonding step, in conjunction with standard bonding pattern (oval, 18%) as the first step, the improvement in abrasion resistance was even greater compared to the basket-weave sample bonded in a single step (Example 1). As a surprising side effect, samples acquired a texture and bulkiness when embossed with basket-weave pattern with double pass (36% increase of thickness from 250 to 340 μm).
EXAMPLE 3
[0054] A nonwoven base material was produced using 40/60 PE/PET sheath/core bicomponent spunbond fibers through thermal bonding on a calender roll with an oval pattern with 18% bonding area at 265° F. and at a nip pressure of 600 pli. The base material has a basis weight of 40 gsm.
[0055] For the test samples, the base material was thermally point bonded using basket-weave pattern with 30% bond area. The bonding was conducted at a fixed temperature 276° F., at a fixed speed of 200 ft/min and at a nip pressure of 750 pli.
[0056] The thermal point bonding was performed using an embossed roll and a smooth roll in a double pass for the test sample.
[0057] The control sample was prepared in a single pass under the same conditions as the test material except that a single pass is used. Both the test samples and control samples have a basis weight of 40 gsm.
[0058] The test data are summarized in Table 3.
[0000]
TABLE 3
Result
Additional Treatment Step
Bond
Temp.
Pressure
Abrasion
Material
Top Roll
Bottom Roll
Area (%)
(° F.)
(pli)
Resistance
Softness
Test BW3
Smooth
B-W
30
235
400
0.5
29.1
Control 3
NA
NA
18
265
600
2.5
43.3
[0059] In Table 3, results are presented for the test sample BW3 processed through a top roll of steel with smooth surface and a bottom roll of steel with basket-weave patterns and a control sample.
[0060] It can be concluded that the basket weave pattern contributed to improving the abrasion resistance at the speed of 200 ft/min in a double pass setup while retaining softness.
EXAMPLE 4
[0061] A nonwoven base material was produced using 40/60 PE/PET sheath/core bicomponent spunbond fibers through thermal bonding on a calender roll with an oval pattern with 18% bonding area at 265° F. and at a nip pressure of 600 pli. The base material has a basis weight of 30 gsm.
[0062] For the test samples, the base material was thermally point bonded using a cross-hatch pattern with 22.7% bond area, using a diamond pattern with 17.1% bond area, and using a square pattern with 19% bond area at various speeds (98-656 ft/min), at a fixed temperature 257° F. for both top and bottom rolls and at a fixed nip pressure of 286 pli.
[0063] The thermal point bonding was performed using single pass, double pass or S wrap as shown in Table 4. The bottom roll is either absent or a Cold Steel Smooth Roll. The top roll, when present, is a steel roll bearing the respective patterns. All the samples have a basis weight of 40 gsm.
[0064] The test data are summarized in Table 4.
[0000]
TABLE 4
Additional Treatment Step
Bond
Result
Top
Middle
Bottom
Area
Process
T.
P.
Abrasion
Material
Roll
Roll
Roll
(%)
Setup
(° F.)
(pli)
Resistance
Softness
Control 4
NA
Smooth
NA
18
Single
265
600
2.0
13.3
pass
Test
Cross
Smooth
Cold
23
S wrap
257
286
1.8
21.4
CH1
Hatch
Smooth
Test
Cross
Smooth
NA
23
Double
257
286
1.0
25.1
CH2
Hatch
Pass
Test
Diamond
Smooth
Cold
17
S Wrap
257
286
1.3
32.8
Dia4.1
Smooth
Test
Diamond
Smooth
NA
17
Double
252
286
2.3
22.3
Dia4.2
Pass
Test
Square
Smooth
Cold
19
S Wrap
266
286
2.0
31.2
S4.1
Smooth
Test
Square
Smooth
NA
19
Double
257
286
0.5
49.1
S4.2
Pass
[0065] In Table 4, results are presented for the test samples processed using cross-hatch, diamond, or square patterns on a double pass or S wrap setup, compared to a control sample prepared using single pass setup.
[0066] It can be concluded that the cross-hatch pattern, despite its similarity in shape to basket-weave pattern, did not contribute to a noticeable improvement in the abrasion resistance with S Wrap configuration, but gave an improvement using double pass. Improvement in the abrasion resistance did not take place in diamond pattern for the cases of double pass configuration. Some improvement was noticed in abrasion resistance with S Wrap, but softness deteriorated. Improvement in an abrasion resistance took place in square pattern in case of double pass at the expense of softness.
EXAMPLE 5
[0067] Three nonwoven base materials, classified as “DG”, “LG” and “White”, were produced using 40/60 PE/PET sheath/core bicomponent spunbond fibers and posses a density of 30 gsm. “DG” and “LG” are fully bonded samples, which are thermally bonded on a calender roll (oval pattern, 18% bond area) at 275° F., at a nip pressure of 600 pli and at a speed of 550 ft/min. “White” is a lightly bonded sample, which is thermally bonded on calender roll (oval pattern, 18% bond area) at 215° F., at a nip pressure of 400 pli and at a speed of 550 ft/min.
[0068] For the test samples with basket-weave patterns, the base material was thermally bonded using basket-weave pattern with 30% bond area at various configurations (double pass, s wrap, and 3 stack with idler), at a temperature range of 230-275° F., at a nip pressure of 400-629 pli and at a fixed speed of 656 ft/min.
[0069] For the test samples with patterns other than basket-weave, the base material was thermally bonded using square-patterned sleeves with 33% bond area, square-patterned sleeves with 13% bond area, or square-patterned sleeves with 27% bond area, at a double pass, at a temperature range of 257-266° F., at a nip pressure of 343-514 pli and at a fixed speed of 98 ft/min.
[0070] All the samples have a basis weight of 30 gsm.
[0071] The test data are summarized in Table 5.
[0000]
TABLE 5
Additional Treatment Step
Bond
Result
Top
Middle
Bottom
Area
Process
T.
P.
Abrasion
Material
Roll
Roll
Roll
(%)
Setup
(° F.)
(pli)
Resistance
Softness
Control 5
NA
NA
NA
18
Single
265
600
2.5–3.5
12–13
pass
Test
BW
Smooth
Diamond,
30
S wrap
266
400–629
0.4–0.5
30–35
White 1
19%
Test DG
BW
Smooth
Diamond,
30
S wrap
266
400–629
0.2–0.4
33–46
19%
Test
BW
Smooth
Diamond,
30
3 stack
266
400–629
0.5–1.5
17–18
White 2
19%
with idlers
Test
BW
Smooth
NA
30
Double
266
75
0.5–2.0
12–15
White 3
Pass
Test LG
BW
Smooth
NA
30
Double
266
400–629
0.4–0.5
13–16
Pass
Test
Square
Smooth
NA
33
Double
266
343
0.5
57.3
White 3
Pass
Test
Square
Smooth
NA
13
Double
257
514
1.8
23.6
White 4
Pass
Test
Square
Smooth
NA
27
Double
257
343
0.4
33.7
White 5
Pass
[0072] It can be concluded that the basket-weave pattern at 30% bond area contributed to the improvement in the abrasion resistance significantly for processes of a double pass and a 3 stacks with idlers without compromising softness at the calender speed of 656 ft/min. Softness deteriorated in case of an s wrap whereas it was maintained in case of both a double pass and a double pass of 3 stacks with idlers. Square patterns of similar bond area (about 30%) with negligible transition area showed good abrasion resistance but with softness deteriorated. Square pattern with smaller bond area (13%) showed not only less improvement in abrasion resistance but also deteriorated softness. Strip tensile property was reserved after double pass of calendering with LG.
[0073] As hypothesized earlier, the existence of discernible transition area, as evidenced in FIG. 3 , in the thus produced basket-weave pattern is responsible for improving the abrasion resistance and the softness at the same time. In contrast, the lack of discernible transition area in the cross-hatch pattern, as shown in FIG. 4 , is responsible for its failure to improve softness while improving abrasion resistance.
[0074] The nonwoven sheets/webs with the advantageous patterns can of course be further processed or improved. For example, a laminate can be generated by laminating the nonwoven sheets bearing the patterns with a film. The nonwoven sheets/webs or the laminates can be stretched to generate perforations as desired for certain applications such as those described in U.S. Pat. No. 5,964,742.
[0075] Although only a few exemplary embodiments of this invention have been described in detail above, those skilled in the art will readily appreciate that many modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention. Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the following claims. | A thermal bonding pattern for nonwoven fabric possessing improved abrasion resistance while retaining softness, comprising a basket-weave pattern or other pattern having a transition area ( 2 ) equal to at least 10% of bonding spot area ( 1 ) in FIG. 1 , more preferably a transition area ( 2 ) equal to at least 50% of bonding spot area ( 1 ), and most preferably a transition area ( 2 ) equal to at least 100% of bonding spot area. | 3 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates in general to control devices for controlling automotive automatic transmissions, and more particularly to control devices of a type that includes a so-called speed change completion degree estimating system that estimates the speed change compression degree assumed by the transmission, particularly estimates, upon selection of a drive range from a non-drive range, the time (or timing) when a friction element needed for the drive range starts its actual engaging operation following completion of piston stroke thereof.
2. Description of Related Art
In an automotive automatic transmission, there are installed a plurality of friction elements, such as clutches and brakes, and a hydraulic actuating means for selectively actuating the friction elements. That is, by actuating the friction elements that are selected, a certain power transmission path is provided to establish a desired gear, and by switching the friction elements that are to be actuated, another power transmission path is provided to establish another gear while carrying out a speed change of the transmission.
The transmission is powered by an engine through a torque converter. That is, the torque inputted to the transmission is outputted therefrom while being subjected to a speed change according to a selected gear.
One of the speed change completion degree estimating systems is described in Japanese Patent First Provisional Publication 6-109130. The system is constructed to estimate, upon selection of a drive range from a non-drive range, the time (or timing) when a friction element needed for the drive range starts its actual engaging operation following completion of piston stroke thereof, by detecting a speed drop from the torque converter to the transmission. That is, before starting of the engaging operation of the friction element, the hydraulic pressure for the element is so controlled as to obtain an optimum piston stroke, and after starting of the engaging operation, the hydraulic pressure is so controlled as to obtain an optimum speed change. That is, the completion of the piston stroke, namely, the timing of starting the actual engaging operation of the friction element is estimated by the drop of rotation speed of input means of the transmission.
Japanese Patent First Provisional Publication 4-366063 describes another system that estimates completion of the piston stroke, namely, the time of starting the actual engaging operation of a friction element. In this system, when, upon selection of a drive range from a non-drive range, a speed ratio between input and output speeds of a torque converter is reduced to indicate a value corresponding a drop of an input means of the transmission, estimation is so made that the friction element has finished the piston stroke, namely, started its actual engaging operation.
SUMMARY OF THE INVENTION
In the above-mentioned known systems, the estimation for completion of the piston stroke is based on the assumption that when, under standstill of an associated motor vehicle, the rotation speed of an output shaft of the transmission is 0 (zero) and when, due to engagement of the friction element, the input and output shafts of the transmission are engaged, the rotation speed of the input shaft is 0 (zero), and even under this condition, the engine is able to keep its operation due to a slip effect of the torque converter.
Accordingly, the above-mentioned systems have the following weak points due to their constructional inherence.
That is, if, during running of a vehicle (viz., transmission output shaft speed>0), the driver moves the shift lever from D-range to N-range by mistake and then noticing the mistake, he or she returns the shift lever back to D-range, there is such a possibility that the rotation speed of the turbine of the torque converter (viz., transmission input shaft speed) increases with progress of the speed change in the transmission. In this case, the estimation to completion of the piston stroke of the friction element (namely, the timing of starting the actual engaging operation of the element) is not achieved.
The above matters will be clearly understood from the following explanation which is made with the aid of FIGS. 7 to 10 .
That is, as is shown in FIG. 7, when, at time “t 1 ”, the driver moves the shift lever back to D-range from N-range upon noticing the miss-shifting, a command value “Po” of hydraulic pressure of the friction element is set to instantly increase the pressure to a relatively high level for instantly completing the piston stroke as shown. However, actually, the hydraulic pressure “Pc” fed to the friction element is forced to increase with a certain time lug, as is indicated by a solid curve.
However, during running of the vehicle, it sometimes occurs that with starting of actual engaging operation of the friction element at time “t 2 ”, the turbine rotation speed “Nt” (viz., transmission input shaft speed) is increased as shown in FIG. 7 irrespective of the engine rotation speed “Ne”. In this case, detection of the time “t 2 ” when the piston stroke of the friction element is completed (viz., the actual engaging operation starts) is not achieved by the above-mentioned known estimation system because the system is constructed to use the drop of the turbine rotation speed “Nt” as a sign of that completion.
Thus, in reality, upon sensing such sign, it becomes necessary to set the command value “Po” to assume the character as shown by the alternate long and two short dashes line in order that, after the time “t 2 ”, the turbine rotation speed “Nt” is smoothly increased to the level “No” of transmission output shaft speed. (In the illustrated example, explanation is based on third gear having a gear ratio of 1:1, and thus, the level is equal to the transmission output shaft speed “No”). Thus, it is necessary to control the actual hydraulic pressure “Pc” in a manner as is indicated by the alternate long and short dash line.
However, actually, due to the above-mentioned reasons, even after the time “t 2 ”, the command value “Po” is kept high that is set for controlling the piston stroke.
Accordingly, in the above-mentioned known system, the actual hydraulic pressure “Pc” is forced to increase rapidly toward and finally to the level of the higher command value “Po”, as is indicated by the solid line, so that after the time “t 2 ”, the turbine rotation speed “Nt” is rapidly increased to the transmission output shaft speed irrespective of a desired speed acceleration gradient, inducing a possibility of a marked select shock.
Furthermore, as is shown in FIG. 8, after the time “t 2 ” when the actual engaging operation of the friction element starts following completion of the piston stroke effected by the actual hydraulic pressure “Pc” that is increased to follow the command value “Po” of hydraulic pressure due to the shift back of the shift lever from N-range to D-range at the time “t 1 ”, it becomes necessary to increase the command value “Po” of hydraulic pressure in such manner as is indicated by the alternate long and short dash line for the purpose of smoothly effecting the change gear. However, in the known system, for the abovementioned reasons, the timing, viz., the time “t 2 ”, of starting the actual engaging operation of the friction element can not be detected because the shifting from N-range to D-range is made under running of the associated vehicle. Thus, in the known system, even after the time “t 2 ”, the command value “Po” of hydraulic pressure for the friction element is kept at the value for controlling the piston stroke as is indicated by the solid line, and thus, the actual hydraulic pressure “Pc” is settled to the kept value of the command value “Po” without increasing.
Accordingly, in reality, after the time “t 2 ”, with progress of the gear changing operation, it becomes necessary to smoothly bring the turbine rotation speed “Nt” to the transmission output shaft speed as is indicated by the alternate long and short dash line. In the illustrated example, the gear ratio is 1:1 because of taking the third gear, and thus, the turbine rotation speed “Nt” is equal to the transmission output shaft speed. However, actually, due to the above-mentioned reasons, as is indicated by the solid line, the turbine rotation speed “Nt” fails to reach the transmission output shaft speed (viz., “No”), and thus, an actual speed change progress is stopped and thus subsequent control for the hydraulic pressure is suppressed.
In order to eliminate the weak points possessed by the above-mentioned known systems, the following measures may be thought out, which will be described with reference to flowcharts of FIGS. 9 and 10. As will become apparent hereinafter, in such measures, estimation for completion of the piston stoke is carried out in respective cases.
That is, in step S 31 of the flowchart of FIG. 9, the variation direction of the turbine rotation speed “Nt” is derived, in such a manner as is depicted in the flowchart of FIG. 10 .
In FIG. 10, at step S 41 , a current turbine rotation speed “Nt 1 ” is read, and at step S 42 , a turbine rotation speed “Nt 2 ” after gear change is calculated from the following equation:
Nt 2 =(gear ratio set after gear change)×(transmission output shaft speed “No”) (1)
At step S 43 , judgement is carried out as to whether “Nt 1 ” is greater than “Nt 2 ” or not. If YES, the operation flow goes to step S 44 where it is judged that the turbine rotation speed “Nt” has lowered. While, if NO, the operation flow goes to step S 45 where it is judged that the turbine rotation speed “Nt” has increased. The result of the step S 44 or S 45 goes to step S 32 of the flowchart of FIG. 9 .
In the flowchart of FIG. 9, if it is judged that the turbine rotation speed “Nt” has lowered, the operation flow goes to steps S 33 and S 34 and judges the completion of the piston stroke (viz., starting of actual engaging operation) if the turbine rotation speed “Nt” is lower than a predetermined level. While, if it is judged that the turbine rotation speed “Nt” has increased, the operation flow goes to steps S 35 and S 36 and judges the completion of the piston stroke (viz., starting of actual engaging operation) if the turbine rotation speed “Nt” is greater than a predetermined level.
However, the applicant notes that the above-mentioned measures are not practical because of complicated steps for estimating completion of the piston stroke.
Accordingly, an object of the present invention is to provide a speed change completion degree estimating system of an automatic transmission, which can easily estimate the speed change completion degree in every gear changes of the transmission.
Another object of the present invention is to provide a speed change control device of an automatic transmission, which controls operation of a friction element of the transmission based on information provided by the speed change completion degree estimating system.
According to a first aspect of the present invention, there is provided a speed change completion degree estimating system for use in an automatic transmission driven by an engine through a torque converter, the transmission including a plurality of friction elements which are selectively engaged to provide a selected gear thereby to transmit the power of engine to an output shaft of the transmission while changing the rotation speed. The system comprises a first section that derives a difference (Nt−Ne) between an input rotation speed (Nt) of the transmission and an engine rotation speed (Ne); a second section that derives a difference (g×No−Ne) between the input rotation speed (g×No) of the transmission provided after completion of the speed change operation and the engine rotation speed (Ne); and a third section that calculates a speed change completion degree (Shift) of the transmission by using a ratio between the (Nt−Ne) and the (g×No−Ne).
According to a second aspect of the present invention, there is provided a method for estimating a speed change completion degree of an automatic transmission which is driven by an engine through a torque converter, the transmission including a plurality of friction elements which are selectively engaged to provide a selected gear thereby to transmit the power of engine to an output shaft of the transmission while changing the rotation speed. The method comprises deriving a difference (Nt−Ne) between an input rotation speed (Nt) of the transmission and an engine rotation speed (Ne); deriving a difference (g×No−Ne) between the input rotation speed (g×No) of the transmission provided after completion of the speed change operation and the engine rotation speed (Ne); and calculating a speed change completion degree (Shift) of the transmission by using a ratio between the (Nt−Ne) and the (g×No−Ne).
According to a third aspect of the present invention, there is provided a speed change control device of an automatic transmission which is driven by an engine through a torque converter, the transmission including a plurality of friction elements which are selectively engaged to provide a selected gear thereby to transmit the power of the engine to an output shaft of the transmission while changing the rotation speed. The control device comprises a first section that derives a difference (Nt−Ne) between an input rotation speed (Nt) of the transmission and an engine rotation speed (Ne); a second section that derives a difference (g×No−Ne) between the input rotation speed (g×No) of the transmission provided after completion of the speed change operation and the engine rotation speed (Ne); a third section that calculates a speed change completion degree (Shift) of the transmission by using a ratio between the (Nt−Ne) and the (g×No−Ne); a fourth section that, upon shifting of a shift lever of the transmission from a non-drive range to a drive range, estimates a time when an actual engaging operation of selected one of the friction elements starts, with reference to the speed change completion degree (Shift); and a fifth section that, before the time, controls a hydraulic pressure of the selected friction element to carry out the engaging operation thereof in a first given manner and after the time, controls the hydraulic pressure to carry out the engaging operation thereof in a second given manner.
According to a fourth embodiment of the present invention, there is provided a method for controlling an automatic transmission which is driven by an engine through a torque converter, the transmission including a plurality of friction elements which are selectively engaged to provide a selected gear thereby to transmit the power of the engine to an output shaft of the transmission while changing the rotation speed. The method comprises deriving a difference (Nt−Ne) between an input rotation speed (Nt) of the transmission and an engine rotation speed (Ne); deriving a difference (g×No−Ne) between the input rotation speed (g×No) of the transmission provided after completion of the speed change operation and the engine rotation speed (Ne); calculating a speed change completion degree (Shift) of the transmission by using a ratio between the (Nt−Ne) and the (g×No−Ne); estimating, upon shifting of a shift lever of the transmission from a non-drive range to a drive range, a time when an actual engaging operation of selected one of the friction elements starts, with reference to the speed change completion degree (Shift); and controlling, before the time, a hydraulic pressure of the selected friction element to carry out the engaging operation thereof in a first given manner and controlling, after the time, the hydraulic pressure to carry out the engaging operation in a second given manner.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and advantages of the present invention will become apparent from the following description when taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic block diagram of an automotive automatic transmission to which the present invention is practically applied;
FIG. 2 is table showing ON/OFF relation between selected gears and friction elements of the automatic transmission;
FIG. 3 is a flowchart, showing operation steps programmed for detecting or estimating completion of piston stroke of a selected friction element in case of shifting shift from N-range to D-range;
FIG. 4 is a time chart showing time series variations of various factors and a speed change completion degree “Shift” in a case wherein, with an associated motor vehicle being at a standstill, the shift lever is moved from N-range to D-range;
FIG. 5 is a time chart similar to FIG. 4, but showing a case wherein the motor vehicle is running;
FIG. 6 is a time chart showing time series variations of various motions that are provided when a select speed change control of the invention is effected;
FIG. 7 is a time chart showing time series variations of various factors, that are provided by a known estimating system when, under running of a motor vehicle, the shift lever is moved from N-range to D-range;
FIG. 8 is a time chart similar to FIG. 7, but showing a different condition;
FIG. 9 is a flowchart showing operation steps programmed in the known estimating system for detecting completion of a piston stroke of a selected friction element; and
FIG. 10 is a flowchart showing operation steps programmed in the known estimating system for detecting whether a turbine speed is increasing or lowering.
DETAILED DESCRIPTION OF THE INVENTION
In the following, the present invention will be described in detail with reference to the accompanying drawings.
Referring to FIG. 1, there is schematically shown an automatic transmission to which the present invention is practically applied. As will become clear as the description proceeds, in accordance with the present invention, there are provided a speed change completion degree estimating system and a speed change control device that practically uses the estimating system.
In FIG. 1, denoted by numeral 1 is an engine, such as an internal combustion engine or the like, and denoted by numeral 2 is an automatic transmission.
In accordance with a depression degree of an accelerator pedal (not shown) actuated by a driver, the output of the engine 1 is controlled. More specifically, in response to the movement of the accelerator pedal, a throttle valve (not shown) of the engine pivots between a full-closed position and a full-open position to control the engine output.
The output of the engine 1 is transmitted to the automatic transmission 2 through a torque converter 3 , as shown.
The automatic transmission 2 generally comprises input and output shafts 4 and 5 which are aligned and front and rear planetary gear units 6 and 7 which are coaxially disposed on and about the input and output shafts 4 and 5 .
The front planetary gear unit 6 comprises a front sun gear S F , a front ring gear R F , front pinions P F operatively disposed between the front sun gear S F and the front ring gear R F , and a front carrier C F rotatably holding the front pinions P F .
The ring planetary gear unit 7 comprises a rear sun gear S R , a rear ring Gear R R , rear pinions P R operatively disposed between the rear sun gear S R and the rear ring gear R R , and a rear carrier C R rotatably holding the rear pinions P R .
For deciding a transmission path (viz., selected gear) of the planetary gear units 6 and 7 , there are employed several friction elements which are a low clutch L/C, a second/fourth speed brake 2-4/B, a high clutch H/C, a low reverse brake LR/B, a low one-way clutch L/OWC and a reverse clutch R/C. These friction elements are associated with one another in the following manner.
That is, the front sun gear S F is engaged with the input shaft 4 when the reverse clutch R/C assumes an engage position, and is fixed to a case of the transmission when the second/fourth speed brake 2-4/B assumes an engage position.
The front carrier C F is engaged with the input shaft 4 when the high clutch H/C assumes an engage position.
Due to function of the low one-way clutch L/OWC, the front carrier C F can be suppressed from rotation in a direction reverse to that of the engine 1 . Furthermore, due to function of the low reverse brake LR/B, the front carrier C F is fixable to the transmission case.
The front carrier C F and the rear ring gear R R are selectively engageable with each other by the low clutch L/C.
The front ring gear R F and the rear carrier C R are constantly engaged and these friction elements R F and C R are fixed to the output shaft 5 to rotate therewith.
As is seen from Table-1 of FIG. 2, various gear positions (viz., first, second, third and fourth gears and reverse gear) of the transmission are obtained by selectively operating the friction elements R/C, H/C, L/C, LR/B, L/OWC and 2-4/B. In the table, engage condition is indicated by a solid line circle. In case of the low one-way clutch L/OWC, the solid line circle indicates a self-engagement condition. The engage condition of the low reverse brake LR/B assumed when engaging braking is needed is indicated by a dotted line circle.
For controlling the friction elements L/C, 2-4/B, H/C, LR/B and R/C, there is employed a control valve unit 8 (see FIG. 1 ). This control valve unit 8 is incorporated with a manual valve (not shown), a line pressure solenoid 9 , a low clutch solenoid 10 , a second/fourth speed brake solenoid 11 , a high clutch solenoid 12 and a low reverse brake solenoid 13 .
Due to ON/OFF operation of the line pressure solenoid 9 , the line pressure is controlled in magnitude. In accordance with movement of a shift lever actuated by a driver, the manual valve (not shown) is moved to a forward drive range (D), a reverse range (R) or a parking/neutral range (P, N).
When the manual valve is in the forward drive range (D), duty control is made to the low clutch solenoid 10 , the second/fourth speed brake 2-4/B, the high clutch H/C and the low reverse brake LR/B to control the hydraulic pressures fed to the corresponding friction elements L/C, 2-4/B, H/C and LR/B respectively, by feeding the line pressure to selected hydraulic circuits. With this, the first, second, third and fourth gears “1st”, “2nd”, “3rd” and “4th” as shown in Table-2 (see FIG. 2) are selectively obtained.
When the manual valve is in the reverse range (R), the line pressure is directly fed to the reverse clutch R/C to engage the same, and at the same time, due to the duty control applied to the low reverse brake solenoid 13 , the hydraulic pressure led to the low reverse brake LR/B is subjected to a time series control to engage the same. With this, the reverse gear “Rev” as shown in Table-2 (see FIG. 2) is obtained.
When the manual valve in the parking/neutral range (P, N), the line pressure is not fed to any of the hydraulic circuits, so that all of the friction elements are kept disengaged. With this, the transmission assumes a neutral condition.
Referring back to FIG. 1, the ON/OFF control of the line pressure solenoid 9 and duty control of the low clutch solenoid 10 , the second/fourth speed brake solenoid 11 , the high clutch solenoid 12 and the low reverse brake solenoid 13 are carried out by a transmission controller 14 . The transmission controller 14 has therein a microprocessor which comprises a CPU (central processing unit), a RAM (random access memory), a ROM (read only memory) and input and output interfaces.
For such control, various information signals are led to the transmission controller 14 , which are a signal (viz., signal representing an open degree “TVO” of a throttle valve) from a throttle valve open degree sensor 15 , a signal (viz., signal representing a turbine speed “Nt” of a torque converter 3 ) from a turbine speed sensor 16 , a signal (viz., signal representing a rotation speed “No” of a transmission output shaft 5 ) from an output shaft speed sensor 17 , a signal (viz., signal representing a selected range) from an inhibitor switch 18 and a signal (viz., signal representing engine speed “Ne”) from an engine speed sensor 19 .
In the following, an automatic transmission operation in case of D-range will be described.
Following a control program and based on the throttle open degree signal “TVO” and the transmission output shaft speed signal “No” with respect to a predetermined gear change map, programmed operation steps are carried out in the transmission controller 14 to derive a target gear (first, second, third or fourth gear) needed in an existing condition of an associated motor vehicle.
Then, in the controller 14 , a judgement is carried out as to whether the existing gear agrees with the derived appropriate gear or not. If NO, that is, when the existing gear does not agree with the target gear, a speed change command is issued for matching the existing gear with the target gear. That is, based on the information given by Table-2 (see FIG. 2 ), the solenoids 10 to 13 are subjected to a duty control respectively thereby to allow the friction elements to carry out their engage/disengage operations. With this, the first, second, third or fourth gear is actually and automatically established.
In the following, with aid of the flowchart of FIG. 3, a speed change completion degree estimating process according to the present invention will be described with respect to a gear change from N-range to D-range, that is, with respect to a case wherein the low clutch L/C starts its actual engaging operation following completion of a piston stroke.
At step S 21 , the following calculation is carried out to derive a speed change completion degree “Shift”:
Shift=( Nt−Ne )/( g×No−Ne ) (2)
wherein:
Nt: turbine rotation speed,
Ne: engine rotation speed,
No: transmission output shaft speed,
g: gear ratio upon completion of gear change.
In the following, the basis for using the “Shift” as the speed change completion degree will be described with reference to the time charts of FIGS. 4 and 5.
In FIG. 4, there are shown two time series variations, one (viz., upper one) showing the actual rotation speeds “Ne”, “Nt” and “No” with respect to elapsed time, and the other (viz., lower one) showing the “Shift” with respect to the elapsed time. That is, at the time when the transmission output shaft speed “No” is 0 (zero), the shift lever of a vehicle under standstill is moved from N-range to D-range. At a time “t 1 ”, a friction element (viz., low clutch L/C) completes its piston stroke, and at a time “t 2 ”, the friction element (viz., low clutch L/C) completes the speed change, that is, the drive and driven parts of the low clutch show a relative rotation of 0 (zero).
In FIG. 5, there are shown two time series variations similar to those of FIG. 4, but showing a case wherein the vehicle is under running (viz., transmission output shaft speed>0) at the third speed of the transmission. That is, at the time when the transmission output shaft speed is higher than 0 (zero), the shift lever of the vehicle under running at the third gear is moved from N-range to D-range. At a time “t 1 ” after completion of the engaging operation of the high clutch H/C, the friction element (viz., low clutch L/C) completes the piston stoke, and at a time “t 2 ”, the friction element (viz., low clutch L/C) completes the speed change, that is, the drive and driven parts of the low clutch show a relative rotation of 0 (zero). As shown, in this case, the turbine speed “Nt” becomes equal to the input shaft speed of the transmission that is established when the speed change is completed. It is to be noted that since the gear ratio (g 3 ) is 1:1 in the third gear, the input shaft speed established when the speed change is completed is equal to the output shaft speed.
For ease of description, such input shaft speed will be referred to “speed change completed input speed” in the following.
It is to be noted that the alternate long and short dash line in FIG. 5 shows an operation condition at the time when the shift lever is moved from N-range to D-range under running at the fourth gear. That is, after such movement of the shift lever, the second/fourth brake 2-4/B is engaged, and thereafter, the turbine speed “Nt” is gradually converged to the “speed change completed input speed” (g 4 ·No) as the engaging operation of the high clutch H/C advances. It is to be noted that the “speed change completed input speed” (g 4 ·No) in this case is represented by multiplication of the gear ratio (g 4 ) and the output shaft speed “No” of the transmission.
As is seen from both the time charts of FIGS. 4 and 5, at the time “t 1 ” when the friction element (viz., low clutch L/C, however, high clutch H/C in case of the fourth gear) starts its actual engaging operation following completion of the piston stroke, the speed change completion degree “Shift” starts its rising. Accordingly, the starting of rising of the degree “Shift” can be regarded as a sign of the start of the actual engaging operation of the friction element (viz., low clutch L/C, however, high clutch H/C in case of the fourth gear) that would take place after completion of the piston stroke.
Furthermore, as is seen from FIGS. 4 and 5, with advancement of the speed change operation, the speed change completion degree “Shift” increases. Accordingly, from a quantitative point of view, it can be estimated that the progress rate of the speed change operation increases with increase of the degree “Shift”.
As is seen from the equation of (2), when the turbine speed “Nt” is equal to the engine speed “Ne”, the degree “Shift” shows 0 (zero), and when the turbine speed “nt” is converged to the “speed change completed input speed” (g·No), the degree “Shift” shows 1 (one, or 100%).
Although the above description is directed to the select speed change from N-range to D-range, the speed change completion degree “Shift” is applicable to other speed change. That is, the starting of rising of the degree “Shift” is regarded as a sign of the start of the actual engaging operation of a friction element following the piston stroke, and it is estimated that the progress rate of the speed change operation increases with increase of the degree “Shift”.
Referring back to the flowchart of FIG. 3, at step S 22 , judgment is carried out as to whether the speed change completion degree “Shift” starts its rising or not. If YES, that is, when the degree “Shift” shows the sign, the operation flow goes to step S 23 to estimate that the friction element (viz., low clutch L/C, however, high clutch H/C in case of the fourth gear) has started the actual engaging operation following the piston stroke. However, if NO at step S 22 , that is, when the degree “Shift” does not show the sign, the operation flow goes to END.
As will be understood from the above description, the judgement for starting the actual engaging operation following piston stoke according to the present invention is quite simple and thus practical as compared with that used in the measures of FIGS. 9 and 10.
In the following, with aid of the time chart of FIG. 6, an actual speed change control will be described with respect to a case wherein, with a motor vehicle being standstill, the shift lever is moved from N-range to D-range.
As is seen from the time chart, within a period “ΔT 1 ” from a time “t 1 ” to a time “t 2 ”, the command value “Po” of the hydraulic pressure led to the friction element (viz., low clutch L/C) is increased sharply for the purpose of completing the piston stroke of the friction element as soon as possible. As shown, a high pre-charge pressure is kept in the period “ΔT 1 ” for that purpose.
However, at the time “t 2 ”, the command value “Po” is sharply lowered to a certain value. That is, if completion of the piston stroke is carried out with such high pre-charge pressure, undesired shock is produced by the friction element (viz., low clutch L/C). As shown, from the time “t 2 ”, the command value “Po” is gradually increased at a given increasing rate that suppresses the shock.
As shown, the speed change completion degree “Shift” shows the starting of rising at a time “t 3 ”. That is, it is estimated that at the time “t 3 ”, the friction element (viz., low clutch L/C) has finished the piston stroke and started the actual engaging operation thereof. Upon detecting the sign of the time “t 3 ”, the following engagement capacity control is carried out.
As is seen from the time chart, upon detecting the sign “t 3 ”, the output torque of the transmission is gradually increased at an increasing rate that suppresses a select shock. However, for obtaining a speed change advancing speed that increases at a rate that brings about a notable deterioration of the select response, the command value “Po” of the hydraulic pressure is increased at a given increasing rate from the time “t 3 ”.
The rising of the command value “Po” is continued until a time “t 4 ” when the speed change completion degree “Shift” shows a value that is somewhat smaller than 100%, that is, until a time just before completion of the speed change operation. From the time “t 4 ” to a time “t 5 ” for which a period “ΔT 2 ” is defined, the increasing rate of the command value “Po” is reduced to almost 0 (zero) causing the output torque of the transmission to show a smoothed curve having no peak torque as shown. With this, undesired shift shock, which would occur upon completion of the speed change operation, is suppressed.
From the time “t 5 ” to a time “t 6 ” for which a period “ΔT 3 ” is defined, the command value “Po” of the hydraulic pressure is rapidly increased to the highest level, that is, to the line pressure to finish the speed change operation.
In the above-mentioned speed change control, by using the operation steps shown in the flowchart of FIG. 3, estimation is made on the time “t 3 ” (see FIG. 6) when, upon shifting from N-range to D-range, the friction element (viz., low clutch L/C) starts its actual engaging operation, and until the estimated time “t 3 ”, the command value “Po” of the hydraulic pressure led to the friction element is so controlled as to carry out the piston stroke in a given manner, and after the time “t 3 ”, the command value “Po” is so controlled as to carry out the speed change operation in another given manner. Thus, before and after the estimated time “t 3 ”, the command value “Po” of the hydraulic pressure for the friction element is differently but appropriately controlled in a desired manner.
Furthermore, as is seen from the description directed to the time charts of FIGS. 4 and 5, the estimation of the time when the friction element starts its actual engaging operation following the piston stoke is available not only in the case wherein the vehicle is standstill but also in the case wherein the vehicle is running. Accordingly, the above-mentioned advantageous speed change operation is obtained upon shifting from N-range to D-range under running of the vehicle.
Referring back to the time chart of FIG. 6, denoted by the alternate long and short dash line is a line for showing the speed change completion degree “Shift” that is effected when the shift lever is moved from N-range to R-range.
As is seen from the table of FIG. 2, upon selection of R-range from N-range, the reverse clutch R/C and the low reverse brake LR/B are brought to their engage condition to cause the transmission to assume Reverse gear. As has been described hereinabove, when the manual valve is shifted to R-range, the reverse clutch R/C is engaged by the coming line pressure and the low reverse brake LR/B is engaged by the duty control applied to the low reverse brake solenoid 13 . Thus, the reverse clutch R/C is engaged first and then the low reverse brake LR/B is engaged, and upon starting of the actual engaging operation of the low reverse brake LR/B, the speed change completion degree “Shift” starts its rising at the time “t 3 ” (see FIG. 6 ).
Accordingly, also in case of the shifting from N-range to R-range wherein the reverse clutch R/C and the low reverse brake LR/B are both engaged, the starting of rising of the degree “Shift” can be regarded as the sign of the starting of the actual engaging operation of the friction element (viz., low reverse brake LR/B) that would take place after completion of the piston stroke.
In the time chart of FIG. 6, denoted by the dashed line is a line for showing the speed change completion degree “Shift” that is effected when, like in garaging, the shift lever is moved from R-range to D-range and then to R-range repeating forward and reverse movement of the vehicle.
In this case, the transmission is forced to assume the reverse gear or forward first gear, and thus, the speed change completion degree “Shift” indicates 100%. Thus, upon release of the engaged condition of one friction element, the degree “Shift” lowers and, at the time “t 3 ” when another friction element starts its actual engaging operation following completion of the piston stroke, the degree “Shift” starts to rise. Thus, also in this case, the starting of rising of the degree “Shift” can be regarded as the side for estimating the completion of the piston stroke of the latter friction element.
In the above-mentioned embodiment, the description is directed to transmissions of a type wherein hydraulic pressures for the friction elements are directly controlled by respective solenoids and wherein a so-called select speed change is carried out. However, the present invention is not limited to such type. That is, the present invention is applicable to other types of transmissions under the substantially same concept of the invention.
The entire contents of Japanese Patent Application 2000-282337 (filed Sep. 18, 2000) are incorporated herein by reference.
Although the invention has been described above with reference to the embodiment of the invention, the invention is not limited to such embodiment as described above. Various modifications and variations of such embodiment may be carried out by those skilled in the art, in light of the above description. | An automatic transmission is driven by an engine through a torque converter. The transmission includes a plurality of friction elements which are selectively engaged to provide a selected gear thereby to transmit the power of engine to an output shaft of the transmission while changing the rotation speed. A speed change completion degree estimating system is provided, which comprises a first section that derives a difference (Nt−Ne) between an input rotation speed (Nt) of the transmission and an engine rotation speed (Ne); a second section that derives a difference (g×No−Ne) between the input rotation speed (g×No) of the transmission provided after completion of the speed change operation and the engine rotation speed (Ne); and a third section that calculates a speed change completion degree (Shift) of the transmission by using a ratio between the (Nt−Ne) and the (g×No−Ne). | 8 |
This is a division of application Ser. No. 09/280,448, filed Mar. 30, 1999, now U.S. Pat. No. 6,579,862 which is incorporated herein by reference.
FIELD OF THE INVENTION
This invention relates to the novel use of D-ring unsaturated pregnadienols/pregnadienones represented by general formula (I) as shown in the accompanying drawings, possessing both pronounced hypolipidemic and hypoglycemic activities and devoid of androgenic and progestational activities. More particularly this invention relates to the novel use of 3β-hydroxy-pregna-5,16-dienone an important prototype of this class, represented by the formula (II) as shown in the accompanying drawings, for the treatment of diabetes and pronounced hypolipidemic and hypoglycemic activities.
BACKGROUND
High plasma cholesterol and related lipids are known to be one of the factors that predispose an individual to atherosclerosis and thus to myocardial infarction. Diabetes mellitus, which eventually impairs the function of kidneys, eyes, nervous and vascular systems, is quite often associated with lipid disorders. Both hyperlipidemia and diabetes mellitus require long term management and pose problems in choice of pharmacotherapeutic interventions when these conditions manifest together. Though a number of drugs are known separately to treat these conditions, there are a number of side effects associated with them which limit their long term use.
The most important hypolipidemic drugs available today belong to the statin and fibrate classes [McCarthy, P. A., Med. Res. Rev., 13, 139-59 (1993)] whereas hypoglycemic drugs fall into the category of sulphonylureas, biguanidines and amidines [Wolff, M. E. (Ed), Burger's Medicinal Chemistry Part II, 1045 (1981), John Wiley & Sons, New York]. However, these therapeutic agents are not free of side effects-statins (HMG-CoA reductase inhibitors) the most widely used drugs today which hitherto were thought to be very safe drugs, have exhibited side effects following long term therapy [Carrier, M. et al.; Ann. Thorac. Surg., 57, 353-6 (1994)]. The adverse effects which have become the source of concern, are increases in hepatic transaminases and myopathies [Witztum, J. L., In Goodman & Gilman's The Pharmacological Basis of Therapeutics, eds. Hardman, J. et al. 9 th edition, McGraw Hill, New York pp. 875-98, Fukami, M. et al; Res. Exp. Med., 193, 263-73 (1993); Appelkvist, E. et al.; Clin. Invest., 71 (suppl 8), 597-102 (1993), Wills, R. A. et al.; Proc. Natl. Acad. Sci. (US), 87, 8928-30 (1990)] and carcinogenesis, especially breast cancer in subjects undergoing treatment with pravastatin [Braunwald, E.; Scrip, 2117, 33 (1996)); Ciaravino, V. et al.; Mutat. Res.; 353, 95-107 (1995)]. The incidence of myopathy associated with rhabdomyolysis and renal failure is increased subsequent to such treatment [East, C. et al.; N. Engl. J. Med., 318, 47-48 (1998); Pierce L. R. et al.; J. Am.Med. Assoc., 265, 71-75 (1990)]. Also, these HMG-CoA inhibitors block mevalonate production which occurs at an early stage in cholesterol synthetic pathway. Mevalonate is a common precursor for all isoprenoids such as ubiquinones (Co-enzyme Q-10), the dolichols, isopentenyl t-RNA etc. Therefore, long term blockade of mevalonate synthesis leads to Q-10 deficiency. Serum Co-enzyme Q-10 is important for cardiac function [Laaksonen, R. et al., Eur. J. Clin. Pharmacol. 46,313-7 (1994); Bargossi, A. M. et al; Int.J. Clin. Lab. Res., 24, 171-6 (1994)]. The most common side-effects of fibrates and particularly clofibrate therapy are gastrointestinal upsets including nausea, vomiting, diarrhoea, dyspepsia, flatulence and abdominal discomfort [Oliver, M. F. et al.; Br. Heart J., 40,1069-1118 (1978)]. Elevated creatine phosphokinase concentration during clofibrate therapy may be associated with a syndrome of muscle pain and weakness. Large-scale long-term studies have demonstrated an increased incidence of cholecystitis, gallstones and sometimes pancreatitis in patients receiving clofibrate and some studies have indicated cardiovascular disorders [The coronary Drug Project Research Group; N. Engl. J. Med., 296, 1185-90 (1977)]. The unexpected finding of an increased mortality rate in patients taking clofibrate in the WHO study produced serious concern over the long-term safety of clofibrate and ultimately led to its withdrawal in many countries [Oliver, M. F. et al.; Lancet, ii, 600-604 (1984)].
The adverse effects of biguanidine antidiabetic agents include gastro-intestinal disturbances like diarrhoea and lactic acidosis [Paterson, K. R. et al.; Adverse Drug React Acute Poisoning Rev., 3, 173-82 (1984)]. With sulphonylureas the commonly associated adverse effects are hypoglycemia, gastrointestinal disturbances, hypersensitivity and vascular complications [Paice, B. J. et al., Adverse Drug React. Acute Poisoning, 4, 23-26 (1985)]. As diabetes and hyperlipidemia are quite commonly manifesting together, it would be of great clinical benefit if the same compound could have both these activities together because the available drugs are not free of toxic effects and neither data regarding toxic manifestations are available when drugs for two clinical conditions are mixed together.
Two approaches currently being pursued in search of drugs with hypolipidemic and hypoglycemic activities together. The first approach emerged during detailed study of antihypertensive action of adrenergic receptor modulators. The study revealed that a,-adrenergic blockers (particularly Doxazosin and Prazosin) [Lithell, H. O.; J. Hypertens, 15 (Suppl 1), S 39-42 (1997); Poliare, T. et al.; Diabetologia, 31, 415-420 (1988); Anderson, P. E. et al.; Am. J. Hypertens, 9, 323-333 (1996)] and β 3 -adrenergic agonist (BTA-243, BRL-37344, CGP 12177, CL 316243 [Arch, J. R. S. et al.; Med. Res. Rev., 13, 663-729 (1993); Largis, E. E. et al.; Drug Dev. Res., 32, 69-76 (1994)] also affect plasma lipoprotein metabolism and increase insulin sensitivity. As a result such antihypertensive drugs exhibit lipid lowering and hypoglycemic actions together. α 1 -adrenergic receptor blockers, however have the inherent limitations of causing orthostatic hypotension and syncope [Matyus, P.; Med. Res. Rev., 17(6), 523-35 (1977)]. The essential requirement of β 3 -agonist for antiobesity and antidiabetic actions is the need for high selectivity for β 3 -adrenoceptor. Any substantial β 1 - or β 2 -agonism would likely cause increased heart rate and muscle tremor respectively which are unacceptable in a drug which could be administered on long term basis [Connacher, A. A. et al.; Brit. Med. J., 296,1217-20 (1988); Mitchell, T. H. et al; Int. J. Obesity., 13(6), 757-66 (1989)]. The second line of approach for dual activity came into light during the study of anti-oxidant property of drugs. There have been many reports describing relationships between peroxidation and diseases such as diabetes mellitus, atherosclerosis and myocardial ischemia in terms of radical oxidation. Troglitazone, an antioxidant drug has been developed as an oral hypoglycemic agent which enhances the action of insulin in peripheral tissues and liver besides its hypolipidemic effects. However, troglitazone is also not free of major side effect causing liver damage. The drug, troglitazone, has been implicated in 35 cases of liver disease leading to one transplant and one death [Warner-Lambert; Chem. & Ind., No. 22, 897 (1977)]. Thus to the best of our knowledge no class of compound is yet available which has both effects together as the main action and have a fair safety margin.
We, in early eighties started our work for search of such compounds which have effect on endogenous transportation of lipids and glucose rather than interfering with exogenous transportation. Our research was mainly based on secondary metabolic actions of progesterone.
Progesterone, apart from its classical hormonal action on the reproductive system, is known to modulate lipid, carbohydrate, insulin and protein metabolism. The rise in the level of progesterone in the first trimester of pregnancy causes hyperphagia, pancreatic islet hypertrophy, hyperinsulinemia and body fat and glycogen deposition, when the metabolic demands of the fetus are very low. However, in the latter half of pregnancy, although the progesterone levels are still high, the carbohydrate, lipid and protein reservoirs shift into circulation to meet the needs of the growing fetus. [Kalkhoff, R. K.; Am. J. Obstet. Gynecol., 142, 735-38 (1982)].
Progesterone thus, having actions both on the reproductive and metabolic systems, seemed to offer the possibility of dissociating these two biological activities by structural modifications. The experience of the development of second generation progestins supported this contention. The first generation progestins such as levonorgestrel exhibited undesirable pharmacologic effects like alteration in carbohydrate and lipoprotein metabolism, weight gain and hypertension, which was shown to be related to their intrinsic androgenic/anabolic activity and ability to bind with androgen receptors. The androgenic affinity has been attributed to C-17 hydroxy functionality which makes these molecules resemble androgens. In recently discovered second generation progestins such as gestodene and 3-keto-desogestrel, an additional olefinic bond either in C- or D-ring brought a dramatic decrease in their affinity to androgen receptors (Table 1). As a result these compounds have a very high order of progestational effect with practically no androgenic activity and did not cause hyperlipidemia [London, R. S.; Obstetrical & Gynocological Survey, 47, 777-81 (1992)].
TABLE 1
Relative Binding Affinity of Contraceptive Progestins
for Progesterone and Androgen receptors
Progestin
Androgen
Receptor
Receptor
Selectivity
Binding
Binding
Index*
Affinity
Affinity
(A/P ratio)
Progesterone
1.00
0.005
93
Levonorgestrel
5.41
0.220
11
3-Keto-desogestrel
8.6
0.120
33
Gestodene
9.21
0.154
28
*The higher the selectivity index, the greater the separation between the dose needed to achieve the desired progestational effect and the dose associated with the undesired androgenic effect [Collins, D. C.; Am. J. Obstet. Gynecol. 170, 1508-13(1994)].
OBJECTS OF THE INVENTION
It is an object of the invention to explore the possibility of designing pregnadienones which while preserving the ability to modulate lipid and carbohydrate metabolism would not have any progestational effect. It would be pertinent to point out that earlier, the applicants had isolated a D-ring modified pregnenolone, named Gugulsterone represented by formula (9) as shown in Table 2, from guggul resin obtained from Commiphora mukul , which had potent hypolipidemic effect without any progestational effect [Arya, V. P.; Drugs Fut. 13, 618 (1998)].
It is another object of the invention to explore the possibility of dissociating the hypolipidemic and insulin sensitizing activities of progesterone from its hormonal actions. Accordingly, the applicants focused their attention to prepare and investigate analogues/prototypes with additional substituents in ring-D of pregnadienones.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
FIG. 1 (A) represents the structural formula of compounds belonging to the class of pregnadienones and pregnadienols and
FIG. 1 (B) represents the structural formula of 3β-hydroxypregna-5,16-dien-20-one.
FIGS. 2 (A)- 2 (F) represents the structural formulae of hormones.
SUMMARY OF THE INVENTION
In accordance with the above objectives, the applicant's present invention relates to a method of using D-ring unsaturated pregnadienones represented by structural formula (I) which causes significant fall of serum cholesterol, triglycerides, LDL-cholesterol and glucose with mild increase in HDL-cholesterol, said method comprising administration of effective amounts of said compounds of formula (I) to mammals. The compounds possess fair safety margin having antioxidant and cardio protection activities.
The invention also provides a method of treatment of hyperlipidemic and hyperglycemic conditions which comprises administration to a recipient a therapeutic composition comprising a pharmaceutically effective amount of compound D-ring unsaturated preganadienones represented by the general formula (I) as shown hereinbelow and in the accompanying drawings:
Wherein X═OH or O or combination thereof and positioning of olefinic bonds are at 4(5); 5(6); 16(17); 17(20) or various combinations
DETAILED DESCRIPTION OF THE INVENTION
The present invention concerns methods for lowering serum cholesterol, triglycerides and glucose levels in subjects with obesity and diabetic conditions or prophylactically holding in check the symptoms of such a disease state.
In particular, the applicants, during their study, have observed that the prenadienone, 3β-hydroxypregna-5,16-dien-20-one represented by the structural formula (II) shown hereinbelow and in the accompanying drawings is useful for the and hyperglycemic conditions.
Accordingly, the invention provides a method of using compounds represented by the structural formula (I) as shown in the accompanying drawings, containing at least one olefinic bond in or on their D-ring for the treatment of hyperlipidemic and hyperglycemic conditions in mammals, said method comprising administering an effective amount of the said compounds to recipient mammals.
In one embodiment, the compounds of formula (I) are administered in the form of tablets, capsules or injectibles.
In another embodiment, the compounds of formula (I) are characterized as pregnadienones and pregnadienols.
In yet another embodiment, the most preferred compound belonging to the family of preganienones and pregnadienols represented by formula (I) is 3β-hydroxy-pregna-5,16-dien-20-one, which is represented by the structural formula (II) as shown in the accompanying drawings.
In a further embodiment, the compounds of formula (I) are optionally administered to the recipient mammal as an admixture with conventional anti-platelet, anti-atherosclerotic, hypolipoproteinic and antidiabetic drugs.
In still another embodiment, the compounds of formula (I) are essentially free of side effects associated with conventional hypolipidemic and hypoglycemic drugs.
In an embodiment, the compounds of formula (I) exhibit cardioprotective, anti-diabetic, anti-atherosclerotic and anti-oxidant properties.
Further, the invention provides a method of treatment of hyperlipidemic and hyperglycemic conditions in mammals, which comprises administration to a recipient, a therapeutic composition comprising an effective amount of compound of formula (I) with conventional carriers.
In an embodiment, the recipient mammals are selected from the group comprising rats, human beings, rhesus monkeys and rabbits.
In another embodiment, the conventional carriers are selected from anti-platelet, anti-atherosclerotic, hypolipoproteinic and anti-diabetic drugs.
In yet another embodiment, the said compounds of formula (I) essentially contain an olefinic bond in or on their D-ring.
In a further embodiment, the compounds of formula (I) are essentially free of androgenic, progestinal and side effects.
In still another embodiment, the therapeutic composition is administered in the form of tablets, capsules and injectibles.
In another embodiment, the said preganadienones and preganadienols exhibit cardio protective, antidiabetic, antiatheroselerotic and antioxidant properties.
In yet another embodiment, the said preganadienones and pregnadienols of formula (I) essentially contain olefinic bond in one of the D-rings.
Method of Synthesis/production
The methods of synthesis are essentially known in the literature, can be obtained from diosgenin by chemical degradation [G. Rosenleranz “History of Steroids”, Steroids, 57, 409 (1992)]. Although, it was later isolated from Veratrum Grandiflorum [Kanko, K. et al; Phytochemistry, 12 1509 (1973)] but yield is too low to be of any practical value. Oppenauer oxidation of 2 with aluminium-isopropoxide and cyciohexanone in toluene produces 4,16-dienpregna-3,20-dione [16-dehydroprogesterone, (3)]. The C-16 (17) olefinic bond in (1) is selectively reduced with Pd-C in diethylether at very low hydrogen gas pressure. The resultant product 4 on basic hydrolysis furnishes 5. The procedure of Benn and Dodson [J. Org. Chem. 29, 1142 (1964)] was followed for the preparation of Gugulsterone (9). The reduction of 16-DPA (1) with lithium aluminium hydride produces diol 6 which after Sigmatropic rearrangement in presence of p-toluenesulphonic acid, acetic acid and acetic anhydride produces the diacetate 7. Basic hydrolysis of the diacetate 7 followed by Oppenauer oxidation furnishes an 80:20 mixture of E&Z-Gugulsterone (9).
5. BIOLOGICAL ACTIVITY
5.1 Hypolipidemic Activity
The primary hypolipidemic effect of these compounds was established in triton induced hyperlipidemia in Charles Foster rats. The compounds which exhibited significant lipid lowering effect in this model were then evaluated for their hypolipidemic effect in normal, and diet induced hyperlipidemic rats, rabbits and rhesus monkeys.
5.1.1 Hypolipidemic Activity in Triton Treated Rats
The cholesterol lowering effect of some representative compounds of pregrenadienols and pregrenadienones as compared to clofibrate and gugulsterone in triton treated Charles Foster rats is described in Table-2.
TABLE 2
Cholesterol lowering effect of pregnane compounds as compared to Clofibrate in
Triton treatcd rats
%
Compd.
Dose (i.p.)
Change
No.
Compound
Structure
mg/kg
S. Chol.
1
3β-Acetoxypregna- 5,16-dien-20-one (16-DPA)
50
−43
2
3β-Hydroxypregna-5,16- dien-20-one
50
−46
3
4,16-Dienpregna-3,20-dione
50
−13
4
3β-Aceoxypregna-5-en-20- one
100
−12
5
3β-Hydroxypregna-5-en-20-one
100
−09
6
5,16-Dien-pregnane-3,20-diol
50
−10
7
5,17(20)-Dienpregna-3,16- diol-diacetate
50
−33
8
5,17(20)-Dienpregna-3,16-diol
50
−31
9
Gugulsterone
50
−44
10
Clofibrate
200
−15
The results showed that of the compounds tested, the highest effect was exhibited by 16-DPA (1) and its 3-des-acetyl analog 2 comparable to gugulsterone (9), and that the removal of double bond in ring D of 1 or 2 almost abolished the effect.
5.1.2 Hypolipidemic Activity of 3β-Hydroxypregna-5,16-dien-20-one (2) in Normal Rats
In normal rats, 3β-hydroxypregna-5,16-dien-20one (2), at 50 mg/kg produced a significant lowering of serum cholesterol and triglycerides as describe in Table-3 below. The animals did not develop any tolerance to the compound even after administering for 30 days.
TABLE 3 Hypolipidemic activity of 3β-Hydroxypregna-5, 16-dien-20-one (2) in normal rats Serum Serum Cholesterol Triglycerides % Fall (mg %) (mg %) compared Treatment 0 Days 30 Days % Fall 30 Days to control 2 (50 mg/kg) 71.5 ± 1.8 43.2 ± 2.9 40 42.0 ± 2.8 35 (8) Clofibrate 82.3 ± 3.3 53.2 ± 2.0 36 47.3 ± 3.2 28 (50 mg/kg) (6) Normal 83.3 ± 3.1 80.1 ± 1.4 — 65.2 ± 2.9 — saline (control) (6) Mean values ± SD. FIG. in parenthesis represent number of animals.
5.1.3 Hypolipidemic Activity in Diet Induced Hyperlipidemic Rats
Twenty three normal male rats average weight 110-120 g were taken for study and were divided into four groups. Group l: animals received special diet and 3β-hydroxypregna-5,16-dien-20-one (2) 50 mg/kg p.o. in 1% gum acacia. Group II: animals received 3β-hydroxypregna-5,16-dien-20-one (2), 100 mg/kg p.o. in 1% gum acacia and special diet. Group III: animals received special fat diet and 1% gum acacia and served as control. Group IV: animals were fed with stock diet and served as normal control. All animals were sacrificed at the end of 36 days. Blood was drawn from the tail at 10 days and from the aorta at the time of sacrifice for estimation of serum cholesterol, triglycerides and HDL-cholesterol. LDL-cholesterol was calculated as described. [Roschlau, P. In: Methods of Enzymatic Analysis 4th ed., H. U. Bergmeyer, Ed (Academic Press, New York) 1975 p 1890; Wahlefield, W. A. In: Methods of Enzymatic Analysis, 4th ed.; H. U. Bergmeyer, Ed. (Academic Press, New York) 1974 p 1831.]
Results
Animals treated with 3β-yydroxypregna-5,16-dien-20-one (2), at 50 and 100 mg/kg showed a significant lowering in serum cholesterol by 31 and 59%, triglycerides by 55 and 62%, LDL-cholesterol by 27 and 74% respectively (Table -4 & 5).
TABLE 4
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) on serum cholesterol and
triglycerides in hyperlipidemic rats
Serum Cholesterol (mg %)
Serum Triglycerides
Days
(mg %)
Treatment
0
10
36
0
36
I
69.1 ± 9.9
212.4 ± 23.8
165 ± 26.7
48.8 ± 7.0
61.5 ± 10.5
2(50 mg/kg) + HFD
(7)
(7)
(7)
(6)
(6)
% Decrease
16
31
55
(Compound to
group III)
II
60.8 ± 10.3
145.5 ± 10.6
106.4 ± 4.6
50 ± 7.1
53.0 ± 7.5
2(100 mg/kg) + HFD
(6)
(6)
(5)
(5)
(5)
% Decrease
48
59
62
(Compound to
group III)
III
73.2 ± 5.8
325 ± 29.8
293.2 ± 16.6
48.75 ± 5.1
137.5 ± 8.5
HFD
(5)
(5)
(5)
(4)
(4)
IV Normal Diet
72 ± 7.1
48.2 ± 4.3
(5)
(5)
HFD = High fat diet, Values are Mean ± SD. FIGS. in parenthesis are number of animals
TABLE 5 Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) on HDL and LDL-cholesterol in hyperlipidemic rats HDL-Cholesterol LDL-Cholesterol (mg %) (mg %) Treatment Day 0 Day 36 Day 0 Day 36 I HFD 37.25 ± 5.0 39.75 ± 2.8 27.5 ± 6.3 189.25 ± 18.0 (4) (4) (4) II 2(50 mg/kg) + 34.8 ± 5.8 37.57 ± 2.8 24.5 ± 14.2 123.87 ± 14.0 HFD (7) (7) (7) (6) % Change 181 271 III 2(100 mg/kg) + 43.4 ± 8.3 47.2 ± 3.7 10.02 ± 8.5 48.64 ± 5.1 HFD (5) (5) (5) (5) % Change 161 741 HFD = High fat diet. Values are Mean ± SD. FIGS. in parenthesis are number of animals
5.1.4 Hypolipidemic Activity in Hyperlipidemic Rabbits
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) was studied on hypercholesterolemic albino rabbits. Twelve male albino rabbits (approx 1.5-2 kg) on a stock diet were made hyperlipidemic by feeding daily cholesterol 0.5 g/kg in 2 ml of groundnut oil for 45 days and then blood was drawn from the marginal vein in the ear of rabbits for serum cholesterol and triglycerides estimation.
Two controlled experiments were carried out for a period of three months. In one set of experiments, the control group received 0.5 g/kg of cholesterol for 90 days and 3β-Hydroxypregna-5,16-dien-20-one (2) in dose of 100 mg/kg and 50 mg/kg while in control group (given only cholesterol) a massive rise of serum cholesterol and triglycerides were seen after 90 days, the addition of 3β-Hydroxypregna-5,16dien-20-one (2) at 50 and 100 mg/kg doses kept the rise well under control. The percentage decrease at 100 mg dose was 28% at 30 days to 52% at 90 days for cholesterol and 45 to 81% for triglycerides. In the 50 mg/kg dose group the decrease percentage ranged from 40% at 30 days to 50% at 90 days for cholesterol and 45% at 30 days to 75% at 90 days for triglyceride (Table6)
TABLE 6
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) in
hyperlipidemic male albino rabbits
S. Cholesterol (mg %)
S.Triglycerides
Days
(mg %) Days
Treatment
30
60
90
30
60
90
Expt. 1.A
296.3
435.5
1337.5
69.0
150.0
161.0
Control + cholesterol(0.5 g/
kg)
Expt. 1.B
213.3
309.3
633.7
79.0
54.0
44.2
2(100 mg/kg) + cholesterol
(0.5 g/kg)
% Decrease
28
42
53
46
64
81
Expt. II.A Control +
317.8
531.8
1334.6
145.0
185.8
232.0
cholesterol(0.5 g/kg)
Expt. II.B 2 (50 mg/kg) +
190.5
305.5
660.3
79.5
67.0
56.5
cholesterol(0.5 g/kg)
% Decrease
40
43
51
45
64
76
TABLE 7 Hypolipidemic effect in hyperlipidemic rabbits (120 days experiment) Stock diet + HFD + Guglip + HFD + 2 Parameters Normal saline HFD 2(100 mg/kg) (100 mg/kg) Serum Cholesterol (mg/dl) 56.3 ± 3.1 1367.0 ± 203 258.6 ± 28.2 350.0 ± 28.1 % Decrease (Compared with 81 74 HFD) Serum Triglycerides 50.0 ± 2.1 188.0 ± 10.2 66.2 ± 4.1 74.2 ± 10.3 % Decrease (Compared with 65 61 HFD)
5.1.5 Hypolipidemic Activity in Rhesus Monkeys
In Rhesus monkeys: 3β-Hydroxypregna-5,16-dien-20one (2) was administered orally daily for 90 days in doses of 62.5, 125 or 650 mg/kg to different group of animals. Significant decrease in serum cholesterol was observed (45-52%). At 90 days, percentage decrease in triglycerides varied from 14 to 36%. Compound 2 caused a marked decrease in low density lipoprotein (75-90%) whereas changes in HDL-cholesterol were not significant (Table-8 & 9)
TABLE 8
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) in Rhesus monkeys
S. Cholesterol
S. Triglycerides
Days
Days
Treatment
0
90
% Fall
0
60
% Fall
Expt. I
119.8 ± 16.6
90.5 ± 9.0
26
82.0 ± 2.5
62.0 ± 1.0
24
Control + 1% gum acacia
Expt. II 2(62.5 mg/kg)
156.8 ± 23.0
83.3 ± 8.5
47
77.5 ± 7.0
66.3 ± 6.9
14
Expt. III 2(125 mg/kg)
133.3 ± 8.5
65.8 ± 2.2
50
69.8 ± 9.9
60.0 ± 2.9
13
Expt. IV 2(650 mg/kg)
132.8 ± 6.4
63.3 ± 2.3
53
90.5 ± 3.9
58.5 ± 3.8
36
Mean ± SD values mg/dl. Each set of experiment involved 4 monkeys
TABLE 9
Effect of β-Hydroxypregna-5,16-dien-20-one (2) on HDL-and LDL-cholesterol
in Rhesus monkeys
HDL-Cholesterol
Days
LDL-Cholesterol
Treatment
0
90
% Change
0
90
% Fall
Expt. 1 Control + 1% gum
45.5 ± 7.4
43.0 ± 0.5
−6
57.9 ± 16.2
35.0 ± 8.8
39
acacia
Expt. II 2(62.5 mg/kg)
50.0 ± 4.5
45.0 ± 2.5
−8
91.8 ± 27.0
24.3 ± 8.0
75
Expt. III 2(125 mg/kg)
46.3 ± 2.0
50.8 ± 0.5
+10
63.5 ± 7.4
4.6 ± 0.9
90
Expt. IV 2(650 mg/kg)
39.3 ± 1.3
41.8 ± 0.9
+6
72.7 ± 8.4
13.1 ± 0.7
82
Mean ± SD values mg/dl. Each set of experiment involved 4 monkeys.
5.2 Hypoglycemic Activity
The compounds were tested for their hypoglycemic effects in normal, glucose loaded and streptozotocin induced diabetic rats. The experimental details of the testing of one such compound 3β-hydroxypregna-5,16-dien-20-one (2) is described below which possessed marked hypoglycemic effect in two models. (Tables 10 and 11).
5.2.1 Hypoglycemic Activity in Glucose Loaded Rats
The experiments were carried out with albino rats (Charles Foster strain) of either sex weighing 150-160 g. They were fed on laboratory diet prepared by M/s Lipton India Ltd. and maintained under 12 hr. light/dark cycle at 25±2° C.
The animals were divided into eight groups, each of six rats; group I was given 1% gum acacia (0.1 ml/100 g body weight) intragastrically (p.o.) and the group II were given 3β-hydroxypregna-5,16-dien-20-one (2) in 1% gum acacia. Animals of group III were given the standard antidiabetic drug, tolbutamide in the similar fashion. 2.0 g/kg glucose was given p.o. to all the rats along with the vehicle/Compound/Standard antidiabetic drug. Blood samples were taken from retroorbital plexus at periodic intervals. Glucose levels in the blood samples were measured by glucose oxidase method [Bergmeyer and Benut, 1963 cited in “Methods of Enzymatic Analysis” ed. H. Bergmeyer, Verlag Chemie, GmBH, Weinheim, Beroster, pp123, Academic press, New York].
TABLE 10 Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) and standard antidiabetic drug on post-prandial blood glucose level after challenge with glucose Maximum Blood Blood Glucose Level Glucose (mg/dl) Change Group 0 min 30 min 60 min 90 min 120 min (%) Control 40.35 ± 2.9 102.3 ± 6.11 68.91 ± 1.95 66.48 ± 2.12 50.61 ± 1.27 Compund 2 (100 mg/kg) + Glucose 42.43 ± 1.64 76.15 ± 6.07 56.06 ± 4.65 55.06 ± 2.61 49.59 ± 1.66 −18.7 (48) (55) (54) (34) Tolbutamide (100 mg/kg) + Glucose 38.15 ± 2.02 76.31 ± 6.29 27.26 ± 3.1 24.64 ± 1.92 23.07 ± 3.11 −41.7 (35) (100) (100) (100) FIG. in parenthesis indicates % inhibition compared to control Mean ± SD values mg/dl. Each set of experiment involved 6 rats.
5.2.2 Hypoglycemic Activity in Streptozotocin Induced Hyperglycemic Rats
Hyperglycemia in rats was produced by streptozotocin treatment. The animals showing blood glucose levels between 250-350 mg/dl were selected. Blood samples were collected after treatment at intervals and blood glucose levels were estimated immediately. The results showed lowering in blood glucose level within 1 hr and the maximum fall was observed at 12 hrs.
TABLE 11
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) and Tolbutamide on
blood glucose level of streptozotocin
induced diabetic rats.
Blood glucose level mg/dl
Treatment
0 hr
1 hr
2 hr
3 hr
4 hr
5 hr
I Streptozotocin
301 ± 7
314 ± 11
318 ± 12
328 ± 10
328 ± 15
333 ± 21
(50 mg/kg i.p.)
II Streptozotocin
274 ± 9
243* ± 10
231* ± 14
203** ± 20
183*** ± 14
157*** ± 21
(50 mg/kg p.o) +2
(11.3)
(15.6)
(25.9)
(33.2)
(42.7)
(100 mg/kg p.o.)
IV Streptozotocin
292 ± 10
218** ± 14
207** ± 17
202** ± 19
195** ± 23
183** ± 23
(50 mg/kg i.p. +
(25.3)
(29.1)
(30.8)
(33.2)
(37.3)
Tolbutamide
(100 mg/kg p.o.)
Treatment
6 hr
7 hr
8 hr
24 hr
I Streptozotocin
347 ± 19
355 ± 24
340 ± 22
349 ± 12
(50 mg/kg i.p.)
II Streptozotocin
133*** ± 16
102*** ± 9
91*** ± 8
128*** ± 18
(50 mg/kg p.o) +2
(51.4)
(62.7)
(66.7)
(52.2)
(100 mg/kg p.o.)
IV Streptozotocin
174*** ± 23
192** ± 29
242* ± 18
332 ± 26
(50 mg/kg i.p. +
(40.4)
(34.2)
(17.1)
Tolbutamide
(100 mg/kg p.o.)
Mean ± SD values mg/dl., Parenthesis shows % lowering from zero hour value. *P < 0.05, **P < 0.01, ***P < 0.001
5.3. Antioxidant Activity
The free radical oxidative stress has been implicated in the pathogenesis of a variety of human disease conditions including atherosclerosis. Polyunsaturated fatty acids within cell membranes and lipoproteins are oxidized and resulting active species modify macrophages and bystander cells monocytes which then move to subeudothelial space, engorge cholesteryl esters and are transformed into what are known as foam cells. Group of these foam cells form atherosclerotic plaques in the intima. The antioxidant potential of compound 2 was evaluated against metal induced oxidation of LDL as well as generation of hydroxy (OH) radical.
In vivo experiment with cholesterol fed animals caused marked formation of lipid peroxides in serum lipoproteins. Simultaneous treatment with compound 2 caused significant reversal of the lipid peroxide levels in serum VLDL, LDL and liver in cholesterol fed animals. However gemfibrozil failed to protect the phenomenon of lipid peroxidation (Table 12). Human serum LDL was oxidized with Cu ′2 in different concentrations of test compound in 0.05 mole PBS, pH 7.4 for 16 hr at 37° C. Thiobarbituric acid reactive lipid peroxides are measured by standard procedure. Compound 2 and α-tocopherol inhibit the generation of LDL lipid peroxide in concentration dependent manner. However the gemfibrozil at tested concentrations did not inhibit the oxidative modification (Table 13). Cu ′2 induced oxidation in LDL lipids are mainly due to the free OH radical during incubation. Therefore the effect tested for generation of OH radical in vitro in nonenzymatic system of Fe ′2 , sodium ascorbate, hydrogenperoxide and deoxyribose oxidative attack of oxy radical on deoxyribose caused fragmentation and formation of dialdehyde which are spectrophotometrically measured after their reaction with thiobarbituric acid. As observed in case of oxidation of LDL by metal ion, the compound 2 inhibits the generation of OH radical in concentration dependent manner. However, the activity of 2 is of low order to that of mannitol, a selective inhibitor of OH radical (Table 14)
TABLE 12
Effect of 3β-Hydroxypregna-5,16-dien-20-one (2) on lipid
peroxidation in cholesterol fed hyperlipidemic rats
Cholesterol +
Serum/
Drug (25 mg/kg)
Tissue
Control
Cholesterol Fed
Compound 2
Gemfibrozil
Serum a
675 ± 82
1228 ± 130
931.5 ± 51
1161 ± 74
(+82)
(−24)
(−5)
VLDL a
237 ± 25
379 ± 20
310 ± 15
346 ± 10
(+60)
(−18)
(−9)
LDL a
351 ± 17
604 ± 24
421 ± 20
568 ± 62
(+72)
(−30)
(−6)
HDL a
123 ± 13
138 ± 17
125 ± 10
134 ± 13
(+12)
(−9)
(−3)
Liver b
74 ± 8
274 ± 28
212 ± 16
253 ± 26
(+57)
(−23)
(−8)
Values are mean ± SD of 6 rats; a = n mol MDA/dl, b = n mol MDA/g. Values in the parenthesis below drug treated groups are % reversal as compared with cholesterol fed rats.
TABLE 13
Effect of 3β-Hydroxy-pregna-5,16-dien-20-one (2),
gemfibrozil and α-Tocopherol on low density
lipoprotein oxidation.
Concentration
(μmol/
Compound 2
Gemfibrozil
α-Tocopherol
ml)
MDA
MDA
Conc. (μmol/ml)
MDA
None
56.5 ± 3
52.0 ± 5.4
None
47.4 ± 3.8
2.5
Ref.
56.0 ± 5.8
52.8 ± 5.7
0.25
Ref.
47.4 ± 4.5
Exp.
41.4 ± 1.7
53.0 ± 6.0
Exp.
44.7 ± 4.5
(26)
(−)
(3)
5.0
Ref.
56.4 ± 5.6
50.7 ± 6.1
0.5
Ref.
47.3 ± 4.5
Exp.
28.7 ± 4.0
48.8 ± 6.7
Exp.
41.6 ± 4.0
(49)
(5)
(13)
10.0
Ref.
40.6 ± 3.7
49.4 ± 5.2
1.0
Ref.
47.4 ± 3.9
Exp.
10.6 ± 0.5
43.8 ± 4.9
Exp.
35.0 ± 3.8
(74)
20
Ref.
37.2 ± 0.8
49.0 ± 2.9
2.0
Ref
47.4 ± 4.4
Exp.
4.0 ± 0.5
41.4 ± 5.0
Exp.
24.3 ± 2.0
(89)
(16)
(51)
Values expressed as n mol MDA/mg protein are mean ± SD of four separate experiments. Values in the parenthesis are % inhibition.
TABLE 14
Inhibition of Hydroxy (OH) radical formation in nonenzymatic system.
α-Tocopherol
Concentration
Compound 2
Gemfibrozil
Conc.
(μmol/ml)
(nmol MDA/hr)
(nmol MDA/hr)
(μmol/ml)
(nmol MDA/hr)
None
90.4 ± 3.8
83.4 ± 7.5
None
78.2 ± 7.0
5
65.0 ± 5.4
79.9 ± 6.8
1
60.4 ± 7.0
(28)
(4)
(23)
10
52.8 ± 4.2
78.5 ± 8.0
2
45.2 ± 3.3
(42)
(5)
(42)
20
23.3 ± 1.8
76.8 ± 7.4
3
32.4 ± 3.5
(74)
(8)
(59)
30
11.7 ± 1.3
76.4 ± 3.8
4
27.1 ± 2.8
(87)
(8)
(65)
40
10.4 ± 2.0
74.3 ± 6.3
5
20.9 ± 2.0
(88)
(11)
(73)
50
9.9 ± 0.8
72.4 ± 8.0
—
—
(90)
(13)
Values are mean ± SD of four separate observations. Values in the parenthesis are % inhibition.
5.4. Cardiac Protection
The underlying cause of myocardial infarction is believed to be the progressive deposition of lipids and fibrotic material into the arterial wall. These pregnadienols and pregnadienous also provided cardiac protection as assessed in isoproterneol induced myocardial necrosis in rat model, which produces myocardial infarction due to an increased blood pressure and heart rate. The protection was comparable with that of gemfibrozil as described in Table 15.
TABLE 15
Effect of 3β-Hydroxypregna-5,16-dien-20-one(2) on serum
and tissue parameters of heart necrosis at
25 mg/kg (p.o.) in rats.
Isoproterneol
Isoproterneol + Drug (25 mg/kg)
(85 mg/kg, p.o.)
% Protection
Parameters
% Change
Gemfribrozil
Compound 2
Serum
CPK
109.9 ↑
33.9
35.7
GOT
41.6 ↑
24.9
27.0
GPT
85.0 ↑
33.4
22.7
Alkaline
28.8 ↑
41.2
24.0
Phosphatase
Heart
Ca. - ATPase
44.5 ↓
30.2
30.2
Glycogen
20.2 ↓
32.1
25.1
Lipid peroxide
65.8 ↑
69.8
72.6
Phospholipase
216.0 ↑
28.2
74.2
5.5. Androgenic Activity
The relative affinity of a few selected compounds in the series for cytoplasmic androgenic receptors present in human breast tumour cells MCF-7 (Michigan Cancer Foundation, MCF, USA) was estimated and compared with 4,5-dihydrotestosterone (DHT). The results showed that the compounds 2,3 and 5 have no or only negligible binding affinity which therefore would be a reflection of their low androgenic effect.
5.6. Progestational and Antiprogestational Activity
The relative affinity of compounds for cytoplasmic progesterone receptors present in human tumour cells (MCF-7) were estimated and compared with 16-ethyl-21-hydroxy-19-norpregna-4-ene-3,20-dione (Org 2058). The experiments conducted revealed that the compounds 2,3 and 5 have no or only negligible binding affinity.
The progestational activity was also tested in vivo by Clauberg assay method. The degree of endometrial proliferation was estimated on the McPhail scale where 3′ or 4′ was considered as a full progestational effect. 3β-Hydroxypregna-5,16-dien-20-one (2) did not exhibit any activity even at 200 mg/kg dose, whereas progesterone showed, as expected marked progestational activity even at 50 mg/kg. | The invention provides a method of using pregnadienones and pregnadienols represented by the structural formula (I) as shown herein below
Wherein X═OH or O or combination thereof and positioning of olefinic bonds are at 4(5); 5(6); 16(17); 17(20) or various combinations and said compounds containing at least one olefinic bond in or on their D-ring for the treatment of hyperlipidemic and hyperglycemic conditions in mammals, said method comprising administering an effective amount of the said compounds to the recipient mammals. | 2 |
RELATED APPLICATION
The present application is a divisional application of U.S. patent application Ser. No. 12/002,750, filed Dec. 18, 2007, now U.S. Pat. No. 8,146,295, which claims the benefit of U.S. Provisional Application No. 60/875,480 filed Dec. 18, 2006, the disclosures of which are incorporated by reference herein in their entirety.
FIELD OF THE INVENTION
The present invention relates to doors. More particularly, the present invention relates to z-bar assemblies for doors.
BACKGROUND OF THE INVENTION
A door assembly, such as a storm door, often involves the use of what is commonly referred to as a “z-bar.” The z-bars are typically formed to mount the door assembly to the jambs or exterior trim of the entry door. Normally there are two z-bars in such an installation: a hinge-side z-bar and a latch-side z-bar. There may also be a z-bar extending over the top of the door that serves as or facilitates a drip cap. The hinge-side z-bar is so named because it accommodates hinges for pivotal mounting of the door. The latch-side z-bar is so named because it is located adjacent the latch side of the door and may serve as part of a system to latch the door in a closed position.
Some manufacturers specify a given door assembly to cover a range of door openings. The door is typically equipped with a door expander or spacer that enables adjustment of the length of the door relative to the opening, as well as the adjustment of the orientation of the lower edge of the door to accommodate door sills and/or door casings that may not be true.
It is often desired that the z-bars extend over the entire length of the storm door or entry door jambs for reasons of aesthetics, connectivity and energy conservation. Accordingly, the z-bars are typically sized to operatively match a maximum or fully expanded length of the door.
However, the height of door openings will often vary and will often be less than the full length of traditional z-bars, requiring the installer to trim the ends of the z-bars off. Conventional methods and techniques for trimming z-bars are innately inconvenient and time consuming. In addition, many casings feature a sill having an inclined upper surface that sheds water. The trimmed ends of these traditional z-bars are typically cut to accommodate the incline. A trimming cut that either leaves the z-bar too short or at an improper angle relative to the incline is generally detrimental to the aesthetic and energy conservation qualities of the assembly, and increases the installation time of the door assembly.
Some manufacturers supply z-bars that are intentionally shorter than the minimum length of the door so that z-bar does not have to be cut to fit the height of the door frame during installation. Such an approach is disclosed in U.S. Patent Application Publication No. 2006/0150524 to Kibbel et al. While this approach negates the need for cutting the z-bar to length, it does not address the aforementioned detriments to aesthetics and energy conservation.
A z-bar assembly that avoids the problems that can result from shortened z-bars, and augments a more efficient installation procedure would be welcome.
SUMMARY OF THE INVENTION
Various embodiments of the invention include a z-bar having an extender for adjusting the length of the overall z-bar assembly. The length of the z-bar is generally undersized, with the extender slidably attached to provide a telescoping adjustment to the overall length of the assembly without need for trimming. The extenders may have substantially the same profile as the z-bar to maintain aesthetic appearance and functionality. The various embodiments may be applicable to both hinge-side and latch-side z-bars.
In one embodiment, a door assembly comprises a door casing or frame including a door jamb and a sill, at least one z-bar member mounted to the casing, and a z-bar extension member or extender mounted to the z-bar member and extending beyond the end of the z-bar member. One end of the z-bar assembly may be factory cut or otherwise formed to accommodate sill incline angles standard in the industry.
In another embodiment, the z-bar assembly includes an exterior z-bar member with an exterior barrel portion, and an interior z-bar extension member with an interior barrel portion. The interior barrel portion of the extension member is slidably engaged within the exterior barrel portion of the z-bar member, enabling the extender to selectively extend beyond the end of the exterior z-bar member.
In another embodiment, the z-bar extension member is made of a resilient material and is mounted on the exterior of the z-bar member by snapping engagement over the barrel portion of the z-bar member.
In another embodiment, the z-bar or z-bar extension member may include one or more score lines extending laterally across the z-bar extension member. The z-bar extension member can be snapped off or otherwise truncated at a selected score line to modify the length of the z-bar extension member. The score lines may also serve as a guide for cutting the z-bar or z-bar extension to a unique length between score lines.
In other embodiments, the z-bar extension member includes a base portion on one end. The base portion may be formed integrally with the z-bar extension member, and may define an obtuse angle with respect to the z-bar extension member to substantially match the incline angles of sills standard in the industry.
In certain embodiments, the interior and exterior z-bar members are formed with mating structures such as, but not limited to, projections and apertures or detents and grooves that cooperate to at least temporarily maintain the mated structures in a generally linear positional relationship with respect to each other to assist in the installation and adjustment of the assembly. In other embodiments, structures or cut-away portions may define slots for slidable engagement that imparts a friction between the interior and exterior z-bar members, thereby aiding in holding the adjustment of the length of the assembly.
In some embodiments, the interior z-bar extension member may be sized and configured such that it is under generally constant resistance within the exterior z-bar member, creating friction and restricting, but not prohibiting, movement of the extension member.
An embodiment is also disclosed wherein a guard assembly may be mounted on a vertical edge of the door, the guard assembly having a shield portion that extends at least partially over the z-bar or z-bar assembly. The guard assembly may extend the length of the vertical edge or only a portion thereof to cover at least a corresponding portion of the gap that exists between the vertical edge of the door and the z-bar assembly. The guard assembly may also take the form of an end cap that mounts to and covers an end of the door expander, to retain insulation within the door expander and/or to prevent debris such as dirt and salt from entering the door expander.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 through 3 are partial perspective views of a door assembly in an embodiment of the invention;
FIG. 4 is a perspective isolation view of the extended z-bar assembly of FIG. 2 ;
FIG. 5 is a partial perspective view of the z-bar of FIG. 4 in isolation;
FIG. 6 is a perspective view of the z-bar extension member of FIG. 4 in isolation;
FIG. 7 is a cross-sectional view of an extended z-bar assembly according to an embodiment of the invention;
FIG. 8 is a perspective of the components of an extended z-bar assembly according to an embodiment of the invention;
FIG. 9 is a side view of a z-bar extension member having ends with oblique angles in an embodiment of the invention;
FIG. 10 is a cross-sectional view of the z-bar extension member of FIG. 9 ;
FIG. 11 is a perspective view of an extended z-bar assembly with weather stripping in an embodiment of the invention;
FIG. 12 is a cross-sectional view of an installed z-bar assembly in an embodiment of the invention;
FIG. 13 is a cross-sectional view of an installed z-bar assembly having a spacer rib in an embodiment of the invention;
FIG. 14 is a partially exploded cross-sectional view of the extended z-bar assembly of FIG. 13 in isolation;
FIG. 15 is a cross-sectional view of an installed z-bar assembly having engaging slots for holding the extended z-bar assembly together in an embodiment of the invention;
FIGS. 15A and 15B are enlarged inset views of the cross-sectional view of FIG. 15 ;
FIGS. 16 and 17 are perspective views of a tongue overlay configuration in an embodiment of the invention;
FIG. 18 is a cross-section of FIG. 17 ;
FIG. 19 is a perspective view of a projection and aperture mating system having paired structures in an embodiment of the invention;
FIG. 20 is a perspective view of a projection and aperture mating system having elongate structures in an embodiment of the invention;
FIG. 21 is a cross section representative of both the FIG. 19 and the FIG. 20 embodiments;
FIG. 22 is a cross-section of a detent and groove mating system in an embodiment of the invention;
FIG. 23 is a perspective view of a z-bar extension member with score lines in an embodiment of the invention;
FIG. 24 is a perspective view of a z-bar assembly in an embodiment of the invention;
FIGS. 24A and 24B are perspective views of the z-bar extension member of FIG. 24 in isolation;
FIG. 24C is an elevation view of the z-bar extension member of FIG. 24 in isolation;
FIG. 24D is a section view of the z-bar extension member of FIG. 24C ;
FIG. 25 is a side view of a dual base z-bar extension member having a base on each end with and with oblique angles in an embodiment of the invention;
FIG. 26A is a partial cut away view of a guard assembly in an embodiment of the invention;
FIG. 26B is a partial perspective view of a guard assembly for capping an expander in an embodiment of the invention;
FIG. 26C is a top view of the guard assembly of FIG. 26B ; and
FIG. 27 is an end view of a guard assembly mounted to a door in an embodiment of the invention.
DETAILED DESCRIPTION
Referring to FIGS. 1 through 3 , a door assembly 30 including an exterior door 32 , a door frame or casing 34 and an extended z-bar assembly 36 having a z-bar 38 and a z-bar extension member 40 is depicted in one embodiment of the invention. The exterior door 32 , which may be a storm door or a screen door, may include a door expander 44 and a hinge member 46 . The door frame or casing 34 may include an exterior trim or door jamb 52 , a sill 54 and a header (not depicted). The sill 54 may have an inclined upper surface 56 . The z-bar 38 may be dimensioned so that a gap 57 exists between an end of the z-bar 38 and the sill 54 . The gap 57 is bridged by the z-bar extension member 40 .
Referring to FIGS. 4 through 8 , various embodiments of the extended z-bar assembly are depicted. In one embodiment, the z-bar 38 includes a flange portion 60 , a barrel portion 62 , a web portion 64 and a projecting portion 66 . The z-bar 38 may also be characterized as having an inward-facing surface 67 (e.g. the surface that generally faces the door jamb 52 ) and an outward-facing surface 68 (i.e. the surface opposite the inward-facing surface 67 that generally faces away from the door jamb 54 to which the z-bar 38 is mounted).
An embodiment of the z-bar extension member 40 may include an extender flange portion 70 , an extender barrel portion 72 , an extender web portion 74 and an extender projecting portion 76 . Not all of these portions are necessary in the construction of a z-bar extension member; some portions may be omitted and still provide effective extension of the z-bar assembly for functional or aesthetic purposes. Like the z-bar 38 , the z-bar extension member 40 may also be characterized as having an inward-facing surface 77 a and an outward-facing surface 77 b . The z-bar extension member 40 may be slidably engaged with the z-bar 38 . Note that some embodiments depicted in FIGS. 4 through 8 do not include the extender flange portion 70 (e.g. FIGS. 6 through 8 ). Also, the ends 79 of the z-bar extension member 40 may be substantially square with respect to a longitudinal axis 82 of the z-bar extension member 40 ( FIG. 8 ).
Referring to FIGS. 9 and 10 , an embodiment of the z-bar extension member 40 having ends 79 that define an oblique angle 80 relative to the axis 82 of the z-bar extension member 40 is depicted. The oblique angle 80 may be provided at just one end of the z-bar extension member, thereby defining a component that accommodates either the hinge side or the latch side of the door assembly 30 (but not both) without need for cutting an angle. The oblique angle 80 may also be provided on both ends, as depicted in FIG. 9 , in which case the same z-bar extension member 40 may be used on the hinge side or the latch side of the door assembly 30 . The z-bar extension member 40 may also include an extender flange projection 78 that projects outward from the extender flange portion 70 .
The embodiment depicted in FIGS. 1 through 3 illustrate the z-bar extension member 40 as being located inside the z-bar 38 . The extended z-bar assembly 36 may also be configured so that at least a portion of the z-bar extension member 40 is positioned over the z-bar 38 . Also, if the z-bar extension member 40 is formed of a resilient material, the z-bar extension member 40 can be flexed and snapped into or over the z-bar 38 , depending on the configuration.
Also, the embodiment depicted in FIGS. 1 through 3 illustrate the gap 57 as existing between the z-bar 38 and the sill 54 . In another embodiment, a gap may exist between the z-bar 38 and the header (not depicted), and the z-bar extension member 40 installed to bridge therebetween.
Functionally, the z-bar extension member enables the z-bar 38 to be fabricated with a length that is intentionally shorter than the length of the door jamb 52 . The barrel portion 62 of the z-bar 38 and the extender barrel portion 72 of the z-bar extension member 40 cooperate to guide the z-bar extension member 40 in an in-line or telescoping manner along the longitudinal axis 82 to bridge the gap between the z-bar 38 and the sill 54 . The extender flange projection 78 projects normal to the mounting surface of the door jamb 52 along the outside edge of the flange portion 60 and provides an externally accessible means for gripping the z-bar extension member 40 for positioning during installation of the extended z-bar assembly 36 .
The use of a resilient material for the z-bar extension member 40 that is mounted over the z-bar 38 (not depicted) enables installation of the z-bar extension member 40 after the z-bar 38 has been mounted to the door jamb 52 . The z-bar extension member 40 may then be secured in place by means known in the art such as with additional fasteners or with an adhesive.
Referring to FIGS. 11 through 15 , a variety of other embodiments of the invention are depicted in assembly. The extended z-bar assembly 36 is attached to the door jamb 52 of the casing 34 with fasteners 84 such as wood screws. The fasteners 84 may pass through the flange portion 60 and the web portion 64 of the extended z-bar assembly 36 to cover a corner 85 of the door jamb 52 that in part defines the exterior opening of the casing 34 .
The flange portion 60 may also be formed with a pair of rails 87 that straddle the fasteners 84 . A cap strip 86 may be formed to accommodate the rails 87 for placement over the heads of the fasteners 84 .
The embodiment of FIGS. 13 and 14 depict a rib 92 that projects from the web portion 64 of the z-bar 38 toward the door jamb 52 . The rib 92 may or may not pass through the z-bar extension member 40 in final assembly.
A weather stripping 88 or other suitable material may be mounted to the face of the projecting portion 66 . The projecting portion 66 may be formed with a pair of L-brackets 94 that define a track 96 for capturing the base of the weather stripping 88 .
Referring to FIGS. 15A and 15B , details of the configuration of FIG. 15 are depicted. In FIG. 15A , the projection portion 66 is limned as having a projection lip 98 that is substantially parallel with the projection portion 66 to define a slot 100 . The end of the extender projecting portion 76 is seated within the slot 100 and captured by the projection lip 98 . Likewise, FIG. 15B portrays a flange lip 102 that is substantially parallel with the flange portion 60 and defines a slot 104 that captures the edge of the extender flange portion 70 . The slots 100 and 104 may be dimensioned to provide a frictional resistance between the z-bar 38 and the z-bar extension member 40 .
Referring to FIGS. 16 through 18 , another embodiment of the extended z-bar assembly 36 is illustrated, including a pair of elongate slots 108 formed on the z-bar extension member 40 . In the depicted embodiment, one elongate slot 108 is located near the junction of the extender barrel portion 72 and the extender web portion 74 , the other near the junction of the extender projecting portion 76 and the extender web portion 74 . The elongate slots 108 may extend from a proximal end 109 of the z-bar extension member 40 along a portion of the length of the z-bar extension member 40 to form a tongue portion 110 of the extender web portion 74 . The elongate slots 108 may be substantially parallel to the longitudinal axis 82 .
The weather stripping 88 can be attached to both the projecting portion 66 and the extender projecting portion 76 . The weather stripping may be adhesively attached, or captured by a track or channel such as the track 96 , or by other means known in the art. The weather stripping 88 may be pre-installed, running the full length of the z-bar extension member 40 , and trimmed off when the desired length of the extended z-bar assembly 36 is established. Alternatively, the z-bar extension member 40 may be assembled without the weather stripping 88 , and a strip of it provided for trimming and mounting to the z-bar extension member 40 after the extended z-bar assembly 36 has been mounted to the door jamb 52 .
In assembly, the extender barrel portion 72 of the z-bar extension member 40 may be inserted into the barrel portion 62 of the z-bar 38 . The z-bar extension member 40 may be formed so that the extender web portion 74 , and therefore the tongue portion 110 , overlays an outer face 112 of the web portion 64 of the z-bar 38 . In this configuration, while the extender barrel portion 72 is engaged with the inward-facing surface 77 a of the barrel portion 62 of the z-bar 38 , the tab portion 110 is engaged with the outward-facing surface 77 b of the web portion 64 of the z-bar 38 in an interlacing fashion ( FIG. 18 ). The elongate slots 108 may be dimensioned to provide a frictional fit between the z-bar 38 and the z-bar extension member 40 .
The number of elongate slots 108 is arbitrary, as well as their placement. Consider, for example, a single elongate slot extending parallel to the longitudinal axis 82 . Such a configuration would enable the extension member 40 to engage both the inward-facing surface 77 a and the outward-facing surface 77 b of the z-bar. Likewise, more than two elongate slots can also be utilized for interlacing contact between the z-bar extension member 40 and the z-bar 38 .
Referring to FIGS. 19 through 22 , various structures for maintaining the lineal relationship between the z-bar 38 and the z-bar extension member 40 are illustrated. The FIG. 19 embodiment includes a plurality of mating projections 138 that extend outward from the extender web portion 74 . In the embodiment depicted, the mating projections 138 are in pairs at a given longitudinal location along the longitudinal axis 82 . The mating projections 138 of each pair are separated at a lateral spacing 139 . A plurality of mating apertures 140 are formed on the web portion 64 of the z-bar 38 , also in pairs having a lateral spacing 139 at a given longitudinal location. The mating projections 138 are dimensioned to engage with the apertures 140 . The layout (dimensional spacing) of the mating projections 168 and the mating apertures 140 are the same, and the respective pairs can be spaced at equal intervals 145 .
A similar concept is illustrated in FIG. 20 . Instead of paired projections and apertures, the web portions 64 and 74 can include elongate mating projections 142 and elongate mating apertures 144 spaced at uniform intervals 145 .
The cross-sectional depiction of FIG. 21 depicts how the embodiments of FIGS. 19 and 20 can appear after assembly.
An embodiment of similar concept is portrayed in FIG. 22 . In this embodiment, the extender web portion 74 is formed with a plurality of detents 146 , and the web portion 64 is formed with a plurality of grooves 148 . The detents 146 and grooves 148 can have a uniform spacing 150 and can be formed to mate or interlock with each other.
It is noted that the various projections, apertures, detents and notches are not limited to being formed on the components specified in FIGS. 19 through 22 . For example, in the FIG. 19 embodiment, mating projections may be formed on the interior of the web portion 64 to cooperate with mating apertures formed on the extender web portion 74 . Also, the detents of FIG. 22 may be utilized in the embodiments of FIGS. 19 and 20 . Furthermore, the positive locking concepts illustrated in FIGS. 19 through 22 may be incorporated with the sliding tab configuration of FIGS. 13 through 16 .
In operation, the z-bar extension member 40 may be slid inside the z-bar 38 until the extended z-bar assembly 36 is at or near a desired length. Depending on the embodiment utilized, at least a portion of the mating projections 138 , 142 or the detents 146 are then aligned with the nearest corresponding mating apertures 140 , 144 or the grooves 148 and snapped into place. The resolution of the adjustment can be minor fractions of an inch, depending on the spacing of the intervals 145 , 150 and the dimension of the mating apertures 140 , 144 or grooves 148 .
For the embodiment that includes the rib 92 , the rib 92 serves as a spacer to accommodate the thickness of the z-bar extension member 40 , thereby augmenting adjustment of the z-bar extension member 40 after the extended z-bar assembly 36 has been mounted to the door jamb 52 .
The slots 100 and 104 can serve to secure the z-bar extension member 40 in slidable engagement with the z-bar 38 during installation. The slots 100 and 104 , if properly dimensioned, also provide a frictional resistance between the z-bar 38 and z-bar extension member 40 that temporarily holds the z-bar extension member 40 in a fixed relationship in line with the z-bar 38 during the installation process.
The various components of the extended z-bar assembly 36 may be made of any suitable material such as extruded metal, forged metal, ferrous or non-ferrous metals, or a resilient material such as high density plastic. Extrudable materials include, but are not limited to, aluminum, aluminum alloy and composite resin materials. The z-bar assembly or components thereof may be of a roll formable material, such as aluminum, aluminum alloy or steel.
Referring to FIG. 23 , another embodiment of the z-bar extension member 40 is depicted wherein the z-bar extension member 40 further includes a plurality of score lines 200 . The score lines 200 may extend laterally across the z-bar extension member 40 (i.e. across the width of the z-bar extension member 40 ). In some embodiments, score lines 200 extend across one or more of the flange portion 70 , the barrel portion 72 , the web portion 74 , and the projecting portion 76 of z-bar extension member 40 . The score lines 200 can be formed on one side of z-bar extension member 40 (e.g. on the inward-facing surface 77 a , as depicted), or alternatively on both sides of z-bar extension member 40 .
The score lines 200 on the z-bar extension member 40 may comprise grooves that extend into the thickness of the z-bar extension member 40 . In this configuration, the z-bar extension member 40 may be rendered frangible or additionally scored at one of the score lines 200 for frangible separation. Alternatively, the score lines 200 may comprise printed guidelines to guide the installer in scoring the z-bar extension member 40 .
In operation, the frangible score lines 200 may enable the length of the z-bar extension member 40 to be modified by snapping off z-bar extension member 40 at the desired score line 200 . In one embodiment, the z-bar extension member 40 may be snapped off by application of a manual force. In another embodiment, additional tools such as clamps or wrenches may be used to assist an installer to snap z-bar extension member to a desired length.
For z-bar extension members 40 having the score lines 200 located only on the inward-facing surface 77 a , the outward-facing surface 77 b may have a smooth finish, which may have desirable aesthetic and maintenance qualities.
Where guide lines or light score lines are utilized instead of frangible score lines, the installer may cut the z-bar extension member 40 to any length whether on the guideline or not. The guidelines may provide the installer with sufficient resolution to create a desired cut between the guidelines.
In another embodiment of the invention, the score line concept is applied to the z-bar 38 (not depicted). That is, a plurality of score lines may be located proximate one or both ends of the z-bar 38 to enable an installer to readily shorten the z-bar. In this way, the z-bar 38 may be oversized initially. The scored lines on the z-bar 38 can be configured in any of the variety of ways discussed in relation to the scored lines 200 on the z-bar extension member 40 .
During installation, the installer could shorten the scored z-bar 38 for suitable clearance between the z-bar 38 and the sill 54 and /or header. Such clearance, however, may be less than a z-bar manufactured to provide clearance over a variety of door sizes, thus enabling coverage of the clearance gap with a shorter z-bar extension member 40 (or, in some cases, without need for a z-bar extension member at all). Generally shorter z-bar extension members may provide functional advantages to the door assembly, such as an ability to seal the entire inward-facing surface 77 a with a caulk or sealant to provide a more reliable moisture and/or thermal barrier. The shorter z-bar extension member may also provide aesthetic advantages as well.
In various embodiments, the length of z-bar extension member 40 may be modified by additionally scoring and/or cutting the z-bar extension member 40 using the desired score line 200 as a guide. Tools may be used to perform this operation, such as a saw, utility knife, hot wire, or other cutting tool. Also, the score lines 200 may be formed at an obtuse angle relative to the longitudinal axis 82 to conform to a given sill incline angle after being trimmed (not depicted).
Referring to FIGS. 24 and 24A through 24 D, a z-bar assembly 230 including the z-bar 38 and a molded z-bar extension member 240 comprising a moldable material is depicted in an embodiment of the invention. As in the previous embodiments, the molded z-bar extension member 240 may include an extender flange portion 270 , an extender barrel portion 272 , an extender web portion 274 and an extender projecting portion 276 . The z-bar extension member 240 may also be characterized as having an inward-facing surface 278 and an outward-facing surface 280 .
In one embodiment, a base portion 284 may be attached or integrally formed on one end of the molded z-bar extension member 240 . For the molded extender 240 , an integrally formed base 284 may be effected by the shape of the mold. The base portion 284 may be generally perpendicular with a longitudinal axis 286 of the z-bar assembly 230 . Alternatively, the base 284 may define an obtuse angle 288 (i.e. an angle that is greater than 90 degrees), as depicted in FIG. 24D .
The extender projecting portion 276 may include a slot or channel portion 290 and a deflecting portion 292 . The channel portion 290 and the deflecting portion 292 may be connected through a flexure or hinge portion 294 such as a living hinge. The base portion 284 may be formed with an aperture 296 immediately adjacent the deflecting portion 292 . In this way, the deflecting portion 292 is not directly connected to the base portion 284 , thus enabling the deflecting portion 292 to rotate about the hinge portion 294 .
The extender flange portion 270 may include a pocket structure 300 sized to accommodate the flange portion 60 , rails 87 and cap strip 86 of an embodiment such as depicted in FIG. 14 . In cross section, the pocket structure 300 may form a closed loop (not depicted) or a partially closed loop (as depicted).
The molded z-bar extension member 240 is generally comprised of a moldable material. Moldable materials include, but are not limited to, polypropylene, polyvinyl chloride (PVC), nylon, polycarbonate, acrylonitrile butadiene styrene (ABS), styrene and delrin. Other moldable materials available to the artisan may be utilized.
Functionally, the molded z-bar extension member 240 may be slidably engaged with the z-bar 38 . The channel portion 290 cooperates with the projecting portion 76 of the z-bar 38 to help secure the molded z-bar extension member 240 to the z-bar 38 . When the door is brought into contact with the deflecting portion 292 , the deflecting portion 292 can act as a positive sealing member against the door, thereby serving as a barrier or seal akin to a weatherstrip. Alternatively, the deflecting portion 292 may be excluded from the z-bar extension member 240 and weather stripping mounted to the z-bar 38 left exposed to perform the barrier function. Weatherstrip may also be adhesively attached to the projecting portion 276 to extend weather barrier protection beyond the end of the z-bar 38 .
The pocket structure 300 may be dimensioned to surround the lower end of the cap strip assembly (as depicted) or to abut with the cap strip 86 . The partial loop depicted in FIGS. 24 enables any water that enters the pocket from the top to drain out. Alternatively or additionally, slits or holes (not depicted) may be formed at the base of the pocket structure 300 for the drainage function.
The obtuse angle 288 between the base potion 284 and the longitudinal axis 286 may be formed to correspond with the incline of a sill (e.g. sill 54 of FIG. 1 ). The base portion 284 may serve as sealing structure that engages a door expander spline at the base of a door expander (not depicted) for a better seal between the door expander spline and the sill.
In other embodiments, the base may be formed separately. In these embodiments, the z-bar extension member and/or separate base may be formed by a process such as molding, extrusion, or roll forming, then glued, fused, fastened or otherwise connected to the molded z-bar extension member.
Referring to FIG. 25 , a dual base z-bar extension member 320 having an extension portion 322 , a first base portion 324 and a second base portion 326 is depicted in an embodiment of the invention. The extension portion 322 may define a longitudinal axis 328 . The ends may form substantially right angles with respect to the longitudinal axis 328 (not depicted) or obtuse angles 330 with respect to the longitudinal axis 328 (as depicted).
Functionally, the dual base z-bar extension member may be severed along a line 332 between the first and second base portions 324 and 326 to provide left side and right side z-bar extension members. Severability may be provided by a score line, or the user may cut the dual base z-bar extension member 320 at an arbitrary location between the first and second base portions 324 and 326 .
Referring to FIGS. 26A through 26C , a guard assembly 352 is depicted in another embodiment of the invention. The guard assembly 352 may be comprised of a base portion 354 having a first major surface 356 , a second major surface 358 , a top end 360 , a bottom end 362 , a front edge 364 and a back edge 366 . One or more rail portions 368 may extend in a direction substantially orthogonal to the first major surface 356 . A shield portion 370 may extend from the second major surface 358 . The rail portions 368 and the shield portion 370 may be formed integral to the base portion 354 , and may be flush with the front and back edges 364 and 366 . A spacing 372 may be defined between rail portions 368 so that the guard assembly 352 effectively caps a vertical edge 373 of the door 32 .
In one embodiment, the guard assembly 352 may be operatively coupled to the vertical edge 373 of the door 32 . The length of the guard assembly may cover substantially the entire length of the vertical edge 373 of the door 32 , or a portion thereof.
The guard assembly may serve as an end cap to the door expander 44 . The spacing 372 between the rail portions 368 may be dimensioned to provide an interference or snap-on fit between the end of the door expander 44 and the guard assembly 352 . The guard assembly 352 may be sized so that the top end 360 extends above the door expander 44 and the bottom end 362 extends below the door expander 44 so as to cover the end of the door expander 44 .
Referring to FIG. 27 , the top end 360 and/or the bottom end 362 of the guard assembly 352 may be formed or cut at an angle 374 relative to the front edge 364 . The angle 374 may correspond to the inclined surface 56 of the sill 54 .
In assembly, the guard assembly 352 may be mounted to one or both edges of the door 32 for engagement with either the hinge side or the latch side z-bar or z-bar assembly. Coverage of the guard assembly 352 may be along the entire vertical edge or edges 373 of the door 32 or just a portion thereof such as the expander 44 . In an alternative configuration, the rails may be spaced to fit both inside the door expander 44 while capping the vertical edge 373 of the door 32 . The guard assembly 352 may be placed over the end of the door expander 44 and adjusted to a position appropriate to provide contact or near contact with the top of the sill 54 when the exterior door 32 is closed. The guard assembly 352 may also be mounted to the end of the door expander 44 with glue, or with fasteners (not depicted), or by other means available to the artisan.
To accommodate mounting the guard assembly 352 with fasteners, the one or more rail portions 368 may extend over one or more of the faces of the door expander 44 or the door 32 at a distance sufficient to accommodate the head of a fastener (not depicted). The various means of mounting the guard assembly 352 to the door expander 44 herein disclosed or otherwise known to the artisan may be utilized separately or in combination.
For embodiments that include the angle 374 on the top and/or the bottom end 360 and 362 , the guard assembly 352 may be installed without need for cutting the guard assembly 352 . When both ends 360 and 362 have inclines 370 , the same guard assembly 352 may be utilized on either the hinge side or the latch side of the exterior door 32 .
Functionally, the shield portion 370 may engage or nearly engage the z-bar 38 when the door 32 is in a closed position. The guard assembly 352 enables the z-bar 38 to be dimensioned shorter than the length of the door jamb 52 , and bridges the gap 57 (e.g. FIG. 2 ) between the z-bar 38 and the door jamb 52 . The guard assembly 352 provides a barrier at the end of the door expander 44 that inhibits collection of matter such as dirt, sand and salts that may corrode the door expander 44 over time. The guard assembly 352 may also enhance the thermal insulative quality of the exterior door assembly in at least two ways. First, the guard assembly 352 inhibits the flow of air through the door expander 44 , thereby providing a dead air pocket 376 within the door expander 44 and enhancing the thermal resistance of the door assembly 30 ; the dead air pocket 376 may alternatively be filled with an insulation 378 that is contained when guard assemblies 352 are utilized on both ends of the door expander 44 . Second, the guard assembly 352 serves as an additional barrier for impeding air flow and inclement elements such as rain and snow into a gap 380 between the door 32 and the z-bar assembly 36 ( FIG. 26C ), particularly when the guard assembly 352 extends over an appreciable length of the vertical edge 373 of the door 32 .
The guard assembly 352 may be utilized without the z-bar extension member 40 , as depicted in FIGS. 26A through 26C , or in conjunction with the z-bar extension member 40 to provide the additional barrier characteristics outlined above.
The guard assembly 352 may be fabricated from a resilient material, such as metal or high density plastic, or from a more compliant material such as a rubber or silicone, or from a combination of resilient and compliant materials. Additionally, the shield portion 370 may be fitted with weather stripping or other suitable material to provide further insulative characteristics to the door assembly 30 and to compensate for dimensional intolerances that may occur in fabrication and installation.
In another embodiment, the shield portion 370 may be connected to the base portion 354 of the guard assembly 352 through a hinge portion (not depicted). The hinge portion may be a separate member, such as a spring-loaded pivot pin that connects the base and shield portions 354 and 370 , or a living hinge that is integral to the base and shield portions 354 and 370 , or by other hinging techniques known to the artisan. The hinge concept can provide compliance between the shield portion 370 and the z-bar 38 that compensates for dimensional intolerances that may occur in fabrication and installation, or which develop over time. The hinge concept may find enhanced utility in conjunction with hinge-side z-bars; the tight radius of rotation of the shield portion 370 about the z-bar 38 may cause over extension of the flexing of the shield portion 370 relative to the base portion 354 of the guard assembly 352 whenever the exterior door 32 is partially or fully opened. Repeated over extension may lead to fatigue failure between the shield portion 370 and the base portion 354 . The hinge member or hinge portion could be designed to reduce the fatigue of the components, thereby extending the life of the guard assembly 352 .
As previously discussed, a z-bar may be mounted to the header of a door casing, defining an upper gap between the z-bar and the header (not depicted). The guard assembly 352 may be utilized on the top edge of the door 32 to cover the upper gap when so configured.
References to relative terms such as upper and lower, front and back, left and right, or the like, are intended for convenience of description and are not contemplated to necessarily limit the present invention, or its components, to any specific orientation. All dimensions and aspect ratios depicted in the figures may vary with a potential design and the intended use of a specific embodiment of this invention without departing from the scope thereof.
Each of the additional figures and methods disclosed herein may be used separately, or in conjunction with other features and methods, to provide improved devices and methods for making and using the same. Therefore, combinations of features and methods disclosed herein may not be necessary to practice the invention in its broadest sense and are instead disclosed merely to particularly describe representative and preferred embodiments of the instant invention. Because various modifications, substitutions, and changes of this invention may be made by one of skill in the art without departing from the spirit thereof, the invention is not limited to the embodiments illustrated and described herein. Rather, the scope of the invention is to be determined by the appended claims and their equivalents. | A method of assembling a z-bar extension member to a z-bar that negates the need for trimming the z-bar. The apparatus includes an exterior z-bar member having an exterior barrel portion and an interior z-bar member having an interior barrel portion. The interior barrel portion is slidably or snappingly engaged within the exterior barrel portion. Mating structures may be included on the cooperating components to maintain a positional relationship therebetween during assembly. A guard assembly that mounts to the edge of a door or on the end of a door expander to cover the gap between the z-bar and the casing is also disclosed that may be used in conjunction with or as an alternative to the z-bar extension member. | 4 |
RELATED APPLICATION DATA
[0001] This application is a continuation-in-part of U.S. application Ser. No. 09/959,262, filed Oct. 22, 2001, which is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] This invention relates generally to medical skin piercing devices including blood sampling devices, and more particularly to skin prickers.
BACKGROUND
[0003] Blood sampling devices are used to draw a small drop of blood for analysis. One type of blood sampling device is a skin pricker. Such skin prickers are widely used by diabetics, for example, who need to know their sugar level. However, there are many other applications.
[0004] There are many different types of skin prickers, including spring-loaded devices that fire disposable lancets. Some pricking devices are entirely disposable after a single use. Regardless of the form, the pricker punctures the skin of the user and inflicts pain. While this pain is somewhat trivial and transitory, many users would welcome its reduction.
SUMMARY
[0005] This invention is a skin pricker designed to divert attention from the pain involved in the puncture of the skin tissue by a blood sampling device. The skin pricker of this invention increases comfort when lancing by affecting the sensation and perception of pain. Projections on the distal end of a lancing device, or skin pricker, contact the skin surface to confuse the nerves in the area of the prick to make the prick less noticeable. This approach disguises the lancing action to provide a more comfortable sample.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a perspective view of a skin pricker of this invention.
[0007] FIG. 2 is an enlarged perspective view of the depth adjuster of the skin pricker of FIG. 1 .
[0008] FIG. 3 is an exploded perspective view of the skin pricker of FIG. 1 .
[0009] FIG. 4 is a side elevation view in cross-section of the skin pricker of FIG. 1 .
[0010] FIG. 5 is a side elevation view of the skin pricker of FIG. 1 .
[0011] FIG. 6 is an end view of the skin pricker of FIG. 1 .
[0012] FIG. 7 is a top plan view of the skin pricker of FIG. 1 .
DETAILED DESCRIPTION
[0013] A skin pricker of this invention is a lancing device 20 for firing a lancet, as shown in the Figures. As may be seen by reference to FIGS. 1 and 2 , lancing device 20 includes depth adjuster 22 , which includes interior threads (not shown) adapted to engage a front clip 24 , which engages a body 26 . In the description below, distal refers to the nose or lancing end generally, while proximal indicates a direction away from the nose of the device.
[0014] Lancing device 20 may be used with a suitable disposable lancet, which may be inserted into lancet holder 28 by removing the assembly of the depth adjuster 22 and front clip 24 . Dialing depth adjuster 22 relative to front clip 24 alters the distance between the front clip 24 and the depth adjuster 22 , but does not disrupt engagement between the clip 24 and adjuster 22 . Therefore dialing of the adjuster 22 controls how far the lancet tip will project beyond aperture 30 of adjuster the embodiment shown, depth adjuster 22 includes indicia 32 that correspond to penetration depth indicator 34 , which together reflect the expected penetration level of the lancet into the skin of the patient.
[0015] As may be shown by reference to FIGS. 3 and 4 , depth adjuster 22 includes platform 36 and aperture 30 . Projections 38 encircle aperture 30 , and each projection 38 has a shallow conical form with a rounded tip 40 . The number and arrangement of the projections 38 may vary, as may the size and shape of the individual projections. For example, the arrangement may zigzag as it surrounds the aperture. Pyramidal projections may be used, or any other suitable shape. Alternatively, two rows of projections may encircle the aperture. The two rows may include projections having various shapes and may spaced at various distances. Projections having various shapes may also be used on the same device. The projections contact the skin surface to confuse the nerves in the area of the prick, making the prick less noticeable.
[0016] As shown in FIGS. 2 and 4 , lancet retention clip 42 fits into groove 44 on lancet holder 28 , retaining a lancet in lancet holder 28 . Clip 42 includes slit 48 , which allows clip 42 to expand for installation. Wings 50 of lancet holder 28 are adapted to be received in corresponding wing slots 52 on the distal portion of body 26 .
[0017] Recoil spring 54 fits around lancet holder 28 between cap 56 and wings 50 , and urges lancet holder 28 in a proximal direction, or rearward, in a resting state where the lancet does not project beyond the nose. The recoil spring 54 urges the lancet back to this resting state immediately after tiring and lancing. Wings 50 translate in slots 52 , and catch on wing stops 58 , preventing the lancet holder 28 from being recoiled beyond the distal portion of the body 26 after firing of the lancet.
[0018] Hammer 60 is urged toward the distal end of body 26 by main spring 62 . The distal end of the main spring 62 contacts the proximal end of the hammer 60 , fitting around ring 64 that projects from the proximal end surface of the hammer 60 and that surrounds the aperture 66 of the hammer 60 . The proximal end of main spring 62 rests against inner end surface 68 of the force adjuster 70 .
[0019] Body 26 includes button frame 72 adapted to receive firing button 74 . Foam pads 76 on the interior of firing button 74 contact the outer surface of body 26 , and clips (not visible) on the interior of the button 74 are received in holes (not visible) in the body 26 , securing the button 74 to the body 26 in the frame 72 . In a loaded position, finger 82 of hammer 60 translates in loading slot 86 of body 26 . Depressing firing button 74 causes button tab 88 to depress finger 82 of hammer 60 , so that main spring 62 urges hammer 60 forward, forcing finger 82 out of loading slot 86 and into firing slot 90 of body 26 . Knob 92 on the distal end of hammer 60 is adapted to fit into the proximal end of lancet holder 28 , so that the main spring 62 pushes the hammer 60 into contact with lancet holder 28 , expelling the lancet beyond the platform 36 of the depth adjuster 22 and into contact with the patient. In this manner, hammer 60 is projected toward lancet holder 28 , firing the lancet and pricking the patient.
[0020] Force adjuster ring 94 fits around body 26 proximal to the button 74 . Force adjuster 70 includes longitudinal flange 96 and tab 98 . Flange 96 is adapted to translate in flange opening 100 of body 26 , while tab 98 translates in tab slot 102 of body 26 . Flange opening 100 includes detents (not visible), so that flange 96 is locatable at set positions. In one embodiment, flange opening 100 subtends approximately 80 degrees of the circumference of the body 26 in a generally spiral path and three detents in the proximal edge of opening 100 can receive flange 96 alternatively to provide three different levels of force.
[0021] Flange 96 is captured between a pair of ridges 106 on the inner surface 108 of force adjuster ring 94 . Extensions 110 on either side of body 26 abut annular ring 112 on the inner surface 108 of ring 94 , maintaining the axial position of the ring 94 . Extensions 110 have the force of leaf springs that are compressed when ring 94 is pressed into position and then spring out so that their ends abut annular ring 112 and thereby capture ring 94 and retain it on the body 26 .
[0022] Rotating force adjuster ring 94 causes ridges 106 to force flange 96 distally or proximally to adjust the force of main spring 62 when the lancet device 20 is triggered. Thus, the force is adjusted by turning the ring 94 , which moves the force adjuster 70 axially to adjust the compression of the main spring 62 . Force adjustment indicator 114 on body 26 may be aligned with one of the notches 116 on ring 94 , allowing the user may set the amount of force with which to deliver the lancet.
[0023] Body sleeve 118 includes two semi-cylindrical halves, which fit around proximal end of body 26 , over body spring 120 , which extends between cap 122 of body 26 and internal lip 124 of sleeve 118 . Keys 126 of body sleeve 118 are received in and move axially along keyways 128 of body 26 . Body spring 120 urges sleeve 118 distally in a resting, or loading, state.
[0024] Sleeve 118 includes shelf 130 having an aperture 132 adapted to receive the cap 134 of the loading rod 136 and the cap 138 of the support rod 140 . Loading rod 136 and support rod 140 each include a flat edge that abut each other, so that the two rods extend through the force adjuster 70 and the ends of the rods are received in the proximal end of hammer 60 . The use of the two part rod structure, rods 136 and 140 , permit insertion of first rod 136 through the opening 66 of hammer 60 and then rod 140 , so that combined rods 136 and 140 substantially fill opening 66 of hammer 60 . Loading rod 136 also includes a hook 142 that engages ledge 144 of hammer 60 , preventing removal.
[0025] After firing, pulling sleeve 118 in the proximal direction compresses body spring 120 and draws the assembly of the sleeve 118 , the rods 136 , 140 and the hammer 60 rearward, or distally, resetting finger 82 of hammer 60 into loading slot 86 . The lancet may then be removed, and a new lancet inserted, by removing the assembly of the depth adjuster 22 and front clip 24 .
[0026] All variations of the structures illustrated in the drawings and the materials described above are within the scope and spirit of this invention and the following claims. | A blood sampling device designed to divert attention from the pain involved in the puncture of the skin tissue by increasing comfort when lancing the skin by affecting the sensation and perception of pain. Projections on the distal end of a skin pricker contact the skin surface to confuse the nerves in the area of the prick to make the prick less noticeable. | 0 |
TECHNICAL FIELD OF THE INVENTION
[0001] The present invention is related to a method for operating a hearing system with the aid of a camera as well as to a hearing system.
DESCRIPTION OF THE RELATED ART
[0002] One of the most important goals of a hearing system is to enhance the intelligibility of speech also in adverse listening conditions. A beam former is one of the functionalities, which improves the intelligibility of speech, when the speaker is in front of the hearing device user. But in many situations this is not the case.
[0003] It is difficult to analyse acoustically to which person the hearing device user wants to listen to, especially when several individuals are talking. There is no hearing system yet that enables the hearing device user to select the individual the user wants to listen to and that tracks the location of this individual such that the hearing device optimizes the intelligibility exactly to this location.
[0004] There are solutions that propose to use further sensors, especially image sensors, to improve the beam former of a hearing device. For example, the teaching U.S. Pat. No. 6,707,921 B1 discloses an image based solution to determine when a speaker is speaking. Furthermore, DE 10 147 812 B4 discloses a hearing system comprising a camera. The known hearing system may use image processing to determine a number of speakers, perform lip-reading and to control a beam former.
SUMMARY OF THE INVENTION
[0005] It is an object of the present invention to provide a method for operating a hearing system as well as a hearing system that are significantly improved with regard to the known solutions.
[0006] It is pointed out that the term “hearing device” covers a hearing aid—such as a BTE-(Behind-The-Ear), an ITE-(In-The-Ear), a CIC-(Completely-In-Channel) hearing device or the like—and also an implantable device that is used to improve the hearing of a hearing impaired person.
[0007] First, the present invention is directed to a method for operating a hearing system comprising a hearing device, a camera and an auxiliary device. The inventive method comprises the steps of:
providing an input signal for said hearing device, capturing an image or a sequence of images of at least sections of a surrounding of a user wearing said hearing device, processing said image or said sequence of images in said auxiliary device for obtaining consolidated data of a sound source being important for said user, transmitting said consolidated data to the hearing device, generating an output signal in said hearing device by processing the input signal and by taking into account said consolidated data, and feeding said output signal to an output transducer of said hearing device.
[0014] The step of “providing an input signal for said hearing device” shall be understood as capturing an acoustic signal impinging on the input transducer of the hearing device. The input transducer comprises two or more microphones, for example. Two or more microphones are required if the hearing device shall have beam forming capabilities.
[0015] The present invention results in an improved intelligibility for the hearing system user while energy resources in the hearing device are maintained at the same time.
[0016] In an embodiment of the method according to the present invention, said processing comprises locating said sound source being of importance to said user and said consolidated data of a sound source comprises a directional angle being defined between a sagittal plane of said user and said sound source seen from said user.
[0017] The consolidated data is the result of the processing of the images or sequence of images and may very well be a single parameter as the angle defined between the sagittal plane of the user and the sound source seen from the user.
[0018] Further embodiments of the method according to the present invention further comprise the steps of:
selecting said sound source being important to said user of said hearing device out of a plurality of sound sources, and tagging said sound source by activating an input on the auxiliary device.
[0021] Further embodiments of the method according to the present invention further comprise the step of tracking said sound source.
[0022] In further embodiments of the method according to the present invention, the auxiliary device is one of the following:
a smartphone; a remote control.
[0025] In further embodiments of the method according to the present invention, said camera is positioned at the head of the user.
[0026] Further embodiments of the method according to the present invention further comprise the step of augmenting said consolidated data by information of a sensor unit, such as a compass or an additional microphone signal.
[0027] Further embodiments of the method according to the present invention further comprise the steps of:
detecting a present position of said user relative to the camera, and calculating a direction in which said sound source being important for said user taking into account the present position of said user.
[0030] Further embodiments of the method according to the present invention further comprise the steps of:
detecting a favorite speaker as said sound source by face recognition and comparison to a corresponding data base, and tracking said favorite speaker after a tracking command is received by said auxiliary device.
[0033] In further embodiments of the method according to the present invention, said input signal to the hearing device originate from at least one input transducer or from a streaming unit.
[0034] Furthermore, the present invention is directed to a hearing system comprising:
a hearing device comprising an input transducer, an output transducer and a processing unit being operatively connected to the input transducer and the output transducer, at least one camera for capturing an image or a sequence of images of at least a section of a surrounding of a user wearing said hearing device, an auxiliary device receiving and processing said image or said sequence of images for obtaining consolidated data of a sound source being important for said user, and a transmission channel between said auxiliary device and said hearing device for transmitting said consolidated data to said hearing device,
[0039] wherein said processing unit is adapted to take into account said consolidated data while generating an output signal for the output transducer.
[0040] Complexity of the image analysis requires high computing resources, which may not be available in a BTE-(Behind-The-Ear) or ITE-(In-The-Ear) hearing devices. Otherwise, image analysis would lead to an excessive use of battery power. Continuous streaming of image data would also require too much power.
[0041] In an embodiment of the hearing system according to the present invention, a low power technology is used for the transmission channel, such as Bluetooth standard or inductive coupling.
[0042] In further embodiments of the hearing system according to the present invention, the transmission channel is adapted to continuously transmit consolidated data from the auxiliary device to the hearing device.
[0043] In further embodiments of the hearing system according to the present invention, the auxiliary device is a smartphone or a remote control.
[0044] It is expressly pointed out that also all combinations of the above-mentioned embodiments are possible and herewith disclosed. Only those embodiments or combinations of embodiments are excluded that would result in a contradiction.
BRIEF DESCRIPTION OF THE DRAWINGS
[0045] The present invention is further described by referring to drawings showing exemplified embodiments of the present invention.
[0046] FIG. 1 schematically shows a known BTE-(Behind-The-Ear) hearing device with its main components,
[0047] FIG. 2 schematically shows a side view of a head of a user wearing the hearing device of FIG. 1 and glasses with a camera,
[0048] FIG. 3 a and FIG. 3 b show two situations a hearing device user may encounter,
[0049] FIG. 4 schematically shows the hearing system with an auxiliary device, and
[0050] FIG. 5 a and FIG. 5 b schematically shows a situation with the user of the hearing device, with the auxiliary device and a person being of interest for the hearing device user.
DETAILED DESCRIPTION OF THE INVENTION
[0051] FIG. 1 schematically shows a known BTE-(Behind-The-Ear) hearing device 1 with its main components comprising a battery 2 , a processing unit 3 , a wireless interface unit 4 , a first input transducer 5 , a second input transducer 6 and a receiver unit 7 , to which a tube is connected (not shown in FIG. 1 ) to conduct sound generated by the receiver unit 7 to an ear of a hearing device user via an ear tip positioned in the ear canal, for example. The battery 2 is providing energy to the wireless interface unit 4 as well as to the processing unit 3 , in which input signals of the first and second input transducers 5 and 6 are processed and in which an output signal is generated for the receiver unit 7 .
[0052] FIG. 2 shows a side view of a head 10 of a hearing device user wearing the hearing device 1 of FIG. 1 . Besides the internal components of the hearing device 1 a sound tube 8 is also shown that is connected to an ear piece (not shown in FIG. 2 ) arranged in the ear of the hearing device user. As can be seen from FIG. 2 , the hearing device user is wearing glasses 13 to which a front camera 11 and a side camera 12 are attached. Furthermore, a sensor unit 14 is also attached to the glasses 13 , the sensor unit 14 being a microphone or a compass, for example.
[0053] The cameras 11 , 12 and the sensor unit 14 generate output signals that must be processed, for example by applying a tracking algorithm for tracking a person being of interest for the hearing device user. As a matter of fact, such a processing is rather intense and asks for a rather powerful processor. Because the hearing device 1 typically has limited processing power and limited battery capacity, the processing of the output signals of cameras 11 , 12 and the sensor unit 14 are processed in an auxiliary device 21 ( FIGS. 4, 5 a and 5 b ). Thereto, the cameras 11 , 12 and the sensor unit 14 are connected to said auxiliary device 21 , which can be a smartphone or a remote control having ample processing power available. Therefore, the cameras 11 and 12 transmit its raw data to the auxiliary device 21 , in which the raw data is processed according to the envisaged task. In fact, by applying the envisaged tasks, e.g. the tracking algorithm to track a person being important to the hearing device user, consolidated data is generated from the raw data by the auxiliary device 21 . These consolidated data are taken into account in the hearing device 1 , i.e. in the processing unit 3 , while generating the output signal of the hearing device 1 by processing the audio signal.
[0054] The consolidated data can be, for example, an angle or a direction towards a person being important for the hearing device user. The angle is updated on a regular basis in order that said person can be tracked without delay.
[0055] The tracking algorithms run on a powerful processor of the auxiliary device 21 . The result (i.e. an angle) is transmitted to the hearing device 1 via a wireless connection, for example.
[0056] Since the consolidated data is small in comparison to the raw data (e.g. an image or a sequence of images), taking into account the consolidated data in the processing unit 3 of the hearing device 1 only results in a low battery load.
[0057] The sensor unit 14 attached to the glasses 13 (as shown in FIG. 2 ) or attached to the auxiliary device 21 is used, in a further embodiment of the present invention, to enhance robustness of the algorithms being implemented. If a tracking algorithm is implemented, the auxiliary device 21 may very well be used to initialize the tracking of a person being important to the hearing device user. This can be achieved by pressing a bottom on the auxiliary device 21 while pointing to said person at the same time.
[0058] It has already been described that some embodiments of the present invention comprise more than one camera 11 , 12 .
[0059] While the first or main camera 11 is pointing to the front, further cameras may be attached at the side of the head of the hearing device user. Preferably the cameras 11 , 12 are attached on the glasses 13 (as shown in FIG. 2 ), or on the hearing device 1 (not shown). However, it is important that the cameras 11 , 12 move with the head of the hearing device user to detect the angle between a sagittal plane of said user and the person (speaker) being important for the hearing device user.
[0060] In a further embodiment, at least one of the cameras 11 , 12 is a TOF-(Time-of-Flight) camera, such as used in “Microsoft Kinect” or in a smartphone. It is noted that the smartphone may also comprise two cameras that might be used according to the present invention.
[0061] In case that the hearing device 1 is not mechanically coupled to the head of the hearing device user, it is necessary to detect a head movement of the hearing device user in order to track said person being important for the hearing device user (e.g. a speaker). Such an information could be derived from a further sensor in the hearing device 1 , such further sensor being a camera looking at the head of the hearing device user, for example.
[0062] A synchronization of the acoustic detection of speech pauses of the person being important for the hearing device user (speaker or target person) with the visual detection of the conversation activity of the target person (e.g. by detecting whether said person is talking or is silent) by analysing an image taken by the camera, makes the tracking algorithm more robust and may help for a fast adaptation to conversational turns (e.g. changing the target person) by visual detecting speech pauses of the target person in continuous manner. In a further embodiment of the present invention, the microphone of the auxiliary device (e.g. smartphone) may be used for such a detection.
[0063] FIGS. 3 a and 3 b schematically show top views of the hearing device user 10 among a number of people 15 to 19 surrounding said user 10 . The hearing device user 10 wears the hearing device 1 illustrated in and described in connection with FIG. 2 .
[0064] In the situation depicted in FIGS. 3 a and 3 b , it is assumed that the hearing device user 10 is interested in listening to what the speaker A (person 15 ) says. In order that the hearing system according to the present invention is able to track speaker A, the hearing device user 10 must enable tracking of speaker A. Thereto, an initial sign indicating speaker A must be given to the hearing system in order that the hearing system may track speaker A.
[0065] In FIG. 3 a , a situation is depicted in which the hearing device user 10 initializes a tracking of speaker A. Such an initialization can be done, for example, by pointing with the camera 11 to the speaker A, i.e. the hearing device user 10 looks to the speaker A. In case the camera 11 is not fixed to the head of the hearing device user 10 , an orientation of the camera relative to the head of the user 10 needs to be known. For this purpose a compass comprised in the hearing device 1 may be used. In further embodiments, similar orientation signals, e.g. a compass signal form the auxiliary device 21 or of a further camera can be used.
[0066] Once the hearing device user 10 decides to start tracking speaker A, one of the following initialization procedures may be performed:
A button on the auxiliary device 21 is pressed. Instead of pressing a button, any other input method may be used, such as, for example, a voice command. If the hearing system incorporates acceleration sensors, a specific head movement by the hearing device user 10 —like a head tilt with a specific angle—can be detected. If the hearing system incorporates an eye-tracking system, the hearing device user 10 may look into different directions with a specific directional pattern that is detected to start tracking speaker A. Alternatively, twinkling with the eyes may be also detected to start tracking speaker A.
[0071] In a further embodiment, the hearing system according to the present invention comprises face recognition capabilities and comprises a database of faces of known speakers (favorites). In such an embodiment, the initialization of tracking a speaker may be done by a voice command, such as “listen to Lisa”. The system would then try to find the face of Lisa. Once the face of Lisa has been identified, Lisa is defined as the sound source being most important to the hearing device user 10 and therefore is tracked. A person that is selected to be tracked but is not in the database could be added to the database, if a proper snapshot of the face of this person can be taken during a conversation.
[0072] Disabling tracking may work similar as enabling tracking. In addition, situation specific actions can disable tracking a speaker, like:
Speaker A stops talking for a certain while. Speaker A or the hearing device user leaves the scenery (e.g. speaker A appears smaller in the captured sequence of images or disappears from the images). No signal coming from the speaker A for a predefined time.
[0076] According to the present invention, a number of possible criterions are being implemented for tracking a person being important for the hearing device user. One criterion might be typical characteristics of a face of a person to be tracked, whereas these face characteristics are memorized and used with image processing methods for face recognition. In general, recognizing the presence of a face and tracking the movement of this face, whereas such an algorithm may be enhanced by
detecting the acoustic direction of any incoming signal/voice, assuming that it is the voice of the tracked person; the synchronization of the acoustic onsets and offsets of any signal/speech signal (originating from the same direction) with the movement of the mouth or head captured with the camera; capturing acoustic properties of the voice of the speaker during the enabling process (according to speaker recognition algorithms) and comparing this signal with the video analysis (e.g. moving source and/or face recognition and/or movement of the mouth) (synchronization of speech pauses or/and directionality of the source); in case the hearing device user wears any movement sensors on the head, any head movements can be incorporated in the calculation of the angle between the speaker and the hearing device user. In case the angle between the body of the speaker and the body of the hearing device user are the same, the tracking of the head movement of the hearing device user is sufficient to calculate the wanted angle. matching characteristics of the face with characteristics of the voice (e.g. low pitch of the voice and male characteristics in the face). matching size of the face and acoustic distance of the speech (if possible, signal processing optimizes for distant speech as well, e.g. mixing between streaming-microphone mode toward more percentage of the streaming signal).
[0083] FIG. 4 shows the hearing device user 10 wearing a hearing device 1 and glasses 13 as depicted in FIG. 2 as well as a person 15 being important for the hearing device user 10 . In addition, the auxiliary device 21 is also shown in FIG. 4 being linked to the cameras 11 and 12 , the sensor unit 14 and the hearing device 1 via a wireless link being proprietary or a standardized link, e.g. Bluetooth or the like. As has been already mentioned, processing of image or sequences of images are processed in the auxiliary device 21 by generating consolidated data (e.g. an angle α being defined between a sagittal plane of the hearing device user 10 and the person 15 being important for the hearing device user 10 . Only the consolidated data are then transmitted to the hearing device 1 , where it is taken into account while processing the signal or signals of the input transducers 5 , 6 .
[0084] It is pointed out that a sound source being important for the hearing device user is not always a speaker as it is described in connection with FIGS. 3 a and 3 b . A sound source being important for the hearing device user 10 may very well also be an audio source from a Radio or TV set, for example.
[0085] FIGS. 5 a and 5 b show two situations with an alternative sound source 22 being of interest to the hearing device user 10 , the situation depicted in FIG. 5 b being a mixture of the alternative sound source 22 and a speaker A (reference sign 24 ).
[0086] In FIG. 5 a , the hearing device user 10 wearing glasses 13 , as explained in connection with FIG. 2 , is positioned before a TV set 22 comprising a wireless interface unit 23 for streaming the audio signal of the TV set 22 via the auxiliary device 21 to the hearing device. As a matter of fact, an audio signal that is emitted by the loudspeaker of the TV set 23 and picked up by an input transducer 5 , 6 ( FIG. 1 ) of the hearing device 1 is replaced by the audio signal of the TV set 23 being streamed via the wireless interface unit 23 . Therewith, the quality of the signal received for processing in the hearing device 1 is higher than for a signal picked up by the input transducers 5 , 6 as these input transducers 5 , 6 also pick up noise and surrounding sounds.
[0087] In other words, if the loudspeakers of the TV set 23 comprises streaming means, the signals picked up by the input transducers 5 , 6 can automatically be substituted by the streamed audio signal. It is pointed out that any device may be upgraded to include streaming means. In particular, a remote microphone may comprise streaming means in order to transmit the picked-up sound directly to its destination or processing unit.
[0088] The presence of streaming means may be recognized by using the camera of the auxiliary device 21 . The camera detects the TV set 23 or may recognize that a speaker is using a remote microphone comprising streaming means. At the same time, the auxiliary device 21 may scan available audio-streams. In case a hearing device user wants to track such a sound source having streaming means, the user may connects his auxiliary device 21 to an audio stream coming from the corresponding sound source. The auxiliary device 21 may than act as a relay station between the streaming device and the hearing device. Alternatively, a direct streaming from the streaming device to the hearing device is possible. | A method for operating a hearing system including a hearing device, a camera and an auxiliary device, the method including the steps of providing an input signal to the hearing device, capturing an image or a sequence of images of at least sections of a surrounding of a user wearing the hearing device, processing the image or the sequence of images in the auxiliary device) for obtaining consolidated data of a sound source being important for the user, transmitting the consolidated data to the hearing device, generating an output signal in the hearing device by processing the audio signal and by taking into account the consolidated data, and feeding the output signal to an output transducer of the hearing device. Thereby, a hearing system having improved capabilities is obtained. | 7 |
This is a division of application Ser. No. 08/044,882, filed Apr. 6, 1993 U.S. Pat. No. 5,395,548.
FIELD OF THE INVENTION
The present invention relates generally to the field of manufacturing processes and particularly to the cleaning of electrical assemblies.
BACKGROUND OF THE INVENTION
Soldering components to a circuit board assembly typically leaves contaminants such as solder flux, resins, and ionic compounds. These contaminants must be removed if the circuit board assembly is to be sealed from the elements by a protective coating. The protective coating may not properly adhere to an assembly containing contaminants. The contaminants may also be removed for aesthetic purposes, to prevent corrosion, or to increase the assembly's insulation resistance.
The cleaning process to remove the contaminants is usually done with chlorofluorocarbon (CFC) based solvents in liquid or vapor form. These solvents are frequently an azeotrope of trichloro-trifluoroethane and another solvent such as an alcohol, an example being methanol. One such solvent is a fluorinated hydrocarbon manufactured by E. I. DuPont de Nemours & Co. and marketed under the trade name FREON TMS.
The cleaning process is typically accomplished by placing the solvent in a container having heating elements at the bottom and condensing elements near the top. The solvent is then heated to its boiling temperature of 43.3° C., producing a solvent vapor above the liquid solvent. The circuit board or electronic assembly to be cleaned is placed in the vapor. The electronic assembly, being at a lower temperature than the vapor, causes the vapor to condense on the assembly, thereby cleaning off the contaminants by dissolving or flushing off the contaminants.
The vapor that did not condense on the electronic assembly is retained in the cleaning apparatus by the condensing elements. These elements, typically operated at a temperature of 10° C., cause the higher temperature vaporized solvent to condense back to liquid, returning to the bottom of the container to repeat the cycle. While the condensing elements in the container keep most of the solvent in the container, some of the solvent diffuses across the air-solvent interface and therefore escapes into the atmosphere. In addition, the assemblies being cleaned may retain small amounts of solvent on their surfaces after removal from the cleaning apparatus. Also, the spilling of solvent by workers refilling the cleaning apparatus can release the solvent into the atmosphere.
The solvent must be retained in the apparatus due to its expense and because of environmental concerns. In recent years, scientific studies have shown that CFCs have been depleting the protective ozone layer above the Earth, causing holes to form in this layer.
Alcohols such as isopropyl, methanol, or ethanol have been tried as an alternative to CFC based solvents. The assembly to be cleaned is initially immersed in and then sprayed with isopropyl alcohol, dissolving and/or washing off the contaminants. Alcohol, while it adequately removes ionic material from the assembly, may leave a white residue. Customers buying the assembly might get the impression that the assembly has not been cleaned or is defective in some way. There is a resulting need for an environmentally safe cleaning solvent that removes ionic material and does not leave a residue on the assembly being cleaned.
SUMMARY OF THE INVENTION
The present invention utilizes a non-azeotropic solvent mixture for printed circuit board or assembly cleaning that does not contain ozone-depleting chemicals. The solvent mixture contains a distillable, low to moderate boiling point halogenated or non-halogenated alcohol, in conjunction with a less volatile, higher boiling point terpene compound or N-methylpyrrolidinone. The invention also relates to a process for cleaning, whereby the article to be cleaned is immersed in the heated solvent mixture, the latter heated to a temperature sufficient to distill the low to-moderate boiling point alcohol and create a vapor zone containing the essentially-purified component for the purpose of drying. The cleaned article is withdrawn from the heated solvent mixture, maintained in the vapor zone for drying, then removed in a cleaned and dried state. The compositions of matter do not incorporate chlorofluorocarbons or other chemicals that deplete the ozone layer.
BRIEF DESCRIPTION OF THE DRAWINGS
The Figure shows the cross section of an apparatus for practicing the method of the present method.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The composition of the present invention comprises miscible liquids for cleaning and defluxing printed circuit assemblies. The first component, subsequently referred to as component A, is a distillable halogenated or non-halogenated alcohol. The second component, subsequently referred to as component B, is a relatively non-volatile organic liquid from the terpene family or a high boiling point aprotic solvent.
In the preferred embodiment, component A represents 5 to 95 parts by weight of a halogenated or non-halogenated alcohol containing from two (2) to four (4) carbon atoms. Also in the preferred embodiment, component B comprises from 5 to 95 parts by weight of a monocyclic or bicyclic terpene, terpene alcohol or mixture thereof. Examples of alcohols suitable for this invention include isopropanol, ethanol, n-propanol, n-butanol, 2,2,3,3,3-pentafluoropropanol, 1,1,1,2,2-pentafluoro-3-propanol, and others. Examples of component B include dipentene, d-limonene, l-limonene, a-terpinene, g-terpinene, carene, camphene, terpinolene, a-pinene, b-pinene, a-terpineol, geraniol, linalool, nerol, and other compounds from the p-menthadiene family.
Additionally, the present invention utilizes a composition of matter useful for cleaning and defluxing printed circuit boards where component B comprises from 5 to 95 parts by weight of N-methylpyrrolidinone (NMP). The use of other aprotic solvents of this type can be envisioned within the scope of this invention.
The compositions of matter disclosed may absorb water in the course of equipment idling or operation via atmospheric humidity or assembly drag-in. This water may be considered part of the distillable cleaning fluid composition, although its presence can be controlled via desiccation if necessary.
The present invention utilizes a cleaning fluid mixture that is non-azeotronic in order to generate essentially purified component A vapor upon heating the miscible liquid mixture at a temperature above the boiling point of component A. The component A vapor is generated via distillation, and accompanied by condensation to provide a vapor zone above the liquid mixture. The necessity for a non-azeotropic solvent mixture can be understood through consideration of a preferred embodiment of this invention, wherein component A is 2,2,3,3,3-pentafluoropropanol. The formation of essentially pure fluorinated alcohol vapor upon distillation of a mixture containing the liquid alcohol plus terpenes will ensure that air will not form a combustible mixture with the heated liquid phase containing terpenes. Azeotropic mixtures can contain sufficient quantities of auxiliary constituents in the vapor phase that, if present as combustible or flammable compounds, can be hazardous if a source of ignition is present and the flammability limit is exceeded.
The vapor density of the pentafluoropropanol in the preferred embodiment is substantially greater than air, allowing stability of the air/fluorinated alcohol interface with minimal air diffusion to the heated mixture containing combustible constituents. Furthermore, the operation of the compositions of matter containing terpene compounds is advantageous for minimizing air oxidation of the terpenes under heated conditions. Terpenes such as d-limonene and carene can undergo oxidation when heated in the presence of air. Antioxidants can be added to the compositions of matter disclosed herein to minimize terpene compound oxidation and decomposition. The non-azeotropic compositions of matter disclosed herein generate essentially pure alcohols upon distillation, such that only trace quantities of warm terpene vapors are generated. The result is enhanced thermooxidative stability of terpene compounds.
The constituents of the compositions of matter described in the present invention perform particular cleaning functions. The lower boiling point halogenated and non-halogenated alcohols are excellent solvents for polar and ionic contamination, such as salts and flux activators. The higher boiling point terpene compounds and N-methylpyrrolidinone are excellent solvents for non-polar and hydrophobic constituents, such as oils, grease, rosin and other solder paste additives. The heated cleaning fluid mixture contains a balance of solvency power for the flux residues typically found on wave soldered and surface mount assemblies. The lower boiling point, distillable alcohols generate a vapor phase above the heated solution that serves as a drying agent in the present invention. The alcohols can also be employed as rinsing agents within the vapor zone to remove the dirty, heated fluid mixture from the cleaned articles.
The individual components A and B possess certain physical properties that are desirable for maintaining the cleaning process of the present invention. The boiling point of component A must be substantially less than the boiling point or boiling point range of component B to ensure the distillate is essentially pure, such that headspace or "free board" above the heated liquid reservoir can be minimized. This is equivalent to a solvent distillation with minimal theoretical plates. In addition, the latent heat of vaporization of component A is sufficiently less than the other components to permit vaporization with minimal energy input. The greater vapor density of component A in comparison to air is essential for the reasons described earlier.
The compositions of matter of the present invention are utilized in a process for cleaning and defluxing printed circuit boards. The actual proportion of components A and B is determined by machine geometry and desired solvency characteristics. In practice, a sufficient quantity of component A (e.g. halogenated or non-halogenated alcohol) is required such that the cleaning apparatus headspace (or "free board") is filled with alcohol vapor when the liquid components A and B are heated. The headspace volume can be calculated if the solution height and condenser position are known. Moreover, some component A liquid is desirable in the heated solution to reduce the operating temperature to below 120° C., thereby minimizing solvent oxidation and shock to printed circuit boards. The volume of the non-azeotropic solvent mixture must be sufficient to permit immersion of the article to be cleaned.
Cleaning of printed circuit assemblies is effected by immersing the article in a heated mixture of components A and B. The temperature of the mixture is regulated so as to permit distillation of component A in an essentially pure form. Those skilled in the art of distillation will recognize that the heated mixture temperature must be greater than that of the pure component A boiling point as a result of boiling point elevation, but less than the component B boiling point. In practice, the heated mixture temperature is 5° to 15° C. greater than the component A vapor temperature. The temperature of the heated mixture that generates component A vapor is dependent on the ratio of component A to B in the mixture, as well as on the quantity of volatile matter. In general, component A diffusional losses must be compensated for by the introduction of pure component A liquid in order to maintain the heated mixture temperature within specified control limits. Thermostats and other temperature sensing elements are required in the cleaning apparatus for control purposes. The duration of exposure, through immersion, spray under immersion or other means, of the article to be cleaned is dependent on the nature of the post-soldering residues, the length of time after soldering and other factors.
The distilled component A is condensed above the level of the heated mixture, at a distance defined by machine geometry and required "free board", and allowed to return to the heated mixture. Alternatively, the condensate comprising essentially purified component A can be withdrawn to a separate tank for use in rinsing articles after immersion in the non-azeotropic heated mixture. The headspace containing essentially pure component A vapor is employed for either 1) drying the cleaned assembly for a given duration to remove liquid from the article, or 2) providing a vapor zone for rinsing using component A in purified form. The component A vapor provides an efficient medium for drying as the cleaned article leaves the heated solution mixture at a temperature greater than the vapor temperature, thereby facilitating the drying process. The article can be removed from the component A vapor zone after an appropriate time and tested for ionic cleanliness levels or sent to the next stage of manufacturing.
The condensate containing essentially pure component A can be employed alternatively for rinsing the article previously immersed in the heated, non-azeotropic solvent mixture in order to remove the higher boiling constituents containing flux and other soils. Rinsing can be performed via spraying or other means, and is conducted within the vapor zone so that the fluid can be collected after contacting the cleaned article through condensation, along with distilled component A. Drying after rinsing is effected by maintaining the cleaned article in the vapor zone and interrupting the flow of rinse solution.
The bottom of the apparatus, illustrated in the Figure, is filled with the non-azeotropic liquid mixture (103). The mixture is heated to a temperature greater than the boiling point of component A. The component A liquid will then vaporize into a layer (102) above the heated mixture (103). Component B, by virtue of its higher boiling point versus component A, will remain in liquid form below the vapor layer (102).
The assembly (104) to be cleaned is first placed in the heated mixture containing components A and B (103) by passing it through the vapor. Next, the assembly (104) is positioned in the vapor layer (102) where it can be sprayed with the condensate containing essentially pure component A (105) to remove the remaining contaminants. The condensate (105), when it strikes the assembly (104), will atomize. This atomization may present the risk of explosion if the atomized mist was exposed to the atmosphere. One purpose of the vapor (102), therefore, is to isolate the heated liquid (103) from the atmosphere.
The vapor (102) mixes with the atomized liquid mixture from the assembly being cleaned. This vapor mixture is then condensed by the condensing elements (101). The now liquid component A and B mixture is returned to the heated liquid mixture (103) below where the component A liquid is again vaporized to repeat the cycle. The condensing elements (101), therefore, retain the vapor (102) that, in turn, retains the heated liquid mixture (103).
Another function of the condensate containing essentially pure component A is to rinse off the solution that is contaminated with flux. Component A then evaporates more rapidly than component B due to its higher vapor pressure. The evaporation dries the assembly.
Alternatively, the assembly (104) can be positioned in the vapor layer (102) subsequent to immersion in the heated liquid (103) without being sprayed for the purpose of drying.
The following examples are included to illustrate the process of the present invention:
#1- A distillable cleaning solvent mixture was prepared by mixing 200 mL of a commercial pine-based terpene mixture (marketed under the tradename Reentry KNI 2000 by Envirosolv Inc.) and 50 mL of 2,2,3,3,3-pentafluoropropanol, wherein the mixture contains 30 wt % pentafluoropropanol. The solution was placed in a one liter beaker and fitted with a water-cooled condenser coil around the opening. The cleaning solvent mixture was heated to a temperature sufficient to distill the more volatile pentafluoropropanol component from the solvent mixture, generating a vapor zone between the solution and cold condenser coil boundaries. A thermometer indicated a solvent mixture temperature of 95° C. and a vapor zone temperature range of 83° C. to 86° C.
A printed circuit assembly that was wave soldered using a commercial, mildly-activated rosin flux was immersed in the warm solvent mixture for one minute in order to deflux the assembly. The board was raised above the solution level within the vapor zone and maintained for two minutes in order to dry the assembly. Upon removal from the vapor zone, the board was dry and free of flux residue as evidenced by optical microscopy.
#2- The mixture and process of Example #1 was employed to clean a board wave soldered with a commercially-available rosin flux. After immersion in the warm solvent mixture for one minute, the board was withdrawn and rinsed with essentially purified, distilled pentafluoropropanol liquid within the vapor zone above the solution level for the purpose of rinsing the solvent mixture (containing flux) from the assembly. The latter was then exposed to the essentially pure pentafluoropropanol vapor for drying the assembly. The board appeared dry and free of flux residue upon removal from the vapor zone.
#3- A mixture containing 60 mL of a commercial pine-based terpene mixture (marketed under the tradename Reentry KNI 2000 by Envirosolv Inc.) and 20 mL of 2,2,3,3,3-pentafluoropropanol was heated in a 250 mL beaker fitted with a water-cooled condenser around the opening. The solvent blend was heated to generate a vapor zone containing the essentially pure fluorinated alcohol with no odor of terpene. The liquid mixture and vapor zone temperatures were 87° C. and 81° C., respectively. A lighted match when dropped through the vapor zone into the warm fluid was extinguished while in the vapor zone of the non-flammable fluorinated alcohol.
The same experiment, when conducted without a fluorinated alcohol vapor blanket, led to burning and combustion of the terpene-based liquid.
In summary, the present invention utilizes a distillable, non-azeotropic solvent mixture for printed circuit assembly cleaning in order to adequately remove solder flux and other residues traditionally removed using CFC-based azeotropes. The mixture is suitable for use in batch degreaser cleaning equipment, and utilizes chemistry that is non-ozone depleting, yet effective at removal of polar and non-polar soils typically found on circuit boards after soldering. | A distillable, non-azeotropic solvent mixture for electronic assembly cleaning in order to adequately remove solder flux and other residues traditionally removed using CFC-based azeotropes. The mixture is heated to at least the boiling point of component A but less than the boiling point of component B. Component A vaporizes (102), forming a vapor layer above the mixture (103). Condensing elements (101) near the top of the cleaning apparatus condense the vapor (102), returning it to the heated mixture (103) to be vaporized again. The assembly (104) to be cleaned is lowered through the vapor and then immersed in the mixture (103) before being positioned in the vapor (102). | 2 |
BACKGROUND OF THE INVENTION
The present invention relates to the technical sector of remote control of inflation and deflation of a capacity from a source of gaseous fluid under relative pressure, and it more particularly relates to the remote control of the inflation pressure of the tires of automobiles and all terrain machines with wheels for industrial, agricultural, civilian or military uses,
In the preferred domains of application above, it is known that it is sometimes useful to be able to remotely control the inflation pressure of the tires of a vehicle, so that it is possible to adapt the supporting ability of these tires as a function of the state of the ground on which the vehicle is moving.
This is the case in particular for all-terrain vehicles which must be able to advance under the best conditions over hard, pebbled, loose ground surfaces capable of alternating, without the driver being obliged to stop in order to manually modify the inflation pressure of the different tires.
It is also the case for agricultural machines such as tractors, towed elements, self-propelled harvesters which, in addition to the problems of advancing in loose ground, must limit the packing of the ground and the formation of ruts in the fields, and handle transports on the road without deterioration of the tires.
These applications are only given as examples because in numerous domains, it also proves useful or even necessary to be able to adapt at a distance the inflation pressure of a certain capacity for containment of a gaseous fluid under relative pressure.
In order to solve this problem above, prior art offers some solutions.
Thus, French patent 9105351 describes a pneumatic valve which has a membrane which moves a cup which has a hole and a seat for a flap, a mobile apparatus of two flaps in opposition, respectively for inflation and outflow, which is sensitive to the position of the membrane, an elastic component which acts on the apparatus in order to maintain the inflation flap in closed position on the seat connected to the membrane, some elastic means associated with the membrane for maintaining the outflow flap in closed position on a seat arranged in the base of the valve, a stop which limits the course of travel of the outfit in opening of the outflow valve. The control of the deflation is ensured by a low positive pressure.
Such a valve partly corresponds to the desired function, but has limitations of use. In effect, the positive control pressure imposes a limit on the minimum pressures which are measurable and prohibits its use for the lowest pressures used on very loose terrain and in particular for agricultural work. Furthermore, its manufacturing which requires a large number of parts is delicate and expensive.
Another known proposal of prior art concerns a controlled pneumatic valve which is described in patent EP-0 296 017, valve which has a membrane connected to a flap automatically controlled and maintained between a half-body and a grooved ring which, with the half-body, delimits a control chamber, and with the grooved ring, delimits an outflow chamber, the latter communicating with a hole which opens in the capacity, the control chamber being subjected to a circuit of pressure-vacuum through a hose, said automatically controlled flap pushing the membrane to close the bore and coaxially incorporating a check valve. Such a valve gives satisfaction but has a certain number of disadvantages.
For example, in case of off-center mounting on the wheel, which is ordinarily imposed by the configuration of the hub, the centrifugal force acts on the ball of the check valve and interferes with closing of this valve at high speed, causing gradual deflation of the tire.
This valve is furthermore difficult to use for agricultural type vehicles with very negative pressures because of the lack of sealing of the check valve, the bearing forces which depend on the pressure held in the capacity not being sufficient to complete the contact between the ball and the seat of the flap.
The present invention aims to solve the problems mentioned previously by providing a simple and inexpensive device which is completely reliable and which can be used in a wide range of pressure and speed.
SUMMARY OF THE INVENTION
The invention therefore relates to a controlled pneumatic valve, intended for remote control of the inflation and deflation of a capacity, which has a membrane maintained between a body and a cover and which delimits a control chamber on the cover side and an outflow chamber on the body side, with it possible for the latter to be put in communication, according to the position of the membrane imposed by the control pressure, on one hand, with a pipe which is normally closed by a flap at rest, and opening into the capacity in the case of deflation, and on the other hand, can be isolated from the atmosphere by a tubular collar which at the same time allows passage of the gaseous fluid between the control chamber and the capacity in the case of inflation.
According to one characteristic, the valve has levers which are moved by a cup connected to the membrane, said levers resting on a stationary part of the cover or of the body, and bringing about the reversal of the direction of the force provided by the membrane during application of a negative pressure, thus ensuring the opening of the flap for isolation of the capacity under the action of a positive control pressure as well as a negative control pressure with respect to the surrounding pressure.
According to another characteristic, the levers are attached on a ring which holds them in position.
In a particular construction arrangement, the ring on which the levers are attached consists of a Belleville spring washer.
Advantageously, the levers are two in number, arranged symmetrically, and are part of the Belleville spring washer.
According to another characteristic, the stationary part on which the levers rest has a sealing ring which can close the annular pipe which connects the control chamber with the outflow chamber.
According to another characteristic, the end of the levers acts on a control rod of the outflow flap which has a maneuvering plate, and the orientation of the levers with respect to the surface of the maneuvering plate is such that, at the beginning of the deflation course of travel, one obtains a high lever arm ratio making it possible to limit the maximum negative pressure value necessary for opening the flap, while at the end of the deflation course of travel, the arm ratio decreasing, the movement of the flap is increased in order to obtain a large cross section of passage.
According to another characteristic, the control rod ensures the guiding of the flap.
The invention also relates to an installation for remote control of inflation and deflation of one or more capacities; which has, for each capacity, a single pipeline connecting the control chamber to two branches, leading respectively to a source of fluid under pressure or to a source of negative pressure, with it possible for said pipeline to be put in connection also with a pressure measuring means and a drain line leading to the open air. An advantage of the valve according to the invention lies in the possibility of being able to control, in complete safety, very low values of pressure, for example, as low as 2×10 4 Pa.
Another advantage lies in the ability to function at high speed on the vehicle, even in the case of mounting in off-centered position on the wheels.
Yet another advantage lies in the ability to easily balance the pressures of two or more capacities, each having one or more valves and controlled from a single pipeline.
Various other characteristics emerge from the description given hereafter in reference to the appended drawings which show some forms of execution of the invention as nonlimiting examples.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic view of an example of application of the object of the invention.
FIG. 2 is a vertical section showing the valve according to the invention according to a first embodiment.
FIGS. 3 and 4 are sections illustrating two particular phases of functioning of this first embodiment.
FIG. 5 is a partial view showing the shape of the levers and their attachment to the Belleville spring washer.
FIG. 6 is a vertical section similar to FIG. 2 , illustrating another embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Represented in FIG. 1 is a pneumatic valve according to the invention, designated by reference ( 1 ), which is applied to the control of the pressure of tire ( 2 ) represented partially and mounted on a wheel of an automobile which is not represented. Valve 1 attached in off-center position on the wheel disk is connected to the tire by pipe ( 3 ), and to a drive and control installation which has pressure-vacuum source by pipeline ( 4 ) in rotation with the wheel, rotating joint ( 5 ), circuit ( 6 ) attached on the axles or the chassis of the vehicle. Circuit ( 6 ) is capable of being put in connection, by the intermediary of isolation valve ( 7 ), with source ( 8 ) for supplying fluid under pressure. Circuit ( 6 ) can also be put in connection with negative pressure source ( 9 ). As an illustration, the source of fluid under pressure can be pneumatic tank ( 10 ), which is itself supplied by a compressor which is not represented, and the negative pressure source will, for example, be a Venturi type liquid jet vacuum pump ( 11 ) which can be supplied by pressure source ( 8 ) by means of pipeline ( 12 ) controlled by isolation valve ( 13 ), while another isolation valve ( 14 ) makes it possible to put circuit ( 6 ) in connection with the negative pressure generated by the venturi. The drain line necessary for ensuring the isolation of the capacity and eliminating pressure on rotating joint ( 5 ) can advantageously be brought about by the opening of valve ( 14 ), valves ( 7 ) and ( 13 ) being closed. The control circuit can act on several capacities alternately or simultaneously; pipe ( 6 ) is then subdivided into as many branches as there are capacities to be controlled, with it possible for each branch to be isolated and opened to the open air by a three way valve 16 , 16 bis, 16 ter.
According to FIG. 2 , device 1 has membrane ( 17 ) gripped between body ( 18 ) and cover ( 19 ). Membrane ( 17 ) makes it possible to delimit, with cover ( 19 ), a first cavity ( 2 O) called control chamber, and with body ( 18 ), another second cavity ( 21 ) called outflow chamber. The first cavity ( 20 ) communicates, through two inclined holes ( 22 ) and well ( 23 ), with pipe ( 6 ), while the second cavity ( 21 ) can communicate, on one hand, with the atmosphere through openings ( 24 ), and on the other hand, with capacity ( 2 ) through pipe ( 25 ).
The assembly of membrane ( 17 ) with body ( 18 ) and cover ( 19 ) can be ensured by any suitable means, such as screwing, crimping, welding.
Preferably, the device is produced in such a way to be present in the form of a body generated by revolution having a main axis x–x′which, facilitates the production of the constitutive parts by turning.
The device furthermore has base ( 26 ) provided with well ( 27 ) in which flap ( 28 ) is housed. The flap ( 28 ), is preferably a truncated cone, which, with the assistance of elastic element ( 29 ) closes pipe ( 25 ). Flap ( 28 ) is extended by push rod ( 30 ) which is itself provided with plate ( 31 ) on which levers ( 32 ) are supported.
Membrane ( 17 ) has, attached in its center, cup ( 33 ), mounted in a sealed manner on the membrane by any suitable means, and for example, by ring ( 34 ) pressed and crimped on the cup.
Cup ( 33 ) has hole ( 35 ) extended on the side of chamber ( 20 ) by conical neck ( 36 ) and on the side of chamber ( 21 ) by cooler ( 37 ).
Inside hole ( 35 ) the cup furthermore has groove ( 38 ) in which ring ( 32 a ) is housed. The ring ( 32 a ) is attached to the end of the levers ( 32 ).
Cover ( 19 ) has protuberance ( 39 ) which advances inside hole ( 35 ) and which, along with the hole, makes an annular pipe. This protuberance is provided, at a well determined level, with sealing ring ( 40 ) whose exterior diameter is suited to hole ( 35 ).
This protuberance is also drilled in its center with blind hole ( 41 ) which is capable of receiving the end of push rod ( 30 ).
In the position as illustrated in FIG. 2 , the so called rest position, the relative control pressure is zero, that is to say that circuit ( 6 ) is open to the open air, valves ( 7 ) and ( 13 ) being closed, with valves ( 14 ) and ( 16 ) open. Flap ( 28 ) closes pipe ( 25 ) by the action of elastic component ( 29 ), cup ( 33 ) attached to membrane ( 17 ) is in middle position between body ( 18 ) and cover ( 19 ); and under the action of the inherent elasticity of the membrane, and levers ( 32 ) maintained between maneuvering plate ( 31 ) and protuberance ( 39 ), the lip of sealing ring ( 40 ) is over hole ( 35 ), at the start of truncated conical neck ( 36 ).
In this position, the device establishes a sealed closure between capacity ( 2 ) and the surrounding environment.
In case of breaking of the drive pipeline during an inflation, deflation or measurement phase, control chamber ( 20 ) is again opened to the open air, and the isolation of capacity ( 2 ) is thus ensured as described above.
When it is a matter of inflating capacity ( 2 ), valves ( 13 ) and ( 14 ) are closed, valves ( 13 ) and ( 16 ) are open. Under these conditions, the pressure rises rapidly in chamber ( 20 ) up to a sufficient value to bring about the deformation of membrane ( 17 ) and the movement of cup ( 33 ) in the direction of valve body ( 18 ). Thus, as emerges from FIG. 3 , the pressure of the fluid coming from source ( 10 ) simultaneously brings about the resting of collar ( 37 ) on the bottom of valve body ( 18 ), then isolating outflow openings ( 24 ), and the opening of flap ( 28 ), due to the direct movement of push rod ( 30 ) by levers ( 32 ) resting without rocking on the exterior of plate ( 31 ).
Furthermore, sealing ring ( 40 ) moves away from neck ( 36 ), in that way allowing the fluid under pressure to run, with a small load loss, from control chamber ( 20 ) to capacity ( 2 ), traveling successively through the annular pipe arranged between hole ( 35 ) and protuberance ( 39 ), the interior of collar ( 37 ) and pipe ( 25 ).
In order to measure the pressure in capacity ( 2 ), it is sufficient, during an inflation operation, or after the beginning of inflation as described above, to close valve ( 7 ) so that the pressure is balanced between capacity ( 2 ) and pipe ( 6 ) because of the stopping of the flow of fluid and the corresponding load losses. The pressure can then be read on manometer ( 15 ) or recorded for processing with any other appropriate measuring means.
The stopping of an inflation operation is brought about by closing valve ( 8 ) and by opening valve ( 14 ). The relative pressure is then canceled in the control chamber, the membrane regains its rest position, and elastic means ( 29 ) simultaneously pushes back flap ( 28 ) to close pipe ( 25 ). The pressure coming from capacity ( 2 ) furthermore strengthens the closing and the seal of this flap.
For deflating capacity ( 2 ), valve ( 7 ) is closed, valves ( 13 ), ( 14 ) and ( 16 ) are opened. The negative pressure generated from liquid jet vacuum pump ( 11 ) is transmitted to control chamber ( 20 ), membrane ( 17 ) deforms and brings about the movement of cup ( 33 ) in the direction of cover ( 19 ) until stopping against it. As emerges in FIG. 4 , the movement of cup ( 33 ) brings about the resting of levers ( 32 ) on the exterior of protuberance ( 39 ) roughly at the level of the middle of said levers, bringing about the rocking of them. The free ends of levers ( 32 ) then come in contact with the edge of collar ( 37 ) and move push rod ( 30 ) to open flap ( 28 ).
During the movement of cup ( 33 ), sealing ring ( 40 ) remains in contact with hole ( 35 ) and closes the annular pipe arranged with protuberance ( 39 ) in order to maintain the negative pressure in control chamber ( 20 ) and isolate it from outflow chamber ( 21 ).
Thus, capacity ( 2 ) is put in connection with the atmosphere through chamber ( 21 ) and openings ( 24 ); collar ( 37 ) which moves away from the bottom of body ( 18 ) provides a large cross section of passage between pipe ( 25 ) and chamber ( 21 ) in order to obtain very rapid deflation.
Furthermore, the profiled shape of the bottom of maneuvering plate ( 31 ) promotes the flow of the fluid, limiting the turbulence and noise generated with outflow.
Stopping of the deflation is obtained by closing of valve ( 13 ); pipe ( 6 ) and control chamber ( 20 ) are then subjected to a zero relative pressure again; the elastic means pushes back flap ( 28 ) to closure and obliges push rod ( 30 , levers ( 32 ) and cup ( 33 ) to return to the rest position.
Represented in FIG. 5 is a top view of a form of execution of levers ( 32 ), of which there are preferably two, which are attached to Belleville spring washer ( 42 ), which has the advantage of maintaining the levers in a preferential rest position and of obtaining a spring effect with saddle curve. Consequently, the return to rest position after deflation is improved, while minimizing the value of the negative pressure which is necessary for opening of flap ( 28 ).
An execution variant of device 1 is represented in FIG. 6 , according to which protuberance ( 39 ) is no longer connected to cover ( 19 ) but rather to body ( 18 ) by two feet ( 43 ).
According to a variant which is not illustrated, levers ( 32 ) can be attached on protuberance ( 39 ) by hinge pins; the exterior ends of the levers are then free in groove ( 38 ) and are not connected to a ring.
The invention is not limited to the examples described and represented, since various modifications can be made to them without leaving the scope of the invention; in particular, the levers can be placed in the control chamber, can be actuated by washer ( 34 ) and act on an intermediate push rod resting on the maneuvering plate; the opening of flap ( 28 ) in inflation is then obtained by the action of fingers integrated in the cup, running out of hole ( 35 ) and resting directly on maneuvering plate ( 31 ). | The invention concerns a controlled pneumatic valve ( 1 ), for remote inflating and deflating of a capacity ( 2 ), comprising a membrane ( 17 ) maintained between a valve body ( 18 ), including orifices ( 24 ) and a cover ( 19 ); and defining with said cover a control chamber ( 20 ) and with the body an escape chamber ( 21 ), the latter being capable of being connected with the capacity ( 2 ) for deflation when the check valve ( 28 ) is thrust by levers ( 32 ) inverting the direction of movement of the membrane ( 17 ) sucked towards the cover ( 19 ). By the action of a pressure in the control chamber ( 20 ), the membrane ( 17 ), bearing a cup ( 33 ) with an annular conduit, moves towards the body ( 18 ), isolates the escape chamber ( 21 ), and opens the check valve ( 28 ) by direct thrust to perform inflation. The inventive device is particularly designed to control and adjust tire pressure. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is an U.S. national phase application under 35 U.S.C. §371 based upon co-pending International Application No. PCT/IT02/00454 filed Jul. 10, 2002. Additionally, this U.S. national phase application claims the benefit of priority of co-pending International Application No. PCT/IT02/00454 filed Jul. 10, 2002, Italian Application No. IT RM2001U000132 filed Jul. 13, 2001, and Italian Application No. IT Rm2002U000056 filed Mar. 27, 2002. The entire disclosures of the prior applications are incorporated herein by reference. The international application was published Jul. 29, 2004 under Publication No. WO 03/006323 A2.
TECHNICAL FIELD
The present invention relates to the field of food products' packaging, and specifically to a packaging designed to contain food products that are ready to be eaten or ready for preparation and that consist of two or more components to be mixed together before use.
For instance, the invention may be used to mix vegetables with their dressings, pasta with sauces or gravies, bread-crumbs % kith beaten eggs (for the preparation of omelettes), meat or fish with their coverings of bread-crumbs (for the preparation of fried dishes), and so on.
Therefore, the invention is not only useful for the final user, that is, for the person who will actually eat the food product, but could be employed in the kitchen of a restaurant, or in the domestic environment, in order to facilitate or speed up the preparation of food products that precedes their successive treatment (e.g. frying, cooking inside a microwave oven, etc.).
BACKGROUND ART
At present, there are known various kinds of packaging for ready-made food products, that are used both in the domestic and non-domestic environment. These kinds of packaging include a plastic-made container (receptacle) which is open uppwardly—like a bowl—, and which is completely wrapped by a sealing film of cellophane or the like.
The container has at least one compartment for a first food component to be seasoned, and at least a second compartment for small bags (sachets) containing a sauce or the like.
The user that has removed the external seating film (or possibly an upper cover of the container) opens one or more sachets available to him, after taking them from the respective compartment, and then pours their content in the compartment that contains the food product to be seasoned.
A drawback of such a packaging for food is that it is very easy to inadvertently pour the content of the small bags on one's clothes or on other objects, and therefore this operation is not very convenient and hygienic to carry out. Moreover, since the food to be seasoned usually occupies (due to space optimisation) the whole volume of its respective compartment (forming the greatest part of the volume of the packaging), the operation of seasoning the food product (e.g. salad) is very difficult, if not impossible to carry out, if one wants to avoid to pour (spread) the food product out of the already opened packaging.
Therefore, an object of the present invention is to provide a packaging for food, that allows to mix the various components of the food in a hygienic and efficient way.
The use of compartmented storage containers is known in the prior art. For example, European Patent Number EP 0790190; Great Britain Patent Number GB 2,211,479 A; U.S. Pat. No. 4,793,476.
DISCLOSURE OF INVENTION
The above objects are attained according to the claims, by means of a ready-made dish disposable packaging with several compartments:
an upwardly open container ( 1 ), an upper closure element (A) of the container ( 1 ), a compartment ( 2 ) of the container ( 1 ) for a first component of the food product, and at least an additional compartment ( 3 ) that is realised integrally with the container ( 1 ) or is rigidly fixed thereto in a non-removable manner, and which is used for an additional component of the food product to be mixed to said first component, said additional compartment ( 3 ), which is initially sealed, having movable members ( 13 , 14 ) that may be actuated by the user from outside the container ( 1 ) and which realise a communication path between the compartment ( 2 ) and said additional compartment ( 3 ), thereby allowing to mix the first component of food product, located inside the compartment ( 2 ), to the additional component of food product coming from the additional compartment ( 3 ), said movable members being formed by a base ( 13 ) of said additional compartment ( 3 ), that is connected by means of a hinge ( 15 ) to the walls ( 9 ) of the compartment ( 3 ), and said base ( 13 ) being movable between a first- or rest-position, and a second position, whereby during the displacement to the second position the base acts on a movable plug ( 14 ) which slides along the walls of said additional compartment ( 3 ); said plug ( 14 ) having lateral apertures which give rise to said communication between the compartment ( 2 ) and the additional compartment ( 3 ), in said second position of the movable base ( 13 ), when said plug ( 14 ) has reached a second, final position, without releasing itself from said walls ( 9 ) of the compartment ( 3 ).
The above objects are also attained by a combination between a disposable packaging for a first component of a food product, and a separate and sealed container ( 24 ) for a second component of the food product, in which:
the packaging comprises a container ( 1 ) with an upper closure element and a lower closure element, a compartment ( 2 ) for the first component of the food product in which said components are to be mixed together, and a coupling hole ( 11 ″) for the connection to said sealed separate container ( 24 );
the initially sealed container ( 24 ) has movable piston-like members ( 13 ′, 14 ) that are actuated by the user and realise a communication path between said compartment ( 2 ), and an additional compartment ( 3 ) defined by the separate sealed container ( 24 ) itself, after the removal of the lower closure element, after the mechanical coupling of the separate sealed container ( 24 ) to the coupling hole ( 11 ″), and lastly, after the actuation of said movable members ( 13 ′, 14 ), said movable members are formed by a base ( 13 ′) of said additional compartment ( 3 ), connected by a hinge ( 15 ′) to the walls ( 9 ′) of the compartment ( 3 ), and wherein said base ( 13 ′) is movable between a first- or rest-position, and a second position, and during the displacement to the second position the base acts on a movable plug ( 14 ) that slides along the walls of said additional compartment ( 3 ); the said plug ( 14 ) having lateral apertures which give rise to said communication path between the compartment ( 2 ) and the additional compartment ( 3 ), in said second position of the movable base ( 13 ′).
As disclosed in more detail, the movable members could also be designed to break the sealing means of the additional compartment, and form—for instance—a push rod or pointed rod having an oblique upper end, designed to break a sealing plastic/aluminium film of the additional compartment.
The pointed rod or push rod is preferably integrally formed with the container during the plastic moulding process.
The push rod has longitudinal channels in order to facilitate the leaking of the sauce, dressing, or the like, from the additional compartment.
The advantages of the present invention will result from the detailed description of its preferred embodiments.
BRIEF DESCRIPTION OF DRAWINGS
The present invention and its specific advantages will be described for purely illustrative and non-limitative purposes, with reference to the accompanying drawings, in which:
FIG. 1 is an axonometric view of the invention, corresponding to an embodiment of the present invention, without the upper sealing film or cover, and with the plug in the opening position;
FIG. 2 is a view similar to FIG. 1 , the plug being in the closure position;
FIG. 3 is a vertical sectional view of the invention shown in FIG. 1 and FIG. 2 , without the plug;
FIGS. 4 a and 4 b are vertical sectional views of the invention, corresponding to an embodiment of the present invention;
FIG. 5 is a view of a detail of the central portion of the container of FIG. 3 , with the plug in the closing position;
FIG. 6 is a view similar to FIG. 5 , the plug being in the opening position;
FIG. 7 is an axonometric view of the lower side of the packaging of FIG. 1 ;
FIG. 8 is a sectional axonometric view of the packaging, corresponding to an embodiment of the present invention;
FIG. 9 is a schematic view of a vertical section of the packaging shown in FIG. 8 ;
FIG. 10 is a schematic view in vertical section, analogous to FIG. 9 , in which, however, the additional compartment is located centrally in the packaging instead of laterally;
FIG. 11 is a vertical sectional view—enlarged with respect to FIGS. 9 and 10 —of the additional compartment containing the dressing or the like;
FIG. 12 is a view analogous to FIG. 11 , showing the use of the push rod for breaking and tearing the sealing film, corresponding to an embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The present invention will be described referring to FIGS. 1–7 .
Then, we will describe the embodiments of the present invention, with reference to FIGS. 8–12 .
In all figures the same reference number is used for an identical component of the packaging, so that the invention may be more readily understood.
The packaging essentially comprises a container 1 which for instance is obtained from a moulding process of plastics.
The configuration of the container 1 is such as to give rise to two separate compartments, denoted by 2 and 3 respectively. The compartment 3 is centrally located and has a cylindrical shape, while the greater compartment 2 , that surrounds the compartment 3 , has a substantially prismatic and polygonal shape with several congruent faces. Obviously, these shapes of the compartments are not limitative, and the same holds for the position of the compartment 3 , although for a more uniform distribution of the food product component contained in the compartment 3 towards the inside of the compartment 2 , containing the other component of the food product, the preferred position is the illustrated one.
The container 1 is formed by:
an upper flange 4 , on which a sealing film is applied (not shown), e.g. by heat sealing, ultrasonic welding, adhesives, or any other possible sealing method suited to close the open upper part of the container 1 ;
a side wall 5 with facets (or faces) having a polygonal horizontal section, the side wall terminating at its lower end in an annular projection 6 —also visible in FIG. 7 —;
an annular lower planar surface 7 —formed on said projection 6 —, to which a second sealing film is applied (not shown) by any known sealing method;
a base wall 8 , extending from the internal upper end of the annular projection 6 , to a cylindrical wall 11 ( 11 ″ in FIG. 4 a );
a movable base 13 ( 13 ′ in FIG. 4 a ) used to actuate a plug 14 , this movable base being connected by means of a hinge 15 ( 15 ′ in FIG. 4 a ) (of reduced thickness), to the cylindrical wall 11 (or 11 ′) of the compartment 3 , in order to reach a convex form when the plug 14 is made to slide inside the “boring” formed by the cylindrical wall 9 (or 9 ′).
Moreover, some pieces of cutlery (e.g. of plastics) or other fittings (e.g. napkins), or additives of the food product, may be received in the annular recess 10 and are retained from below by said film (not shown) which is applied on the planar annular surface of the annular projection 6 ( FIG. 7 ).
In an embodiment the container 1 is integrally formed (e.g. of moulded plastics). However, the plug 14 forms a separate piece (e.g. of plastics).
It must be stressed that the plug 14 has been omitted for clarity in FIG. 3 , to simplify the drawing, since it is shown in any case in the detailed views of FIGS. 5 and 6 . Actually, when the packaging is purchased by the user, it includes the plug 14 (in the closure position illustrated in FIGS. 2 and 5 ), the film applied on the upper side, that is on the upper annular flange 4 (or possibly a removable cover which is also omitted in the drawings), and the film applied on the lower side, that is on the annular planar surface 7 of the projection 6 .
To better understand the structure and operation (use modalities) of the packaging according to the present invention, reference will now be made in particular to the FIGS. 5 and 6 .
The latter figures are representations in vertical section, limited to the central portion of the container 1 , and in particular they show the cylindrical wall 9 of the compartment 3 which contains the sauce or dressing, the lower extension 11 of this cylindrical wall, the circular hinge 15 , and part of the base wall 8 . Moreover, the plug 14 is inserted (in the initial rest position of FIG. 5 ), inside the compartment 3 , and is in sliding engagement with the inner side of the vertical cylindrical wall 9 of this compartment 3 .
The movable base 13 for the actuation of the plug 14 includes centrally a cylindrical rib, or annular cylindrical portion 16 , that is integrally formed on the movable base 13 . Said circular rib 16 receives (e.g. by press-fitting) the lower portion of an axial stem 17 of the plug 14 . Moreover, the plug 14 has two circular peripheral grooves 19 a and 19 b , which are parallel to each other, and the upper end of the cylindrical wall 9 has a (inwardly directed) circular bead or ridge 20 complementary to the shape of the grooves 19 a and 19 b , adapted to engage with the upper groove 19 a in the closing position of the plug 14 ( FIG. 5 ), and with the lower groove 19 b in the opening position of the plug 14 ( FIG. 6 ).
The exact configuration of the plug 14 may be inferred—besides from FIGS. 5 and 6 —also form FIG. 1 . The plug 14 includes a portion shaped like a flanged disc 21 , whose circular flange 18 abuts on the upper end of the cylindrical vertical wall 9 , in the closure position of the plug 14 ( FIG. 5 ); the plug 14 also includes vertical elements 22 , shaped as small rods and extending downwards in a direction perpendicular to the plane of the flanged disc 21 , said vertical elements being integral with the latter. The vertical small rods 22 terminate at their lower end in a cylindrical ring 23 . The plug 14 is able to slide, by means of the external surfaces of its portions 22 and 23 , along the inner side of the cylindrical vertical wall 9 . Moreover, it may be noted that the various vertical small rods 22 of the plug 14 , are arranged at equal angles along the periphery of the flanged disc 21 that forms the upper part of the plug 14 . Thus, the small rods 22 delimit “windows” of equal dimensions, that are dearly visible in FIG. 1 , and which allow the leaking of the sauce or dressing from the compartment 3 , when the plug 14 is in the opening position ( FIGS. 1 and 6 ). In FIG. 1 the small rods 22 are at 90° with respect to each other.
First of all, the user of the packaging shown in FIGS. 1 to 3 , and 5 to 7 , removes the lower film, and then, he/she pushes inwardly the movable base 13 towards the inside of the packaging. The movable base lifts the plug 14 by means of the axial stem 17 , and at the same time it lifts the sauce or dressing contained in the compartment 3 immediately above the movable base 13 . During this operation, the circular ridge 20 —that realised a seal in the rest position of the plug 14 (see FIG. 5 ) thereby preventing the leaking of the sauce or dressing to the compartment 2 —disengages from the upper circular groove 19 a . In the upper position, or end-of-stroke position, of the plug 14 , the circular ridge 20 engages the second (lower) circular groove 19 b of the plug 14 , thereby realising again a sealing, so that the sauce etc. can flow only through the windows defined between the vertical small rods 22 . In the position shown in FIG. 6 , of the plug 14 , the movable base 13 will have an upwardly convex configuration.
In the preceding description it is assumed that the words “upper” and “lower”, and “upwards” or “downwards”, refer to the orientation of the packaging (and therefore of the container 1 ), that is shown for example in FIGS. 1 and 2 .
Without removing the cover (or the upper film), the user turns over the packaging in order to allow the complete downflow of the sauce, or dressing, or bread-crumbs, etc. through the “windows” or apertures formed between the small rods 22 . Then, the user shakes the packaging in order to perfectly and uniformly dress a salad, for instance.
At that time, if the food product (e.g. a salad) can be immediately eaten, the user simply removes the upper sealing film or an upper cover, and can directly use the compartment 2 as a bowl.
On the other hand, in case of a food product that must be fried, the user (in this case a cook) must tear the upper film and pour the content in a frying-pan or the like. However, in case of a microwave oven, it will be possible to directly employ the container 1 as a cooking container.
Therefore, it can be seen that the objects of the invention are fully attained. Particularly, it will be impossible to pour the seasoning out of the container 1 , since the upper film will not be removed, except when the seasoning operation is completed. Moreover, the sachets (small bags) of the prior art are totally superfluous, and the space inside the compartment 2 may be better used.
Now, we will describe an alternate embodiment of the packaging present invention, referring to FIGS. 1 , 2 , 4 a , 4 b and 7 .
In the embodiment, shown in FIGS. 4 a and 4 b , the compartment 3 is formed by a separate container 24 (or “cartridge”), that can be inserted, that is, press-fitted, in a central hole of the container 1 , having an inner diameter substantially equal to the external diameter of the separate container 24 . The separate container, indicated by a denser hatching, has a cylindrical wall 9 ′ with a downward extension 11 ′, and may be inserted inside a sleeve 11 ″ of the container 1 . From the details of FIGS. 4 a and 4 b , it can be seen that the downward projection 11 ′ is flanged at its lower end, and moreover it has an annular projection (ridge) acting as a retainer, in order to mutually lock the respective parts. Obviously, the flange acts as a stop, in order to stop the stroke of the separate container 24 towards the inside of the container 1 . The plug 14 is located (in the initial rest position shown in FIGS. 4 a and 4 b ) inside the cartridge 24 , and is in sliding contact with the cylindrical vertical wall 9 ′ of the compartment 3 .
The movable base 13 ′ for the actuation of the plug 14 has centrally a cylindrical rib, or cylindrical annular portion 16 ′, which is integrally formed on the movable base 13 ′ of the cartridge. Said circular rib 16 ′ receives (e.g. by press-fitting) the lower portion of an axial stem 17 ′ of the plug 14 . Moreover, the plug has two peripheral circular grooves 19 a ′ and 19 b ′, that are parallel to each other, while the upper end of the cylindrical wall 9 ′ has a (inwardly directed) ridge 20 ′, having a complementary shape with respect to the shape of the grooves 19 a ′ and 19 b ′, and adapted to fit inside the upper groove 19 a ′, in the closing position of the plug 14 ( FIGS. 4 a and 4 b ), and with the lower groove 19 b ′ in the opening position of the plug 14 (shown in FIG. 2 ).
The exact configuration of the plug 14 may be inferred, besides from FIGS. 4 a and 4 b , also from FIG. 1 . The plug 14 comprises a portion having the shape of a flanged disc 21 ′, whose circular flange 18 ′ abuts on the upper end of the vertical cylindrical wall 9 ′ of the cartridge or separate container 24 , in the closure position of the plug 14 (see FIGS. 4 a and 4 b ); the plug 14 also has vertical elements 22 ′, in the form of small rods, extending downwards in orthogonal direction to the plane of the flanged disc 21 ′, and being integral to the latter. The small vertical rods 22 ′ terminate at their lower ends in a cylindrical ring 23 ′. The plug 14 can slide, by means of the external surfaces of its portions 22 ′ and 23 ′, along the inner side of the vertical cylindrical wall 9 ′ of the separate container 24 .
Moreover, it can be noted that the various vertical rods 22 ′ of the plug 14 are arranged at equal angles along the periphery of the flanged disc 21 ′ that forms the upper part of the plug 14 . Thus, the small rods 22 form “windows” of equal dimensions, which are clearly visible in FIG. 1 , and which allow the leaking of the seasoning/dressing, etc., from the compartment 3 , when the plug 14 is in the opening position ( FIG. 1 ).
According to this solution, the final user can freely choose the seasoning/dressing he/she prefers, by independently purchasing a separate container 24 sealed by the respective plug 14 , and containing the desired type of seasoning, dressing or the like. Then, after having turned over the packaging, he/she removes the lower sealing film and inserts the separate container 24 (sealed by the respective plug 14 ) inside the hole of the container 1 , defined by the cylindrical sleeve 11 ″. Then, the user simply has to push the movable base 13 ′ inwardly, to the inside of the container 1 , and shake the packaging.
Also in this latter solution, the seasoning or the like cannot leak out of the packaging, since the upper sealing film (or the cover) is removed in the last step, that is at the end of the operation.
The invention has been described only for illustrative purposes with reference to its preferred embodiments. It goes without saying that various modifications may be conceived by a skilled person, within the same scope of protection.
For example, the number of compartments 3 is not limited to a single compartment, and if desired, more compartments could be provided if for the preparation of the food product it is necessary to mix together more than two components that must maintained in a separate state up to the preparation time.
Now, an alternate embodiment of the present invention will be described.
The embodiments are similar in that the compartment 3 does not form a separate element (in contrast with the cartridge 24 that can be inserted in the container 1 ), but is connected to the container in a non-removable manner.
With reference to FIGS. 8 to 10 , the packaging of the present invention essentially comprises a single container 1 a , which for instance is manufactured using a plastics moulding process. The configuration of the container 1 a is such as to give rise to two different compartments, indicated by the numerals 2 a and 3 a respectively. The first compartment 2 a , which has a greater size than the second compartment 3 a , contains the ready-made food product (schematically indicated by a hatching in FIG. 8 ), while the second compartment 3 a is used to introduce therein the seasoning, dressing, or the like (which is also schematically shown by a hatching in FIG. 8 ). Thus, the container 1 a forms a small bowl or small basin, of cylindrical external shape, and having inside it a second cylindrical body, which gives rise to the compartment 3 a for the dressing, seasoning, or the like.
It should be noted that the container 1 a is formed by a thin wall of plastics, that has been adequately shaped in the moulding process, said thin wall being horizontal at the base 8 a of the container 1 a , and vertical at the cylindrical external wall 5 a and at the cylindrical wall 9 a of the inner dressing's compartment 3 a.
The thin cylindrical wall 9 a extends upwards only for a reduced height as compared with the external cylindrical wall 5 a , and then it extends downwards so as to form a kind of “well”; the latter gives rise to the compartment 3 a that contains the dressing, or seasoning, or bread-crumbs, etc. Centrally, the compartment 3 a has a push rod or pointed rod 14 a , which internally is hollow, and is formed again by said thin wall of plastic moulding material. Thus, the container 1 a is really formed of a single moulded piece of plastics, consisting of a thin wall having the described configuration.
The push rod 14 a therefore forms an element having a shape like a frustum of a cone, which is internally hollow (see blind hole 14 b ), and which is itself formed by said continuous thin wall. Due to the presence of the push rod 14 a , the seasoning will occupy—inside the compartment 3 a —, an annular substantially cylindrical region, as may be clearly seen in FIG. 8 . The base 13 a of the seasoning compartment 3 a , having a bulged shape, is located at a level higher than the base 8 a of the compartment 2 a of the ready-made food product, as indicated by the double arrow F. The reason for this will be explained further below.
Even in this embodiment the seasoning or the like is stored separately from the ready-made food product, since a sealing film 14 c is provided at the upper side of the compartment 3 a and is applied laterally—on the circular step 20 a —. Moreover, the container 1 a is sealed at its upper end by a film A, or by a removable cover made of plastics or the like, that temporarily hermetically doses the container 1 a.
The only difference between FIGS. 8 and 9 , on the one hand, and FIG. 10 on the other hand, concerns the position of the compartment 3 a for the seasoning; in FIGS. 8 and 9 this compartment 3 a is located laterally, while in the version shown in FIG. 10 it is located centrally with respect to the base 8 a of the container.
Also in this case the object of the invention can be immediately recognised by the following description of its use.
When the packaging is still sealed, that is before removing the sealing film A from the upper part of the container 1 a , the user presses with his/her hand on the bottom 13 a of the seasoning's compartment 3 a , so as to deform the thin wall of the container at the location of this inner compartment 3 a , as shown in FIG. 12 . Consequently, the push rod 14 a will be lifted and will eventually pierce the closing film 14 c of the inner compartment 3 a . Without relieving this pressure, the user slowly turns over the packaging, in order to allow the complete downflow of the seasoning or dressing towards the inside of the compartment 2 a that contains the food products to be dressed (salad, other vegetables, etc.). Then, the user will simply have to shake the packaging to obtain a perfectly and uniformly dressed salad. At the end of this operation, the external film A (shown clearly in FIG. 8 ) will be detached. From the above description, it follows that in order to prevent an accidental piercing of the film 14 c that seals the compartment 3 a for the seasoning/dressing, during packing, transport and selling operations, it is necessary to provide a safety space (denoted by the double arrow F), that has already been mentioned without however clarifying its function.
For completeness, and referring again to FIGS. 11 and 12 , it should be noted that according to practical tests it results that the downflow of the seasoning/dressing from the compartment 3 a is facilitated by the presence of small channels on the lateral surface of the push rod 14 a used for piercing the closure film 14 c . Thus, the lateral wall of the push rod 14 a is recessed (“milled”) on diametrically opposite sides of the push rod, in such a way as to give rise to respective longitudinal channels, of half-cylindrical shape, which extend each as far as the upper end of the push rod 14 a ; this end is slanted in order to facilitate piercing of the film 14 c.
In FIG. 11 , the arrow P denotes the path of the air (directed towards the inside of the compartment 3 a ) after piercing of the film 14 c (see FIG. 12 ), whereas the arrow Q denotes the path of the seasoning/dressing or the like, that flows out of the compartment 3 a and reaches the adjacent compartment 2 a.
The advantages of the present invention are obvious to the skilled person. In fact, the packaging must be opened only shortly before the food product is eaten, and the system guarantees a perfect dressing.
Although the invention has been extensively described with regard to only some distinct—but specific—embodiments thereof, a skilled person may easily imagine several constructive modifications without thereby arriving at results out of the scope of protection conferred by this document.
The structure of the packaging may also be more complex. The container could—for instance—comprise a sealing and removable cover in lieu of the film A, and/or a sliding push rod 14 a which slides with respect to the base 13 of the compartment 3 a . All these modifications are obviously within the reach of the ordinary skilled person that has taken cognisance of the solutions proposed herein, and for this reason they are to be considered included in the present invention. | Disposable packaging, comprising a container ( 1 ) that defines a main compartment ( 2 ) and at least an additional compartment ( 3 ). The container ( 1 ) is bowl-shaped and is closed on the upper side by a film, or by a cover, in order to prevent the main food component contained inside the main compartment ( 2 )—from coming out. Moreover, the additional compartment ( 3 ) is closed by a slidable sealing system of the cylinder-piston type. In the closure position of the piston, which is formed by a plug ( 14 ), the food component contained in the additional compartment ( 3 ) cannot mix with the food component located in the main compartment ( 2 ), whereas in the opening position of the plug ( 14 ), the dressing/seasoning may leak from the additional compartment ( 3 ) through lateral apertures of the plug ( 14 ), at the time the user turns over and shakes the packaging. | 8 |
[0001] The present invention relates to a three dimensional (3-D) model comprising skin cells, the invention also provides methods of predicting immunogenicity/adverse immune reactions and hypersensitivity or allergic reactions to potential therapeutic compounds, biologics, cosmetics and chemical sensitizers using the 3-D model of skin cells. The methods provide an in vitro assay employing blood derived cells in the 3-D skin equivalent model and is of particular utility in the identification and prediction of skin sensitizers and in particular agents that may cause allergic contact dermatitis. The assay of the present invention provides inter alia methods of screening library compounds for sensitizing activity, identifying optimal therapeutics, ie efficacy testing especially but not exclusively, biological therapeutic products, such as: antibodies, e.g. monoclonal antibodies, antibody conjugates, Fc fusions; or proteins, and kits therefor.
BACKGROUND
[0002] The delayed-type hypersensitivity reaction of Allergic Contact Dermatitis (ACD) can be acquired when a sensitized individual later becomes challenged with the same small molecule. ACD manifests itself during the phase of elicitation; following penetration of the epidermis and acquisition/processing by an antigen presenting cell (APC)—a specialized cell within the skin, which presents the allergen or antigen to other cells known as T cells recruited by chemokines to the skin, causing their activation and the production of high levels of lymphokines. These molecules give rise to a secondary response with skin inflammation and keratinocyte (skin cell) apoptosis. Distinct from its near relative, Irritant Contact Dermatitis (ICD), which is caused by irritants (e.g. soap, detergents, perfumes etc) and which can affect anyone who succumbs to sufficient exposure, ACD is influenced by environmental and genetic factors and may take many years to manifest, long after initial contact. With approximately 20% of the general adult population believed to be allergic to one or more chemical sensitizers, and with a growing list of novel cosmetic and pharmaceutical products becoming available, ACD threatens to be an increasing future occupational and consumer health problem. Developing suitable and sensitive methods for the assessment of a chemical's potential to cause ACD will be a crucial step in combating this disease. As regards to drug allergies, these are rarely detected in non-clinical studies and are usually only observed in Phase 3 clinical trials or during commercialization when larger populations are exposed to the drug. Although the number of drugs that elicit allergic reactions is relatively low, the potential impact is very high due to the late stage of development in which it is detected. Therefore, non-clinical methods to predict for the potential to produce allergic or adverse immune reactions are needed to help in compound selection.
[0003] There is currently no safe cost effective way to assess the allergenicity of novel compounds. The Patch Test creates patient discomfort and can trigger anaphylactic shock. Anaphylaxis, a severe and potentially life threatening reaction occurs in approximately 17,800 of the population each year as a result of exposure to substances to which the sufferer is allergic.
[0004] Identifying chemicals that have the potential to induce hypersensitivity skin reactions is a mandatory component of new product discovery by pharmaceutical and cosmetic industries. Historically, predictive testing has exclusively relied on in vivo animal testing. In the traditional guinea pig test, the product is painted on the body and the guinea pig is then injected with an additional chemical to help accentuate the effect of the test chemical in developing dermatitis. Alternatively in the mouse ear swelling test, the mouse's ears are painted with the test substance and its immunological response is determined by examination of lymph node tissue. However, with an EU ban on animal testing being implemented in March 2013, there is a pressing need for the development of alternative predictive in vitro and in silico techniques. Although it is known from the prior art to gage up and/or down regulation of gene products such as cytokines these assays are laborious and results are inconsistent. No validated in vitro model currently exists to predict immunogenicity and hypersensitivity or allergic reactions to potential therapeutic compounds, including monoclonal antibodies, cosmetics and chemical sensitizers.
[0005] 3-D full thickness human skin models have been used for many years in toxicity testing. Current 3-D models use either: (i) keratinocytes and fibroblasts (derived from the epidermis or dermis respectively) from excess skin from plastic surgery patients or (ii) immortalised cell lines. In either instance, the cells are heterologous, and therefore cannot be truly predictive of a specified individual's response to a skin sensitizer or an allergic reaction. Indeed such assays tend to give a proportionately large number of false negatives.
[0006] There is therefore a need for an in vitro 3-D skin equivalent model and use of the model in an assay to discriminate between sensitizers and non-sensitizers and/or allergens and non-allergens for predicting the sensitizing nature of novel pharmaceutical, biologics, cosmetic and chemical products. There is a need for a simple, robust, cost-effective, accurate assay for testing novel compounds for hypersensitivity, allergic reactions and immunomodulatory capabilities.
[0007] There is especially a need for an autologous 3-D equivalent human skin model for use in personalised medicine and allergy/adverse immune reaction testing.
BRIEF SUMMARY OF THE DISCLOSURE
[0008] According to a first aspect of the invention there is provided a three dimensional (3-D) skin equivalent model, the model comprising a scaffold capable of supporting and maintaining a population of cells, wherein the cell population comprises autologous keratinocytes and fibroblasts derived from a skin biopsy sample.
[0009] Preferably, the skin biopsy sample is a scrape biopsy comprising a strip or square of skin or is a punch biopsy sample of approximately 4 mm in area and 2 mm in depth. It will be appreciated that the autologous dermally derived fibroblast and epidermally derived keratinocytes are prepared from the skin biopsy sample. More preferably, the biopsy sample is taken from a human subject. However, it will be appreciated that it is also possible that other mammalian species for which allergy testing in a veterinarian setting is required are equally applicable.
[0010] The present invention advantageously, by using scaffolds, surprisingly allows smaller numbers of cells to be ‘seeded’ for 3-D model development, it has been shown that sufficient cells can be generated from these very small biopsies for seeding on scaffold surfaces. The small size of the biopsies is particularly ideal in order to use the assay for a personalised medicine approach to therapy and testing of monoclonal antibody or immunomodulatory efficacy.
[0011] In one embodiment the scaffold comprises a tissue engineered collagen support although Alvatex® (Reinnervate Ltd) which is a highly porous polystyrene scaffold is also suitable. In an alternative embodiment the scaffold may comprise a native/natural acellular or decellularised collagen or collagen-like mesh or honeycomb. Any suitable scaffold may be used in the present invention providing that it possesses the appropriate characteristics of pore structure, pore size, ability to support cells and permit their invasion, infiltration, migration and proliferation.
[0012] In an alternative embodiment of the invention the 3-D skin equivalent model may also be seeded with additional cell populations also derived from the same biopsy sample.
[0013] According to a second aspect of the invention there is provided a method of preparing a 3-D skin equivalent model, the method comprising:
(i) isolating autologous keratinocytes and fibroblasts from a skin biopsy sample; (ii) storing the isolated keratinocytes; (iii) seeding a scaffold with the isolated fibroblasts under culture conditions and allowing a sufficient period of time to permit production of an extracellular matrix; (iv) seeding the scaffold comprising the fibroblasts with the keratinocytes; and (v) culturing the seeded scaffold under appropriate conditions.
[0019] It will be appreciated that keratinocytes and fibroblasts are isolated from the same skin sample.
[0020] Preferably, culturing steps are under flow conditions.
[0021] The method of preparing the 3-D skin equivalent model of the invention advantageously results in a product that has increased longevity up to 5 months or so over a skin biopsy sample.
[0022] According to a third aspect of the invention there is provided an in vitro method for identifying chemical compounds that are sensitizers or for discriminating between chemical compounds that are sensitizers and non-sensitizers, the method comprising:
(i) preparing a donor blood sample so as to isolate a population of T cells and monocyte-derived dendritic cells therefrom; (ii) incubating the monocyte-derived dendritic cells with a test compound; (iii) incubating the compound treated monocyte-derived dendritic cells with a population of T cells isolated in step (i); (iv) incubating the mixed T cell and compound treated monocyte-derived dendritic cells with a 3-D skin equivalent model that comprises keratinocytes and fibroblasts isolated from an autologous biopsy sample obtained from the same donor; and (v) assessing hypersensitivity and allergic reactions by graded histological changes in the 3-D skin equivalent model as compared to a control.
[0028] Preferably, the T cells and monocyte-derived dendritic cells (DCs) are isolated from peripheral blood mononuclear cells (PBMC). For example and without limitation, the T cell and monocyte-derived dendritic cells may be separated from PBMC by magnetic activated cell sorting or similar techniques. Preferably, the dendritic cells are either standard or fast matured dendritic cells.
[0029] Preferably, the first incubating step of step (ii) is for between 2 to 24 hours. Typical incubation conditions are carried out at 37° C. in a humidified 5% CO 2 air incubator, a typical culture medium is Roswell Park Memorial Institute 1640 (RPMI 1640, Gibco UK) containing 100 IU/ml penicillin, 100 μg/ml streptomycin (Gibco UK) and 2 mM L-glutamine (Gibco UK) supplemented with 10% v/v heat inactivated foetal calf serum (FCS, Sera Lab). or Ex Vivo (Gibco UK) serum free medium. The culture conditions are non-limiting in so far as other variations in conditions that allow for growth and maintenance of the cells are equally applicable.
[0030] Preferably step (ii) further includes, as a control incubating a further or second set of monocyte-derived dendritic cells with a compound that is a known non-sensitizer. Alternatively the control may be monocyte-derived dendritic cells incubated with no additional chemical compounds at all.
[0031] Preferably, the second incubating of step (iii), comprising incubating DCs with a population of T cells isolated in step (i) is for between 3-7 days using the same culture conditions as for step (ii) except that 10% heat inactivated autologous serum, human AB serum, or an equivalent thereof is used and replaces foetal calf serum. In the instance where a control comprises DCs with a population of T cells isolated in step (i) having been exposed to a non-sensitizer, this further or second set of cells is incubated in identical conditions to the test mixture.
[0032] Preferably, the third incubating step of step (iv), comprising incubating the mixed T cell and DCs cells with an autologous 3-D skin equivalent model biopsy sample, prepared according to the second aspect of the invention, is for between 1 to 3 days. In the instance where a control comprises DCs having been exposed to a non-sensitizer, the cells are incubated with the 3-D skin equivalent model in identical conditions to the test mixture.
[0033] Preferably, the step of assessing hypersensitivity and allergic reactions in the 3-D skin equivalent model by graded histological changes comprises assessment of vacuolisation of epidermal cells, damage to basal keratinocytes and connection between the epidermis and dermis. In one embodiment of the invention, the histological Grades are I to IV, wherein grade I is negative and Grades II to IV are varying degrees of positive. Preferably, Grade I is defined as the skin biopsy showing very mild vacuolisation of epidermal cells, Grade II is defined as the skin biopsy showing diffuse vacuolisation of epidermal cells, Grade III is defined as the skin showing cleft formation between the epidermis and dermis caused by confluent vacuolar damage to basal keratinocytes and Grade IV is defined as the skin showing the complete separation of the epidermis and dermis. FIGS. 1 a - 1 d illustrate the histologically graded damage. Alternatively another grading system may be used.
[0034] Preferably, the control value may be derived from the group comprising:
(i) a further or second set of monocyte-derived dendritic cells that have been incubated in step (ii) with a compound that is a known non-sensitizer; (ii) a further or second set of monocyte-derived dendritic cells that have been incubated in step (ii) with no additional chemical compounds; (iii) a 3-D skin equivalent model that has been incubated with autologous lymphocytes; or (iv) a skin 3-D skin equivalent model that has been incubated with compound alone at the same concentrations as that used in step (ii).
[0039] Preferably, the test compound value is compared to the control value so that an increase or decrease from the control value is indicative of a sensitizing reaction.
[0040] According to a fourth aspect of the invention there is provided an in vitro method of identifying chemical compounds that are sensitizers or non-sensitizers and/or allergens or non-allergens, the method comprising:
(i) separating a population of monocyte-derived dendritic cells from a donor blood sample comprising a population of T cells; (ii) incubating the monocyte-derived dendritic cells with a test compound; (iii) incubating the compound treated monocyte-derived dendritic cells of (ii) with the separated donor blood sample of (i); (iv) determining the level of T cell proliferation and/or IFN-γ expression in the sample of (iii), wherein the level of T cell proliferation and/or IFN-γ expression correlates with a defined grade of histological change observed in a 3-D skin equivalent model, prepared according to the second aspect of the invention, treated with said test compound; and (v) comparing the level of T cell proliferation in the sample with the level of T cell proliferation in at least one control sample treated with a control sensitizer compound and at least one control sample treated with a control non-sensitizer compound and/or at least one control sample treated with a control allergen compound and at least one control sample treated with a control non-allergen compound; or (vi) comparing the level of IFN-γ expression in the sample with the level of IFN-γ expression in at least one control sample treated with a control sensitizer compound and at least one control sample treated with a control non-sensitizer compound and/or at least one control sample treated with a control allergen compound and at least one control sample treated with a control non-allergen compound, wherein comparison of T cell proliferation and/or IFN-γ expression in the sample with T cell proliferation and/or IFN-γ expression in the control samples identifies the test compound as a sensitizer or non-sensitizer and/or an allergen or non-allergen.
[0048] By comparing the level of T cell proliferation and/or the level of IFN-γ expression induced by a test compound to levels induced by a sensitizing and non-sensitizing control compound (or allergen or non-allergen control compound), the method allows prediction of the sensitizing capability of the test compound. The use of sensitizing and non-sensitizing control compounds (or allergen or non-allergen control compound), advantageously provides thresholds values for sensitizing and non-sensitizing and/or allergic and non-allergic levels of T cell proliferation and IFN-γ expression.
[0049] Preferably, the level of T cell proliferation determined in (iv) correlates with a defined grade of histological change observed in a 3-D skin equivalent model treated with said compound. More preferably, the level of T cell proliferation in the 3-D skin equivalent model treated with said compound correlates with an LLNA class observed in a LLNA mouse model treated with said compound.
[0050] Preferably, the level of IFN-γ expression determined in (iv) correlates with a defined grade of histological change observed in a skin explant treated with said compound. More preferably, level of IFN-γ expression in the 3-D skin equivalent model treated with said compound correlates with a LLNA class observed in a LLNA mouse model treated with said compound.
[0051] Preferably, each of said control compounds is administered in a concentration such that at least 70% of treated cells remain viable 24 hours after exposure to the compound. More preferably, at least 75% of treated cells or at least 80% of treated cells remain viable 24 hours after exposure to the compound. Still more preferably, 85, 90 or 95% of treated cells remain viable 24 hours after exposure to the compound.
[0052] Preferably, the percentage of viable cells is determined using a cell viability assay.
[0053] Preferably the cells of the cell viability assay are peripheral blood mononuclear cells, more preferably blood mononuclear-derived monocytes, and more preferably monocyte-derived dendritic cells.
[0054] Preferably, the level of T cell proliferation is determined by [ 3 H] thymidine incorporation. Alternative methods of measuring T cell proliferation include flow cytometric assessment and by an enzyme-linked immunoabsorbent assay (ELISA) based on bromo- 2 ′-deoxyuridine (BrdU) incorporation.
[0055] Preferably, IFN-γ expression is determined by flow cytometry. Alternative methods of measuring IFN-γ production can be by ELISA, ELISPOT and real-time RT-PCR.
[0056] Preferably, the dendritic cells are either standard or fast matured dendritic cells.
[0057] Preferably, the first incubating step of step (ii) is for between 2 to 24 hours. Typical incubation conditions are carried out at 37° C. in a humidified 5% CO 2 air incubator, a typical culture medium is Roswell Park Memorial Institute 1640 (RPMI 1640, Gibco UK) containing 100 IU/ml penicillin, 100 μg/ml streptomycin (Gibco UK) and 2 mM L-glutamine (Gibco UK) supplemented with 10% v/v heat inactivated foetal calf serum (FCS, Sera Lab). or Ex Vivo (Gibco UK) serum free medium. The culture conditions are non-limiting in so far as other variations in conditions that allow for growth and maintenance of the cells are equally applicable.
[0058] Preferably, the incubation of step (ii) comprises incubation with 10% heat inactivated fetal calf serum.
[0059] Preferably, the second incubating of step (iii) is for between 3-7 days. Preferably, the second incubating of step (iii), comprising incubating DCs with a population of T cells isolated in step (i) is for between 3-7 days using the same culture conditions as for step (ii) except that 10% heat inactivated autologous serum, human AB serum, or an equivalent thereof is used and replaces foetal calf serum. In the instance where a control comprises DCs with a population of T cells isolated in step (i) having been exposed to a non-sensitizer, this further or second set of cells is incubated in identical conditions to the test mixture.
[0060] Preferably, the incubation of step (iii) comprises incubation with 10% heat inactivated autologous serum, human AB serum, or an equivalent thereof serum.
[0061] Preferably, the control sample comprises a further or second set of monocyte-derived dendritic cells that have been incubated in step (ii) with the control compound(s). More preferably, said further or second set of monocyte-derived dendritic cells are separated from the donor blood sample of step (i). Alternatively the control may be monocyte-derived dendritic cells incubated with no additional chemical compounds at all.
[0062] According to a fifth aspect of the invention there is provided an in vitro method for detecting allergic reactions to a monoclonal antibody or monoclonal antibody biosimilars therapy, the method comprising using the 3-D skin equivalent model of the first aspect of the invention incubated with autologous peripheral blood derived mononuclear cells or reactive cells from a mixed lymphocyte reaction in the presence of the monoclonal antibody or monoclonal antibody biosimilars and comparing a reaction to a control value.
[0063] According to a sixth aspect of the invention there is provided an in vitro method of assessing efficacy of a biological therapeutic product, the method comprising using the 3-D skin equivalent model of the first aspect of the invention incubated with autologous peripheral blood derived mononuclear cells or reactive cells from a mixed lymphocyte reaction in the presence of the biological therapeutic product and comparing a reaction to a control value, and repeating the method over a period of time.
[0064] A number of chimeric, human and humanised monoclonal antibody products have received FDA approval for use in disease states including cancer, cardiovascular disease, systemic lupus erythematous, transplant rejection, macular degeneration, psoriasis, auto-immune disorders and rheumatoid arthritis. A number of new biological therapeutic products are in development, and all require extensive testing prior to clinical trial and release onto the market, there is currently no known assays for assessment of monoclonal antibody allergenicity. However, the 3-D skin equivalent model of the present invention and the methods of the present invention provide the first real predictive assay for such therapeutic products and offer immediate advantage to the pharmaceutical industry, patients and clinicians alike.
[0065] Preferably, the method of assessing biological therapeutic product is for selecting an appropriate biological therapeutic product, e.g monoclonal antibody therapy for an individual suffering from a disease selected from the group comprising cancer, cardiovascular disease, systemic lupus erythematosus, transplant rejection, macular degeneration, psoriasis, auto-immune disorders and rheumatoid arthritis.
[0066] According to a seventh aspect of the invention there is provided a method of treating an individual suffering from a disease selected from the group comprising cancer, cardiovascular disease, systemic lupus erythematosus, transplant rejection, macular degeneration, psoriasis, auto-immune disorders and rheumatoid arthritis, the method comprising using the 3-D skin equivalent model of the first aspect of the invention in a method according to the fifth or sixth aspect of the invention to select biological therapeutic product to which the patient will respond without a side effect of allergenicity.
[0067] According to a eighth aspect of the invention there is provided a kit comprising a scaffold onto which keratinocytes and fibroblasts may be seeded, a means for separating monocytes from a blood sample and instructions for use thereof. More preferably, said means for separating monocytes comprises a CD14 + cell separation kit and at least one control sensitizer compound and at least one control non-sensitizer compound and/or at least one control allergen compound and at least one control non-allergen compound.
[0068] Preferably, the kit further comprises a means for standard or fast dendritic cell maturation and instructions for use thererof.
[0069] Preferably, that at least one control sensitizer compound and at least one control non-sensitizer compound and/or at least one control allergen compound and at least one control non-allergen compound of the kit are located in defined positions on a solid support. More preferably, said solid support is a 6, 12, 24, 48 or 96 well plate.
[0070] Preferably, the kit comprises at least two control sensitizer compounds, wherein said compounds are DNCB and NiSO4.
[0071] Preferably, the kit comprises at least two control non-sensitizer compounds, wherein said compounds are Triton-X and ZnSO4.
[0072] Still more preferably, the kit comprises at least two control sensitizer compounds, wherein said compounds are DNCB and NiSO4 and at least two control non-sensitizer compounds, wherein said compounds are Triton-X and ZnSO4.
[0073] Features ascribed to any aspect of the invention are applicable mutatis mutandis to all other aspects of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0074] Embodiments of the invention are further described hereinafter with reference to the accompanying drawings, in which:
[0075] FIG. 1 shows histopathological changes for different grades of skin graft versus host reaction (GVHR); FIG. 1A shows Grade I skin GVHR showing very mild vacuolisation of epidermal cells (Negative reaction); FIG. 1B shows Grade II skin GVHR showing diffuse vacuolisation of epidermal cells (Positive reaction); FIG. 1C shows Grade III skin GVHR showing cleft formation between the epidermis and dermis caused by confluent vacuolar damage to basal keratinocytes (Positive reaction) and; FIG. 1D shows Grade IV skin GVHR showing the complete separation of the epidermis and dermis (Positive reaction).
[0076] FIG. 2 shows 3D skin equivalent sections that have been formalin fixed. Sections were paraffin embedded, sectioned and stained with haematoxylin and eosin.
DETAILED DESCRIPTION
[0077] Reference herein to “scaffold” means any 3-D structure either native/natural or tissue engineered that is capable of supporting cell migration, cell infiltration and/or cell proliferation.
[0078] Reference herein to “autologous” means that the blood derived products and skin explants are derived or collected from the same individual.
[0079] Reference herein to a “sensitizer” includes any chemical compound or chemical agent or antibody that causes a substantial proportion of exposed people or animals to develop an allergic reaction in normal tissue after single or repeated exposure to the said compound, antibody or chemical agent.
[0080] Reference herein to an “allergen” and “allergenic” includes any foreign substance such as an environmental substance or chemical that is capable of inducing allergy or a specific hypersensitive reaction in the body. Common allergens include plant pollens, spores of mold, animal dander, house dust, foods, feathers, dyes, soaps, detergents, cosmetics, plastics, and drugs. Allergens can enter the body by, for example, being inhaled, swallowed, touched, or injected.
[0081] Reference herein to a “chemical compound” is intended to include a chemical, therapeutic, pharmaceutical, biologic, antibody or cosmetic agent, substance, preparation or composition.
[0082] Reference herein to a “biologic” is intended to include a preparation, such as a drug, a vaccine, serum or an antitoxin, that is synthesized from living organisms or their products and used as a diagnostic, preventive, or therapeutic agent.
[0083] Reference herein to “biological therapeutic products” includes, but is not limited to, antibodies, e.g. monoclonal antibodies, antibody conjugates, Fc fusions; or proteins or protein based therapeutics.
[0084] We have previously shown that following incubation of chemicals with blood derived dendritic cells or mononuclear cells with monoclonal antibodies then interaction with T cells (in the first instance for chemical sensitisation) and then with skin in the second phase of the reaction it is possible to observe a histopathological damage read out. The prejudice in the art was that it was only possible to show skin sensitisation or allergy to chemicals or other allergies using skin dendritic cells. The prejudice arises from the fact that far fewer dendritic cells can be obtained from skin biopsies than can be prepared from monocytes in whole blood. In the present invention, with improved technology to enable 3-D skin equivalent models to be developed, we provide for the first time an autologous 3-D skin equivalent model that surprising comprises less cells, with increased longevity that can be used as a robust and accurate system for detecting allergic and sensitizing reactions.
[0085] The present invention conveniently provides a 3-D skin equivalent model of autologous mammalian skin cells that can be used in an in vitro assay and methods which allows for the study of primary and secondary immune responses in the presence of potential sensitizing compounds thereby advantageously reducing the need for extensive animal testing.
[0086] The present invention conveniently provides a 3-D skin equivalent model of autologous mammalian skin cells from a specified individual that can be used in an in vitro assay to assess that individual's response to a particular chemical compound or therapeutic agent and also to monitor the efficacy of any treatment regime.
[0087] The present invention is of particular utility to an individual who is about to receive antibody or biologic therapy, in particular but not exclusively an individual suffering from chronic rheumatoid arthritis who is to receive antibody therapy. The present invention will allow a clinician to assess which antibody therapy will be tolerated and which antibody therapy may cause an allergic reaction. It is envisaged that the problem associated with unpredictable allergic reactions to antibody therapy will be overcome by the use of the 3-D skin equivalent model of autologous skin cells of the present invention.
[0088] The ability to grown whole skin models from constituent cells rather than individual punch biopsy sample has many advantages. For example, using a single sample of skin tissue to create an autologous 3-D skin equivalent model with extended longevity it will be possible to use the 3-D model in multiple tests over a period of months rather than a single sample for use in only one assay. The 3-D skin equivalent model is viable over many months rather than weeks in the standard skin biopsy model. It is envisaged that a further advantage is that culturing under flow conditions will achieve a faster cell culture with increased proliferation rates and improved cell viability which will not only reduce the time taken and cost of testing but will also permit repeated dose testing for allergenicity. Using the longer viable 3-D skin equivalent model of the present invention will enable the efficacy of therapy to be assessed over time without the requirement for a further skin biopsy sample being taken from an individual, the only further requirement being a peripheral blood sample. This is of benefit to the individual undergoing the test as it will minimize any pain due to taking of a biopsy sample.
[0089] The products and methods of the present invention are unique and gives insight into the use of a blood based assay on a 3-D autologous skin equivalent model for predicting response to chemical sensitizers and to investigate their potential allergic/inflammatory signals. The present invention provides a blood based assay and 3-D skin equivalent model that improves on the current techniques and provides a novel means of testing novel drugs for hypersensitivity and allergic reactions.
[0090] The product and assay of the present invention provides the advantage over a heterologous three dimensional skin equivalent model as it uses blood with autologous immune cells and autologous skin cells enabling immune responses to be studied and cellular and molecular targets identified thus aiding in drug discovery, improving drug design and optimisation for drug dosage prior to a clinical trial.
[0091] Viability Assay
[0092] A dye exclusion method can be used to investigate cell viability. It is based on the principle that live cells possess intact cell membranes that exclude certain dyes, such as trypan blue, eosin, or propidium, whereas dead cells do not. Cells are treated with different concentrations of the test substance for a period of 24 hours. Cells are harvested and an aliquot of the cell suspension is mixed with trypan blue (1:1) and then visually examined to determine whether cells take up or exclude dye. The trypan blue chromopore is negatively charged and cannot react with a cell unless the cell membrane is damaged, therefore a viable cell has a clear cytoplasm whereas a non-viable cell has a blue cytoplasm. A total of 100 cells are counted. The unstained (viable) and stained (non-viable) cells are counted separately using a haemocytometer and viability recorded. By culturing cells in the presence of the test reagents any adverse effect of the reagents on cell viability can be observed. Cell viability of 70% or more is regarded as adequate for the methods of the present invention. Preferably, the cell viability is 75% or more or 80% or more.
[0093] Preparation of Peripheral Blood Mononuclear Cells (PBMC)
[0094] Peripheral Blood Mononuclear cells (PBMC) from blood obtained from healthy volunteers was prepared by density-gradient centrifugation using Lymphoprep™ solution (Axis-Shields) and diluted 1:1 in Earle's balanced salt solution (EBBS) (Sigma). Mononuclear cells were collected from the density medium:plasma interface and washed in cold PBS and counted using an Improved Neubauer cell counting chamber (Weber Scientific International Ltd., UK). Cell viability was assessed by trypan blue (Gibco).
[0095] Separation of CD14+ Monocytes using the MACS® Technology
[0096] The MACS® (Magnetic-activated cell sorting) technology (Miltenyi Biotec) uses columns filled with magnetic particles to separate magnetically labelled cells. For the separation process these columns are placed in a strong magnetic field (QuadroMACS® separator). Required amount of PBMC were transferred to a fresh 50 ml falcon tube, topped up with PBS and strained through a 100 μm nylon filter to remove any clumps. A maximum of 100×10 6 mononuclear cells were washed and re-suspended in cold MACS buffer (PBS containing 0.5% FCS and 1 mM ethylene diamine tetracetic acid (EDTA) resusupended in 80 μl buffer/10×10 6 cells. The cells were incubated at 2-8° C. for 20 minutes with 10 μl/10×10 6 cells CD14 antibody coupled with magnetic microbeads. The cell suspension was added to the column allowing the negative cells to pass through for collection (as the “T cell” fraction and the positive cells (CD14+) were then collected and assessed for purity by flow cytometry analysis.
[0097] Generation of Monocyte-Derived Dendritic Cells (moDC)
[0098] CD14 positive monocytes purified by MACS® separation were cultured in a 24 well plate at a density of 0.5×10 6 /ml in culture medium with 50 ng/ml GM-CSF and 50 ng/ml IL-4. After 3 days 400 μl of the medium were carefully removed and 500 μl fresh medium containing 50 ng/ml GM-CSF and 50 ng/ml IL-4 (Immunotools) were added and left for a further 3 days. After 6 days immature antigen presenting cells dendritic cells (DC) were either collected or allowed to mature by adding lipopolysaccharides (LPS) (0.1 μg/ml, Sigma), IL-1β (10 ng/ml, Immunotools) and TNFa (10 ng/ml, Immunotools) for a further 24 hours.
[0099] Generation of Mature Fast DC
[0100] CD14 positive selection cells were put into culture (0.3-0.5×10 6 cells per well in 24 well plate) with RP-10 medium supplemented with IL-4 (50 ng/ml) and GM-CSF (50 ng/ml). After 24 hours maturation cytokines TNF-α (10 ng/ml), IL-1β (10 ng/ml), IL-6 (10 ng/ml), 1 uM PGE2, Resiquimod (2.5 μg/ml), CD40L (1 μg/ml) and LPS (0.1 μg/ml) were added to each well for a further 24 hours.
[0101] T Cell Proliferation Assays
[0102] Mature Fast DC treated and untreated with compounds as well as cells from both allogeneic and autologous sources in triplicate at a ratio of 1:10 (DC:T cells) in (200 μl total volume) in 96-well round-bottomed plates for 5 days at 37° C. in a humidified 5% CO 2 in air incubator. After 5 days, 40 μl of supernatant was removed from the top of each triplicate well and stored at −20° C. for further cytokine analysis. [ 3 H]-Thymidine (used at a concentration of 3.7 MBq/ml) was then added to each well using appropriate radiation protection methods and allowed to incubate for 16-18 hours at 37° C. in a humidified 5% CO 2 in air incubator. Cells were harvested and subsequently counted using the 1450 MicroBeta TriLux Microplate Scintillation and Luminescence Counter (PerkinElmer®). Data was interpreted using Graphpad Prism® software.
[0103] Skin Biopsy
[0104] Sections from a 4 mm wide 2 mm deep skin punch biopsy were obtained from an individual. Ideally the skin punch biopsy is obtained from an area of medium skin thickness and low innervations so as to cause as little discomfort as possible to the individual. Autologous keratinocytes and fibroblasts are separated from the biopsy sample
[0105] Generation of Keratinocytes and Fibroblasts
[0106] Autologous keratinocytes and fibroblasts were generated from a 4 mm punch skin biopsy, the skin biopsies were incubated with dispase (final concentration 1 mg/ml) at 4° C. overnight. Following the incubation dispase was removed by washes then the epidermis was peeled from the dermis using sterile forceps. The epidermis was used for generating keratinocytes and dermis used for generating fibroblasts. The epidermis was incubated at 37° C. with Trypsin/EDTA and dermis incubated with collagenase (100 U/ml) to release the keratinocytes and fibroblasts from the tissue matrix into the supernatant. The cells were collected from supernatants following centrifugation. Collected keratinocytes and fibroblasts were cultured with appropriate medium in a 48 or 24 well culture plate as passage 0. The medium used for growing keratinocytes is EpliLIfe™ (Life technologies) and for fibroblasts is Dulbecco's Modified Eagles Medium (DMEM) (Sigma) “containing 100 IU/ml penicillin, 100 μg/ml streptomycin (Gibco UK) and 2 mM L-glutamine (Gibco UK) supplemented with 10% v/v heat inactivated foetal calf serum (FCS, Sera Lab) respectively. Both keratinocytes and fibroblasts would adhere to the plastic surface and have a monolayer growth. The cells were fed twice a week till they reached approx 80% confluence. Then the cells were removed from the culture wells using Trypsin/EDTA. The cells were then collected, washed and reseeded into a larger tissue culture well or a flask as passage 1 to expand further on for example 12 or 24 well scaffold inserts. The cells have been expanded up to passage 3 to obtain 0.5-2×10 6 cells. The successful rate of generating keratinocytes from punch skin biopsies is 60%.
[0107] The skin explant assay consisted of co-incubating the treated and untreated DC cells with T cells from the same donor for 7 days. After this time the T cells are added in 96 well plates or 12 or 24 well inserts to sections of the 3D human skin equivalent model. The skin equivalent model is co-incubated for three days and then routinely stained for histopathology. 3-D skin equivalent models incubated with medium alone or autologous cells alone are used as controls. The 3-D skin equivalent model is then routinely sectioned and stained for graded histopathological damage using a criteria which is very similar to that used and observed in the clinical setting with distinct pathological damage.
[0108] In the present invention DC response to chemical sensitizers versus known non-sensitizers can be assessed by their effect on sensitized cells by assessment in vitro of graded skin damage.
[0109] 3-D Skin Equivalent Model Culture
[0110] Human dermal fibroblasts isolated from dermis of the skin are seeded onto a scaffold and cultured for 3 weeks to allow production of the extracellular matrix (ECM). Keratinocytes from the same piece of skin are isolated (0.5-5×10 6 ) and cryopreserved and at 3 weeks thawed and seeded onto the scaffold, raised to the air-liquid interface, and assessed for growth over 2-5 months. To aid differentiation and growth and use of cell flow conditions at a rate of 100-500 ul/min to increase longevity is also employed.
[0111] Processing Skin
[0112] Preparation of 3T3 Cells
[0113] 3T3 cells (3T3-J2 strain (ATCC# CCL-92)) were grown as feeder cells for keratinocytes. 3T3 cells were grown in 3T3 medium (DMEM supplemented with 10% new-born calf serum, 1% Penicillin-Streptomycin-Fungizone). 3T3 cells were maintained in sub-confluent culture to prevent spontaneous transformation. Medium was replaced every 3-4 days. A flask of 70% confluent 3T3 cells treated with Mitomycin-C (0.4 μg/ml) for 2 hours at 37° C. was prepared before processing epidermis.
[0114] Processing Skin
[0115] Skin was washed and cleaned with PBS and fat removed leaving a thin layer of epidermis and dermis. Skin was then incubated overnight with Dispase (1 mg/ml) at 4° C. The next day skin was removed from the well and epidermis peeled backusing forceps.
[0116] Processing Epidermis
[0117] A flask of 70% confluent 3T3 cells was prepared in advance of processing the epidermis. The peeled epidermis was incubated for 5 minutes at 37° C. with Trypsin/EDTA (T/E). After 5 minutes a serological pipette was used to disrupt the tissue and release cells into the supernatant. Trypsin/EDTA was neutralised by adding 200 ul FCS and 10 mis PBS. Epidermis was removed with a tip and discarded. Supernatant was centrifuged at 500 g for 5 minutes. Supernatant was discarded and the cell pellet resuspended in 20 ml pre-warmed F-Media. 3T3 medium was removed from 3T3 cells treated with mitomycin-C, rinsed X2 with PBS and the resuspended pellet in F-Media was added to the flask. Cells were grown until keratinocytes became visible. Keratinocytes were then removed from the 3T3 cells by trypsination and further cultured in EpiLife medium until the required numbers of cells (2×10 6 ) were acquired. Cells should be between passages 0-3.
[0118] Processing Dermis
[0119] The remaining dermis (after the epidermis peel) was cut into square pieces using a scalpel and placed in to 3 mls RF10 and collagenase enzyme (100 U/ml) and incubated overnight at 4° C. The next day tissue was disrupted using a serological pipette. The supernatant was passed through a cell strainer (100 micron) and centrifuged at 500 g for 5 minutes. The cell pellet was re-suspended in 1 ml DMEM (DMEM+Glut+P/S+20% FCS). Cells were cultured until the required numbers of fibroblasts (0.5×10 6 ) were acquired. Cells should be between passages 0-7.
[0120] 3D Skin Equivalent Model
[0121] Alvetex Scaffold Preparation
[0122] Alvetex was soaked in 70% ethanol for 5 minutes and washed twice in 8 mls DMEM for 2 minutes each. Alvetex was then placed into a 6 well plate.
[0123] Adding Fibroblasts to Alvetex Scaffold
[0124] Fibroblasts were grown to maximum of passage 7 in DMEM to 70% confluence. Fibroblasts were trypsinised with T/E (2 minutes at 37° C.). Cells were centrifuged as before and 0.5×10*6 cells were removed and placed in 100 ul volume DMEM. Fibroblasts were added to the centre of the scaffold. The plate was incubated for 3 hours to allow the cells to attach to the scaffold. The well was then flooded with 8 mls DMEM. Medium was replaced every 2 days for at least 21 days. After 21 days, fibroblast monolayer (dermis) was formed and ready for the addition of keratinocytes.
[0125] Adding Keratinocytes to Alvetex Scaffold
[0126] Keratinocytes were grown to maximum of passage 3 in Epilife to 70% confluence. Keratinocytes were then trypsinised with T/E (2 mins at 37° C.). Cells were centrifuged as before and 2×10*6 cells were removed and placed in 100 ul volume F-Media. Media was removed from the well containing the Alvetex scaffold and keratinocytes were added to the centre of the scaffold. The well was flooded with 4 mls F-Media. The plate was incubated for 3 hours to allow the cells to attach to the scaffold. The well was then flooded with another 5 mls F-Media. The plate was incubated for 3 days. After 3 days medium was removed and replaced with 4 mls F-Media to allow cells exposure to air-surface interface. Medium was replaced every 2 days for at least 14-18 days. After 18 days, 3D skin equivalent was cut out of the plastic holder and formalin fixed. Sections were paraffin embedded, sectioned and stained with haematoxylin and eosin as shown in Fiigure 2 .
[0127] Throughout the description and claims of this specification, the words “comprise” and “contain” and variations of them mean “including but not limited to”, and they are not intended to (and do not) exclude other moieties, additives, components, integers or steps. Throughout the description and claims of this specification, the singular encompasses the plural unless the context otherwise requires. In particular, where the indefinite article is used, the specification is to be understood as contemplating plurality as well as singularity, unless the context requires otherwise.
[0128] Features, integers, characteristics, compounds, chemical moieties or groups described in conjunction with a particular aspect, embodiment or example of the invention are to be understood to be applicable to any other aspect, embodiment or example described herein unless incompatible therewith. All of the features disclosed in this specification (including any accompanying claims, abstract and drawings), and/or all of the steps of any method or process so disclosed, may be combined in any combination, except combinations where at least some of such features and/or steps are mutually exclusive. The invention is not restricted to the details of any foregoing embodiments. The invention extends to any novel one, or any novel combination, of the features disclosed in this specification (including any accompanying claims, abstract and drawings), or to any novel one, or any novel combination, of the steps of any method or process so disclosed.
[0129] The reader's attention is directed to all papers and documents which are filed concurrently with or previous to this specification in connection with this application and which are open to public inspection with this specification, and the contents of all such papers and documents are incorporated herein by reference. | A three dimensional (3-D) model comprising a scaffold and autologous skin cells, the invention also provides methods of predicting immunogenicity and hypersensitivity or allergic or adverse immune reactions to potential therapeutic compounds, biologies, cosmetics and chemical sensitizers using the 3-D model of skin cells. The methods provide an in vitro assay employing autologous blood derived cells in the 3-D skin equivalent model and is of particular utility in the identification and prediction of skin sensitizers and in particular agents that may cause allergic contact dermatitis. The assay of the present invention provides inter alia methods of screening library compounds for sensitizing activity, identifying optimal therapeutics, especially but not exclusively, monoclonal antibodies and kits therefor. | 6 |
TECHNICAL FIELD
[0001] The present invention relates to an access device for pets, particularly for dogs and cats, according to the preamble of claim 1 . By access device in this context are meant, in particular, access devices having doors of a type through which the pets can transit. In principle, however, this term shall also include access devices through which the pets can reach appropriate installations or spatially delimited zones e.g. for food uptake.
PRIOR ART
[0002] Special access devices for pets, particularly for dogs and cats have existed for a long time. These satisfy the need to enable such animal to have independent access to the living zone of an apartment or a house without the need for direct assistance by a person. Such access devices usually comprise a pivotable flap with an upper suspension or a swinging door.
[0003] However, a problem with such access devices is that wild animals, animals that turned wild but also extraneous animals and even predators such as foxes etc. can obtain access. This shall be avoided. Several solutions for this have been suggested in the available art, but all of these appear to have drawbacks.
[0004] US-A-2004/0163316 just discloses a lockable pet door that has all the features that are needed mechanically but that does not support the identification of admissible pets and discrimination of other animals.
[0005] From US-A-2003/0204996 is known an access control wherein a trapdoor is opened by a remote controller. The mechanical arrangement of the trapdoor is rather disadvantageous. An individual access control without intervention of an operator is not contemplated in US-A-2003/0204996. The only possibility to keep out extraneous pets is provided by a timer control which locks again the door automatically after an access.
[0006] From US-A-2002/0011217 is known a pet door with which the pet shall wear a collar that will automatically activate a reed switch and shall open a flap door. This does not provide for an individual access control. Wild animals not wearing such a collar could indeed be kept out. However, an access is possible for any animals wearing a corresponding collar with a magnet that can activate the reed switch. A similar collar solution is known from U.S. Pat. No. 5,872,516, in which a communication by ultrasound is suggested.
[0007] U.S. Pat. No. 5,992,096 proposes a solution with a flap door, according to which a collar detector sends back an individual signal upon query from a reader unit, whereupon the flap mechanism is opened—by taking into account the signal of a movement detector. A similar access door—albeit without a movement sensor—is known from U.S. Pat. No. 6,141,911, which also relies on a temporarily limited opening of the door. In contrast, according to U.S. Pat. No. 6,297,739 B1 an identification sensor is further coupled to a weight sensor so that with the two sensors an unwanted access by non-authorized pets is made difficult.
[0008] On the other hand, US-A-2004/0113796 discloses a sliding door that also works with an RFID identification sensor but is preferably intended to be subsequently mounted in a window.
[0009] These devices may be suitable for the access of a specific individual animal. However, the problem remains that the individualized access doors need to be programmed in such manner that access is allowed to a single animal but not to other animals—be they extraneous pets, animals that turned wild or even wild animals. It is conceivable that on the factory level an identification transmitter is assigned to a very specific identification carrier, that is, e.g., to a collar. However, this solution appears to have little flexibility. Finally, if access shall be provided to a plurality of animals, all the systems known from the art described above reach their limits.
[0010] In the meantime, it is usual e.g. in case of a veterinary treatment but also for legal reasons to implant an RFID transponder to all the pets of a given kind. It would thus be desirable if an RFID transponder that has already been implanted in a pet for other reasons or possibly just for the purpose of access control could also be used for an access control. Of course, it would be possible to equip the access door with an input device for inputting an acceptable code, e.g. a multi-digit number or a bar code. However, it would be a substantial effort if an access device for pets had to be equipped with such an input device.
DESCRIPTION OF THE INVENTION
[0011] It is an object of the invention to provide an access device with individualized access for pets, particularly for cats, that gives access to an individual animal or to a plurality of animals without the need of a complex device for inputting the code of a transponder that is implanted in the animal or attached to the animal.
[0012] The object of the invention is attained by an access device according to claim 1 . The provisions of the invention readily lead to the result that access and exit through the door is made possible individually for the selected pet or for a group of pets, whereas the door remains locked otherwise. Additional access to one or several pets can be provided without the need for manual input of any data. Also, there is no need for additional equipment.
[0013] Advantageous embodiments are defined in claims 2 to 6 .
[0014] The invention may be used advantageously if the reader device for transponders in the neighborhood does not need to be constantly in operation in order to search the neighborhood for pets, but rather if the electronic device is in a partly active standby mode. By means of a touch sensor or an approaching sensor that may be configured as a simple switch at the door but also as a movement sensor like in U.S. Pat. No. 6,297,739 B1, the transponder operation becomes activated so as to establish whether the previously detected contact of the door-flap was triggered by an admitted pet (claim 2 ). Particularly in this case, an operation with a non rechargeable battery or a rechargeable battery is possible (claim 3 ).
[0015] In special cases it may be advantageous if the door is open in one direction independently of the electronic identification, e.g. to allow an animal to leave a protected region anytime and independently of the identified transponder. In other cases, it can be advantageous if the door is closed in one direction independently of the electronic identification, e.g. to allow keeping an animal locked in after its return (claim 4 ). Furthermore, it can be advantageous to allow leaving a protected region anytime and independently of the identified transponder.
[0016] Also advantageous is a manual lock that will function independently of the identified transponder to either lock the door firmly (claim 5 ) or keep the same permanently open (claim 6 ), so as to be preventive regarding e.g. a possible power failure upon which the animal would be unintentionally locked in.
[0017] The embodiment as pet bell, according to which an admitted passage is signaled by a signal tone, is advantageous. This function can also be achieved optically, preferably by means of a light signal (claims 7 and 8 ). The connection between the door and the signaling device can be configured conventionally as a cable, but also as a transmitting device.
[0018] According to claim 9 it is contemplated that in case of a power failure the locking mechanism may be selectively overwritten by a release in one direction, preferably to enable leaving the inner region, or in both directions. This allows one to ensure that in case of a power failure the animal does not stay locked in and, as the case may be, that it has access to e.g. food. However, it is also possible to have the door completely locked, e.g. if there is no pet and thus the access mechanism shall stay closed.
[0019] The previously mentioned elements, as well as those claimed and described in the following working examples, which shall be used according to the present invention, are not subject to any specific exceptions in respect of their size, shape, material use and technical conception, so that the selection criteria known in the respective application fields can be applied without limitation.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Further details, advantages and features of the object of the present invention follow from the following description of the associated drawings which serve to explain—in the form of working examples—the doors according to the present invention. The drawings show:
[0021] FIG. 1 a representation of an access device from the front side according to a working example of the present invention;
[0022] FIG. 2 the installation of the access device according to FIG. 1 in a wall with a thickness of 5 mm;
[0023] FIG. 3 the installation of the access device according to FIG. 1 in a wall with a thickness of 40 mm; and
[0024] FIG. 4 the installation of the access device according to FIG. 1 in a wall with a thickness of 300 mm.
MODES FOR CARRYING OUT THE INVENTION
[0025] The access device for pets denoted by 2 as a whole in FIG. 1 in this working example has a constitution which is particularly useful for cats, but also for dogs and other pets such as e.g. rabbits, turtles, guinea pigs etc., and it can be installed into a wall but also in a normal door, a window, etc.
[0026] The access device has a door constituted by a flap 4 hanging at a horizontally disposed hinge, which flap is fixed to a frame 6 through the hinge. The flap is arranged in such manner as to be flippable upwards to both sides, thereby providing access. An electronic board 8 arranged in the frame 6 primarily controls the locking system 10 . However, the latter can also be controlled manually by keeping the flap constantly locked or constantly open. It is possible to have the constantly open or locked state for one direction. In the present working example, the locking mechanism 10 exhibits a turn knob that in its various positions allows or requires an electrical release. On the access device this is subsequently displayed on display 14 , which in the working example consists of two LEDs.
[0027] In the working example, the electronic board is supplied with electric power from a rechargeable battery, the rechargeable battery 22 being charged by means of an external power supply 18 . The power supply is connected with the access device by means of plug 20 .
[0028] It is important for the invention that the electronic board 8 comprises a reader device for transponders that reads out the code from a transponder chip located in the vicinity of the reader unit and compares the code with a list stored in electronic board 8 . Alternatively, the reader unit can also be arranged separate from the electronic board, e.g. if required by spatial constraints. The reader unit is connected with an antenna device 24 that communicates with the transponder. Advantageously, the transponder will be implanted in a pet, but it is also possible to carry the transponder e.g. on a collar or attach the same to an ear.
[0029] Initially, the list stored on the electronic board 8 is empty, i.e. no access admission has been granted to any pets as initial setting. In order to grant admission to a pet having a corresponding, so far unknown transponder, the pet can be placed in the influence range of the antenna. By actuating the simple switch 12 designed as a push-button, the transponder code of the transponder arranged at or within the pet is read in and added to the list of admitted pets. The entry is confirmed with a signal of display 14 (blinking). In a next approach of this pet, upon comparison with the stored list this particular pet will be recognized and admitted according to the preset permissions (unidirectional or bidirectional admission). Hence, the locking mechanism 10 will be opened insofar as its turn-knob is set to allow for an electrical opening.
[0030] However, according to the present working example, in case of a power failure the locking mechanism can be overwritten by a release at least in the outbound direction, optionally also in the inbound direction, so that the pet is not permanently trapped in case of power failure.
[0031] In the present working example, the access device 2 further comprises an approach sensor 16 . This is because for reasons of saving electrical power the reader device shall remain inactive until the approach sensor 16 detects an object in its proximity. Only then will the electronic circuitry be switched on and the process of reading and comparing the read in transponder code with the list be carried out and a decision be reached concerning the admission of the pet carrying the transponder. Alternatively, instead of the approach sensor 16 , a touch sensor can be built into the flap of the access device then requiring that the animal tries to pass through the door, and only thereafter triggering the reading process by this touch sensor. However, the function is the same.
[0032] As shown in FIGS. 2 to 4 , the access device can be installed in walls of very different thickness from less than 5 mm up to more than 30 mm, because antenna 24 is always arranged at the outside and the flap itself does not shield the radio waves of the reader device.
LIST OF REFERENCE NUMERALS
[0000]
2 access device
4 door
6 frame
8 electronic board
10 locking system
12 push-button for admission
14 indicators for the locked state
16 touch sensor
18 power supply
20 plug
22 rechargeable battery
24 antenna
26 wall | In order to provide for a simple identification of admitted pets in an access device ( 2 ) for pets, particularly for dogs and cats, wherein the releasing and locking of the door ( 4 ) can be controlled by means of an electronic device ( 8 ), it is proposed to configure the electronic device ( 8 ) in such manner that any radio frequency controlled identification devices (RFID) located in proximity to a reader device can be included into the accession list by an input to a simple switching device ( 12 ). | 4 |
FIELD OF THE INVENTION
The present invention relates to instructional systems for industrial environments and more particularly to a thin client solution for deploying educational systems utilizing existing computer and communication infrastructure.
BACKGROUND OF THE INVENTION
Many industrial environments have a requirement for deploying information through a computing medium without replacing computer and networking hardware. This need is perhaps greatest felt in manufacturing facilities striving for flexibility and classrooms where environmental considerations and budget constraints dictate the reuse of existing networking and computer equipment. IBM and Apple have been very active in this marketplace offering various educational solutions that utilize CD ROM technology to provide effective multimedia educational platforms for schools and factories.
The present invention relates to a computer-based teaching system employing networking and computer assisted interactive techniques for enhancing a teacher's efficiency and effectiveness in a classroom. As will be discussed below, among its various attributes, the inventive system enables a teacher:
(1) to monitor progress of a class more closely during each classroom session, and over each section of a course, than has been possible in the past;
(2) to stimulate active participation by all students in a class;
(3) to automate rollkeeping and the giving and grading of quizzes and homework; and
(4) to utilize instructional videos and associated peripheral hardware interactively with the system. The invention thus integrates computers into the mainstream of the learning and grading process at educational institutions, with significant benefit to the classroom environment, including facilitated knowledge of student performance, and associated savings in routine paperwork.
There have been numerous techniques devised for enabling a teacher to more easily convey information and understanding to a class, and ultimately to relieve the teacher, to the greatest extent possible, of a number of the burdens associated with conveying that information to the class. Various electronically-based techniques have been implemented, but these have proved to be quite limiting or otherwise disadvantageous. In one sense, the techniques have been limiting in that interaction between the student and the teacher may be limited to responses to multiple-choice type questions, or to questions requiring only numerical answers. Examples of such systems include those described in U.S. Pat. Nos. 3,656,243; 3,694,935; 3,716,929; 4,004,354; 4,785,472; 5,002,491; 5,176,520; 5,303,042; 5,590,360; 5,812,668; and 5,815,657. Such systems have been further limiting in that they have not provided any way of keeping accurate, detailed records for individual students for the duration of a given class.
Other more recently-proposed systems have taken advantage of advances in technology to interconnect a number of students in the same classroom, or in different classrooms, for purposes of gathering information, or facilitating access to instructional programs. One example is U.S. Pat. No. 4,636,174, which enables students to download instructional programs from a central computer, which acts as a sort of file server. In this system, the student, rather than the teacher, has control over system access and operation.
Another example is U.S. Pat. No. 4,759,717, which discloses detailed networking structure for connecting conventional personal computers. However, there is at most only limited teacher-student interaction contemplated. Rather, this system is directed more toward providing, at a central location, an instructional program which may be downloaded locally so that students can learn various types of computer programs. Yet another example of a conventional student response system is U.S. Pat. No. 4,764,120. This system is intended to collect data of a limited nature (e.g., responses to multiple-choice questions) from a number of classrooms. There is no provision of statistical analysis to inform the teacher of how well a class is learning the concepts being conveyed. This feature also is absent from the other two just-mentioned U.S. patents.
One of the important services an electronically-based classroom teaching system can provide is to enable a teacher to monitor progress of the class and of individual students, and to focus effort in areas where students seem to have the most trouble understanding the concepts being taught. An electronic classroom teaching aid also should assist a teacher in breaking through the reluctance that students have to participating actively in class. Some of this reluctance derives from basic shyness, or fear of seeming different, or fear of seeming superior (or less intelligent, for that matter). Enabling students to respond individually and confidentially by electronic means to questions posed by the teacher can help to break through some of the shyness or reluctance a student otherwise may exhibit.
However, this confidentiality by itself does not suffice to satisfy all students, at all levels, in all teaching situations. Sometimes active participation and motivation can be encouraged better by combining students in small teams (by twos or threes) and requiring that they respond to questions as a team. In this way, students can learn from the insights and difficulties of their peers. The teacher can infer class progress from the responses of the teams. In still other situations it is important to enable students to proceed, if possible, in a self-paced manner, to learn concepts conveyed in the classroom, while still having the teacher present to monitor the situation and to concentrate in areas where the class seems to be having difficulty. Here, it is important that the interactive electronic classroom system advise the teacher, as soon as possible, what percentage of the class grasps the concepts being taught. Certain of the above-mentioned U.S. patents, such as U.S. Pat. No. 4,004,354, describe systems which provide the teacher with a readout of the percentage of students answering a question correctly. However, the types of questions still are limited to multiple choice, and do not provide a vehicle for further discussion and exploration of concepts which appear to be difficult to grasp.
It is desirable to have a system in which students could respond to a wider range of questions, with different types of responses required (for example, a narrative response of limited length). It also is desirable to enable a student to take a quiz at his or her own pace, with questions requiring answers other than multiple choice or simple numerical answers. Further, it is desirable for students to be able to run short didactic programs which are designed to enable students to experiment immediately and actively with the concepts which are being taught in that class, and which simultaneously give feedback to the teacher. Those students who have succeeded in a task may be assigned more advanced work while others may receive remedial instruction. It follows that different portions of a class should be able to work at one time, on different tasks, under control and supervision of the teacher. Such a system would be in complete contrast to conventional computer-based instruction which has tended to have the effect of replacing, rather than assisting teachers.
In summary, it is desirable to have a system which provides networked deployment of instructional information without replacing existing computer and communication infrastructure.
SUMMARY OF THE INVENTION
In view of the foregoing, it is an object of the present invention to provide a computer-based, networked electronic classroom system in which the teacher can monitor class progress, ask questions including those requiring narrative or other more complicated responses, and generally focus efforts in areas where more instruction appears to be needed. It also is an object of the invention to provide classroom facilities for students to perform computer based instructional exercises, run didactic software and simulations, and compete as groups in games or other computer based instructional activities under the close direction and supervision of the teacher, while retaining the benefits of individual feedback associated with single user stand-alone systems.
It is another object of the invention to provide facilities for fully or partially automating the giving and grading of quizzes, class attendance, rollkeeping, grading of homework and other routine paperwork associated with monitoring student progress and recordkeeping. To accomplish these and other goals, the novel, inventive electronic classroom herein described includes a central computer and display at the teacher's desk, a plurality of terminals at desks of individual students and network connection between the central computer and the terminals. The terminals may range in complexity from a simple dedicated keypad with rudimentary display, to a hybrid version of a calculator/terminal with numeric and function keys, to a rudimentary hand-held computer with a full keyboard and single or multi-line display, having a number of other possible functions such as those of calculator, typewriter, organizer, appointment diary, phone directory, thesaurus, and dictionary, up to a full-fledged personal computer capable of operating in a stand-alone mode. The student terminals may be fixed in the classroom, or may be carried by students as portable devices with numerous possible ranges of applications outside a classroom context.
Thus, the inventive system encompasses a range of possible hardware and software embodiments, enabling a range of cost and functionality in its possible implementations. This range also is evident for permissible connections between the central computer and the student terminals. The network connection between the central computer and student terminals consist of a full local area network (LAN), enabling equal connectivity among all stations and any industry accepted physical topology, or (in the preferred embodiment) may consist of one of many possible lower cost network options with unequal connectivity where a special higher level protocol ensures that all messages from student terminals pass through the central computer or through a special network server connected directly to it.
Another component of the inventive system is an electronic display for displaying textual and graphic information for instructional purposes by a teacher to a class. As with other components, this display may take several forms. It may be a liquid crystal display which lies on top of an overhead projector and is driven by the display output from the central computer; it may be a projection video device which also is driven by a display output from the central computer. The information to be displayed may be divided into two categories. The first category consists of any instructional material, such as normally is displayed by teachers in conventional classrooms, and includes questions, directions, or activities. The second category includes student responses and statistical or graphic analyses (or other orderings, sortings or summaries) of the same. The display of all such information in both categories is under control of the teacher, who may view selectively such information privately on the central computer monitor before sending it out for viewing by the students.
Software and hardware that provide the following features are also provided: a communication protocol, associated with the central computer, the network and the plurality of student terminals, for allowing the transmission of command data from the central computer to one or more of the student terminals (selectively or collectively), for allowing the downloading of programs from the central computer to one or more of the student terminals in similar fashion, and for allowing the transmission of student responses or other data from the student terminals to the central computer; a timing environment, associated with the central computer software, the student terminals, and software operating on both the central computer and the student terminals, for allowing each of the terminals to proceed through a sequence of student tasks (those tasks consisting of one or a combination of questions, quizzes, tests, classroom exercises, didactic programs, instructional games, simulations, homework, and other instructional activities) either at each student's own pace, or in lockstep with all other students in the class. If the teacher assigns different tasks to different groups of students in the class, then students within each group may proceed either individually or in lockstep with others in that group, at the selection of the teacher. In all cases the responses would be transmitted and monitored by the central computer, with the teacher retaining control of the pacing of student tasks via the central computer; a command language, with an optional associated menu driven command language generator, for enabling an instructor to prepare a series of student tasks (as described above) prior to a classroom session, and for storing this information or subsequent retrieval and use, for example using non-volatile memory or removable media such as floppy discs; a control program, optionally utilizing menu driven facilities, for enabling a teacher during a class to enter a new student task, or to retrieve and view previously prepared student tasks which then may be executed; a log-on facility for students to identify themselves personally, and by classroom location, to the system; a database facility for storing information input to the system.
This information may be input by the teacher directly via the central computer, by the students via student terminals, by reading from removable storage media (such as floppy disks) or by other means (such as networking between a teacher's private computer and the electronic classroom system). The types of information which might be stored in the database would include class records, student rolls, questions, tests, or other tasks asked during each class, and student responses transmitted to the central computer. The actual repository may be fixed media within the central computer of the electronic classroom system, or it may be removable storage media which may be transferred between the classroom system and another computer outside the classroom (possibly the teacher's private computer). This transferal also may take place via a local area network between the central computer and other computers; presentation and analysis facilities to enable a teacher to view and analyze information gathered by the system. During a classroom session, these facilities would allow a teacher to view and analyze student data and responses. They also would permit the teacher selectively to show certain of these responses and analyses of such responses to the class via the electronic display. Outside a classroom session, probably on a separate computer (possibly, one located in a teacher's office), these facilities would allow a teacher to examine student responses further for a variety of purposes. Such purposes might include a search for weaknesses, or strengths, in areas of understanding for individual students, or for the class as a whole. The might include the tracking of progress of individual students, or the grouping of students with particular weaknesses or strengths. They may include assessments of attendance, class performance, homework performance, or the assignment of grades, possibly with automatic facilities for grading the various components of student performance to a selectable curve. They also may include facilities for directly transmitting student grades to administrative databases via a network.
The range of overall contexts in which the present invention may be installed and used is almost unlimited. However, emphasis on particular features of the system may vary from one context to another. For example, at the primary level there is likely to be more emphasis on the additional variety in activities provided by the system and its capability for instructional feedback to students and teacher. In addition to these factors, at the high school level automatic testing and record keeping become more important, since one teacher instructs many more students. Also, the diagnostic and early warning features become more significant. At the college level, with huge classes, all these features are important, and a professor is likely to have his or her own computer outside the classroom to assist with the preparation of materials and with data management. Thus, it would be desirable to have a flexible industrial communication and education system that could make use of existing hardware and software to deploy applications without requiring replacement of existing computer and networking environments.
DESCRIPTION OF THE DRAWINGS
The foregoing and other objects, aspects and advantages are better understood from the following detailed description of a preferred embodiment of the invention with reference to the drawings, in which:
FIG. 1 is a block diagram of a representative hardware environment in accordance with a preferred embodiment;
FIG. 2 illustrates a teaching architecture in accordance with a preferred embodiment;
FIG. 3 presents a list of many of the WinFrame v1.7 English hot fixes in accordance with a preferred embodiment;
FIG. 4 is a user profile table in accordance with a preferred embodiment;
FIGS. 5 to 7 are system tables in accordance with a preferred embodiment;
FIG. 8 is a tabular display of the optimization level and synchronization in accordance with a preferred embodiment;
FIGS. 9 to 11 are various comparison matrixes of features in accordance with a preferred embodiment;
FIG. 12 is a table of various communication protocols in accordance with a preferred embodiment;
FIGS. 13A to 13 F illustrate various architectures in accordance with a preferred embodiment;
FIG. 14 illustrates a wireless communication architecture in accordance with a preferred embodiment; and
FIG. 15 illustrates a load balancing cluster in accordance with a preferred embodiment.
DETAILED DESCRIPTION
A preferred embodiment of a system in accordance with the present invention is preferably practiced in the context of a personal computer such as an IBM compatible personal computer, Apple Macintosh computer or UNIX based workstation. A representative hardware environment is depicted in FIG. 1, which illustrates a typical hardware configuration of a workstation in accordance with a preferred embodiment having a central processing unit 110 , such as a microprocessor, and a number of other units interconnected via a system bus 112 . The workstation shown in FIG. 1 includes a Random Access Memory (RAM) 114 , Read Only Memory (ROM) 116 , an I/O adapter 118 for connecting peripheral devices such as disk storage units 120 to the bus 112 , a user interface adapter 122 for connecting a keyboard 124 , a mouse 126 , a speaker 128 , a microphone 132 , and/or other user interface devices such as a touch screen (not shown) to the bus 112 , communication adapter 134 for connecting the workstation to a communication network (e.g., a data processing network) and a display adapter 136 for connecting the bus 112 to a display device 138 . The workstation typically has resident thereon an operating system such as the Microsoft Windows NT or Windows/95 Operating System (OS), the IBM OS/2 operating system, the MAC OS, or UNIX operating system. Those skilled in the art will appreciate that the present invention may also be implemented on platforms and operating systems other than those mentioned.
A preferred embodiment is written using JAVA, C, and the C++ language and utilizes object oriented programming methodology. Object oriented programming (OOP) has become increasingly used to develop complex applications. As OOP moves toward the mainstream of software design and development, various software solutions require adaptation to make use of the benefits of OOP. A need exists for these principles of OOP to be applied to a messaging interface of an electronic messaging system such that a set of OOP classes and objects for the messaging interface can be provided.
OOP is a process of developing computer software using objects, including the steps of analyzing the problem, designing the system, and constructing the program. An object is a software package that contains both data and a collection of related structures and procedures. Since it contains both data and a collection of structures and procedures, it can be visualized as a self-sufficient component that does not require other additional structures, procedures or data to perform its specific task. OOP, therefore, views a computer program as a collection of largely autonomous components, called objects, each of which is responsible for a specific task. This concept of packaging data, structures, and procedures together in one component or module is called encapsulation.
In general, OOP components are reusable software modules which present an interface that conforms to an object model and which are accessed at run-time through a component integration architecture. A component integration architecture is a set of architecture mechanisms which allow software modules in different process spaces to utilize each others capabilities or functions. This is generally done by assuming a common component object model on which to build the architecture. It is worthwhile to differentiate between an object and a class of objects at this point. An object is a single instance of the class of objects, which is often just called a class. A class of objects can be viewed as a blueprint, from which many objects can be formed.
OOP allows the programmer to create an object that is a part of another object. For example, the object representing a piston engine is said to have a composition-relationship with the object representing a piston. In reality, a piston engine comprises a piston, valves and many other components; the fact that a piston is an element of a piston engine can be logically and semantically represented in OOP by two objects.
OOP also allows creation of an object that “depends from” another object. If there are two objects, one representing a piston engine and the other representing a piston engine wherein the piston is made of ceramic, then the relationship between the two objects is not that of composition. A ceramic piston engine does not make up a piston engine. Rather it is merely one kind of piston engine that has one more limitation than the piston engine; its piston is made of ceramic. In this case, the object representing the ceramic piston engine is called a derived object, and it inherits all of the aspects of the object representing the piston engine and adds further limitation or detail to it. The object representing the ceramic piston engine “depends from” the object representing the piston engine. The relationship between these objects is called inheritance.
When the object or class representing the ceramic piston engine inherits all of the aspects of the objects representing the piston engine, it inherits the thermal characteristics of a standard piston defined in the piston engine class. However, the ceramic piston engine object overrides these ceramic specific thermal characteristics, which are typically different from those associated with a metal piston. It skips over the original and uses new functions related to ceramic pistons. Different kinds of piston engines have different characteristics, but may have the same underlying functions associated with it (e.g., how many pistons in the engine, ignition sequences, lubrication, etc.). To access each of these functions in any piston engine object, a programmer would call the same functions with the same names, but each type of piston engine may have different/overriding implementations of functions behind the same name. This ability to hide different implementations of a function behind the same name is called polymorphism and it greatly simplifies communication among objects.
With the concepts of composition-relationship, encapsulation, inheritance and polymorphism, an object can represent just about anything in the real world. In fact, our logical perception of the reality is the only limit on determining the kinds of things that can become objects in object-oriented software. Some typical categories are as follows:
Objects can represent physical objects, such as automobiles in a traffic-flow simulation, electrical components in a circuit-design program, countries in an economics model, or aircraft in an air-traffic-control system.
Objects can represent elements of the computer-user environment such as windows, menus or graphics objects.
An object can represent an inventory, such as a personnel file or a table of the latitudes and longitudes of cities.
An object can represent user-defined data types such as time, angles, and complex numbers, or points on the plane.
With this enormous capability of an object to represent just about any logically separable matters, OOP allows the software developer to design and implement a computer program that is a model of some aspects of reality, whether that reality is a physical entity, a process, a system, or a composition of matter. Since the object can represent anything, the software developer can create an object which can be used as a component in a larger software project in the future.
If 90% of a new OOP software program consists of proven, existing components made from preexisting reusable objects, then only the remaining 10% of the new software project has to be written and tested from scratch. Since 90% already came from an inventory of extensively tested reusable objects, the potential domain from which an error could originate is 10% of the program. As a result, OOP enables software developers to build objects out of other, previously built objects.
This process closely resembles complex machinery being built out of assemblies and sub-assemblies. OOP technology, therefore, makes software engineering more like hardware engineering in that software is built from existing components, which are available to the developer as objects. All this adds up to an improved quality of the software as well as an increased speed of its development.
Programming languages are beginning to fully support the OOP principles, such as encapsulation, inheritance, polymorphism, and composition-relationship. With the advent of the C++ language, many commercial software developers have embraced OOP. C++ is an OOP language that offers a fast, machine-executable code. Furthermore, C++ is suitable for both commercial-application and systems-programming projects. For now, C++ appears to be the most popular choice among many OOP programmers, but there is a host of other OOP languages, such as Smalltalk, Common Lisp Object System (CLOS), and Eiffel. Additionally, OOP cap abilities are being added to more traditional popular computer programming languages such as Pascal.
The benefits of object classes can be summarized, as follows:
Objects and their corresponding classes break down complex programming problems into many smaller, simpler problems.
Encapsulation enforces data abstraction through the organization of data into small, independent objects that can communicate with each other. Encapsulation protects the data in an object from accidental damage, but allows other objects to interact with that data by calling the object's member functions and structures.
Subclassing and inheritance make it possible to extend and modify objects through deriving new kinds of objects from the standard classes available in the system. Thus, new capabilities are created without having to start from scratch.
Polymorphism and multiple inheritance make it possible for different programmers to mix and match characteristics of many different classes and create specialized objects that can still work with related objects in predictable ways.
Class hierarchies and containment hierarchies provide a flexible mechanism for modeling real-world objects and the relationships among them.
Libraries of reusable classes are useful in many situations, but they also have some limitations. For example:
Complexity. In a complex system, the class hierarchies for related classes can become extremely confusing, with many dozens or even hundreds of classes.
Flow of control. A program written with the aid of class libraries is still responsible for the flow of control (i.e., it must control the interactions among all the objects created from a particular library). The programmer has to decide which functions to call at what times for which kinds of objects.
Duplication of effort. Although class libraries allow programmers to use and reuse many small pieces of code, each programmer puts those pieces together in a different way. Two different programmers can use the same set of class libraries to write two programs that do exactly the same thing but whose internal structure (i.e., design) may be quite different, depending on hundreds of small decisions each programmer makes along the way. Inevitably, similar pieces of code end up doing similar things in slightly different ways and do not work as well together as they should.
Class libraries are very flexible. As programs grow more complex, more programmers are forced to reinvent basic solutions to basic problems over and over again. A relatively new extension of the class library concept is to have a framework of class libraries. This framework is more complex and consists of significant collections of collaborating classes that capture both the small scale patterns and major mechanisms that implement the common requirements and design in a specific application domain. They were first developed to free application programmers from the chores involved in displaying menus, windows, dialog boxes, and other standard user interface elements for personal computers.
Frameworks also represent a change in the way programmers think about the interaction between the code they write and code written by others. In the early days of procedural programming, the programmer called libraries provided by the operating system to perform certain tasks, but basically the program executed down the page from start to finish, and the programmer was solely responsible for the flow of control. This was appropriate for printing out paychecks, calculating a mathematical table, or solving other problems with a program that executed in just one way.
The development of graphical user interfaces began to turn this procedural programming arrangement inside out. These interfaces allow the user, rather than program logic, to drive the program and decide when certain actions should be performed. Today, most personal computer software accomplishes this by means of an event loop which monitors the mouse, keyboard, and other sources of external events and calls the appropriate parts of the programmer's code according to actions that the user performs. The programmer no longer determines the order in which events occur. Instead, a program is divided into separate pieces that are called at unpredictable times and in an unpredictable order. By relinquishing control in this way to users, the developer creates a program that is much easier to use. Nevertheless, individual pieces of the program written by the developer still call libraries provided by the operating system to accomplish certain tasks, and the programmer must still determine the flow of control within each piece after it's called by the event loop. Application code still “sits on top of” the system.
Even event loop programs require programmers to write a lot of code that should not need to be written separately for every application. The concept of an application framework carries the event loop concept further. Instead of dealing with all the nuts and bolts of constructing basic menus, windows, and dialog boxes and then making these things all work together, programmers using application frameworks start with working application code and basic user interface elements in place. Subsequently, they build from there by replacing some of the generic capabilities of the framework with the specific capabilities of the intended application.
Application frameworks reduce the total amount of code that a programmer has to write from scratch. However, because the framework is really a generic application that displays windows, supports copy and paste, and so on, the programmer can also relinquish control to a greater degree than event loop programs permit. The framework code takes care of almost all event handling and flow of control, and the programmer's code is called only when the framework needs it (e.g., to create or manipulate a proprietary data structure).
A programmer writing a framework program not only relinquishes control to the user (as is also true for event loop programs), but also relinquishes the detailed flow of control within the program to the framework. This approach allows the creation of more complex systems that work together in interesting ways, as opposed to isolated programs, having custom code, being created over and over again for similar problems.
Thus, as is explained above, a framework basically is a collection of cooperating classes that make up a reusable design solution for a given problem domain. It typically includes objects that provide default behavior (e.g., for menus and windows), and programmers use it by inheriting some of that default behavior and overriding other behavior so that the framework calls application code at the appropriate times.
There are three main differences between frameworks and class libraries:
Behavior versus protocol. Class libraries are essentially collections of behaviors that you can call when you want those individual behaviors in your program. A framework, on the other hand, provides not only behavior but also the protocol or set of rules that govern the ways in which behaviors can be combined, including rules for what a programmer is supposed to provide versus what the framework provides.
Call versus override. With a class library, the code the programmer instantiates objects and calls their member functions. It's possible to instantiate and call objects in the same way with a framework (i.e., to treat the framework as a class library), but to take full advantage of a framework's reusable design, a programmer typically writes code that overrides and is called by the framework. The framework manages the flow of control among its objects. Writing a program involves dividing responsibilities among the various pieces of software that are called by the framework rather than specifying how the different pieces should work together.
Implementation versus design. With class libraries, programmers reuse only implementations, whereas with frameworks, they reuse design. A framework embodies the way a family of related programs or pieces of software work. It represents a generic design solution that can be adapted to a variety of specific problems in a given domain. For example, a single framework can embody the way a user interface works, even though two different user interfaces created with the same framework might solve quite different interface problems.
Thus, through the development of frameworks for solutions to various problems and programming tasks, significant reductions in the design and development effort for software can be achieved. A preferred embodiment of the invention utilizes HyperText Markup Language (HTML) to implement documents on the Internet together with a general-purpose secure communication protocol for a transport medium between the client and the Newco. HTTP or other protocols could be readily substituted for HTML without undue experimentation. Information on these products is available in T. Berners-Lee, D. Connoly, “RFC 1866: Hypertext Markup Language—2.0” (November 1995); and R. Fielding, H, Frystyk, T. Berners-Lee, J. Gettys and J. C. Mogul, “Hypertext Transfer Protocol—HTTP/1.1:HTTP Working Group Internet Draft” (May 2, 1996). HTML is a simple data format used to create hypertext documents that are portable from one platform to another. HTML documents are SGML documents with generic semantics that are appropriate for representing information from a wide range of domains. HTML has been in use by the World-Wide Web global information initiative since 1990. HTML is an application of ISO Standard 8879; 1986 Information Processing Text and Office Systems; Standard Generalized Markup Language (SGML).
To date, Web development tools have been limited in their ability to create dynamic Web applications which span from client to server and interoperate with existing computing resources. Until recently, HTML has been the dominant technology used in development of Web-based solutions. However, HTML has proven to be inadequate in the following areas:
Poor performance;
Restricted user interface capabilities;
Can only produce static Web pages;
Lack of interoperability with existing applications and data; and
Inability to scale.
Sun Microsystem's Java language solves many of the client-side problems by:
Improving performance on the client side;
Enabling the creation of dynamic, real-time Web applications; and
Providing the ability to create a wide variety of user interface components.
With Java, developers can create robust User Interface (UI) components. Custom “widgets” (e.g., real-time stock tickers, animated icons, etc.) can be created, and client-side performance is improved. Unlike HTML, Java supports the notion of client-side validation, offloading appropriate processing onto the client for improved performance. Dynamic, real-time Web pages can be created. Using the above-mentioned custom UI components, dynamic Web pages can also be created.
Sun's Java language has emerged as an industry-recognized language for “programming the Internet.” Sun defines Java as: “a simple, object-oriented, distributed interpreted robust, secure, architecture-neutral, portable, high-performance, multithreaded, dynamic, buzzword-compliant, general-purpose programming language. Java supports programming for the Internet in the form of platform-independent Java applets.” Java applets are small, specialized applications that comply with Sun's Java Application Programming Interface (API) allowing developers to add “interactive content” to Web documents:(e.g., simple animations, page adornments, basic games, etc.). Applets execute within a Java-compatible browser (e.g., Netscape Navigator) by copying code from the server to client. From a language standpoint, Java's core feature set is based on C++. Sun's Java literature states that Java is basically, “C++ with extensions from Objective C for more dynamic method resolution.”
Another technology that provides similar function to JAVA is provided by Microsoft and ActiveX Technologies, to give developers and Web designers wherewithal to build dynamic content for the Internet and personal computers. ActiveX includes tools for developing animation, 3-D virtual reality, video and other multimedia content. The tools use Internet standards, work on multiple platforms, and are being supported by over 100 companies. The group's building blocks are called ActiveX Controls, small, fast components that enable developers to embed parts of software in hypertext markup language (HTML) pages. ActiveX Controls work with a variety of programming languages including Microsoft Visual C++, Borland Delphi, Microsoft Visual Basic programming system and, in the future, Microsoft's development tool for Java, code named “Jakarta.” ActiveX Technologies also includes ActiveX Server Framework, allowing developers to create server applications. One of ordinary skill in the art readily recognizes that ActiveX could be substituted for JAVA without undue experimentation to practice the invention.
Introduction
An Information Utility Solution in accordance with a preferred embodiment provides a fully-managed information technology infrastructure designed to meet the current and future Internet connectivity and computing needs of most industrial training centers. The system provides increased computing capabilities and continuing access to technology at lower cost with lower risk.
A preferred embodiment of the solution will be presented utilizing a school education example (K-12), due to the large increase in federal and state funding and attention for information technology in the classroom. The solution will combine thin-client computing architecture, wireless LAN technology, centrally-managed data center operations and desktop outsourcing services to provide clients with an affordable, managed, high-performance desktop environment to almost any end-user device, including 286 PCs and Macintosh computers.
This Solution is both platform independent and operating system independent. Any application from any client and any form of operating system can be installed and used—including Macintosh and Apple II. End users can access the applications and content from either office terminals via LAN or from their home computers via direct dial up or website access via Internet browser.
The preferred embodiment can be configured to employ technology that will ensure that access to the Internet will be restricted to appropriate websites and content. Similar restrictions/access profiles will apply to the use of licensed premium training and educational content as well as computer applications.
The wireless LAN technology facilitates a cost-effective, cable-free installation of computing networks—particularly beneficial to those government entities which have buildings with asbestos contamination. Wireless LANs will also permit rapid installations. Finally, integrating the preferred embodiment architecture and technology will allow ServiceNet-like data centers to provide centralized network and application management—including the ability to remotely update client terminals and minimize LAN maintenance costs.
Management
Single point control for network management. The system can be deployed, managed and applications supported in minutes—not months—from one data center location. User profiles can be defined that are consistent across job categories for application and Internet access. Further, the technology will allow for the development of customized desktop environments for each employee.
Integrated Email, file and Web services.
Scalable solution which can support thousands of concurrent users.
Access
Universal application access that is platform and operating system independent is provided in accordance with a preferred embodiment. The technology will allow workers to access their unique desktops from any client device including the Internet, library, and home computers. No matter which device a person uses to access the system, their desktop will appear to “follow” them—including any restrictions or limitations on access to appropriate applications and content as defined the user profile. Government entities will be able to “rent” access to many applications on an as-needed basis, thereby saving on software licensing fees. The technology will allow government entities to reuse any existing client terminals as well as any existing software programs.
Performance
The architecture of the preferred embodiment keeps network-intense application activity within the data center, which results in bandwidth-independence. The Government Information Utility Solution provides LAN-like performance: regardless of the form of access to the system: modems, WAN, wireless LAN or Internet; and with only 20 KBPS of bandwidth per user.
Security
The Integrated Government Information Utility Solution provides security for applications and data because the data center—not the individual client terminals—is the sole point of installation for licensed software. This protects the government entities as well as the vendors from unauthorized use of the applications. In addition, this structure addresses concerns about the introduction and control of viruses in the LAN. Access to the Internet, software applications and user content will be restricted to only those sites/uses which are deemed appropriate by the government system administrators, as defined in each individual user profile.
Important Technologies in Accordance with a Preferred Embodiment
In addition to readily available hardware and software applications, several strategic technologies and services will need to be tightly integrated in order to offer the complete Newco Government Information Utility Solution:
Thin-Client/Server system software
Wireless LAN technology
Emulation software
Content providers
WAN infrastructure
Data center services
Dial-up infrastructure providers
LAN/Desktop management services (including on-site installation services, first line help support, etc.)
Other technologies will also be needed, including:
Customized applications, which will provide unique functionality, designed by AC.
Internet proxy servers providing a server-based filtering system to restrict Internet access to the appropriate websites and content.
Software emulators (e.g., Macintosh, Apple II).
Educational content providers, for example:
Training/Educational Content
Encyclopedia/Reference
Textbook
Third-Party Strategy Overview
Each component in accordance with a preferred embodiment will be identified and categorized according to strategic value to the offering. Components that can be characterized as mature products or services, widely available in the marketplace, and/or available through multiple vendors providing similar products or services will be considered of low strategic value. Generally, these components are provided on a competitive bid basis to ensure the lowest cost. Components that are unique in the marketplace or are otherwise critical to the system will be sourced through more formal contractual arrangements including, in certain cases, private-label OEM manufacturing agreements or preferred alliance agreements.
Product Profiles
Citrix WinFrame is a multi-user Windows application server based on Windows NT that supports enterprise application deployment using a thin-client architecture. This network-centric approach includes universal, thin-client software that works in conjunction with WinFrame multi-user application server software. Enterprise applications execute on the WinFrame server and are accessed through thin-client software over dial-up, LAN, WAN and Internet connections. The key to this thin-client architecture is a distributed Windows presentation protocol developed by Citrix, called ICA.
Citrix's Independent Computing Architecture (ICA) is a general-purpose presentation services protocol for Microsoft Windows. Conceptually, ICA is similar to the UNIX X-Windows protocol. ICA allows an application's logic to execute on a WinFrame multi-user Windows application server, located on the LAN. Only the user interface, keystrokes and mouse movements are transferred between the server and the client device over any network or communications protocol, resulting in minimal client resource consumption. ICA is designed to run over industry-standard network protocols, such as TCP/IP, NetBEUI, IPX/SPX, and PPP and industry-standard transport protocols, such as asynchronous (ASYNC), ISDN, Frame Relay and ATM.
The ICA protocol presents only the user interface from an executing machine on the display of another machine. ICA provides true location independence for Windows applications by running the Windows application at one location and executing the program's user interface somewhere else. This distributed Windows architecture allows Windows 16, Windows 32 and client/server applications to perform at very high speed over low bandwidth connections. It also allows 16- and 32-bit applications to run on legacy PCs as well as a new-generation of lightweight client devices.
A key component of a preferred embodiment is its RangeLAN2 OEM modules with ISA, Serial and PCMCIA connectors. RangeLAN2 OEM products include all of the industry-leading technology and features of the branded RangeLAN2 products, including 2.4 GHz gallium arsenide RF application specific integrated circuit (ASIC), custom digital signal processor ASIC, and wireless network controller ASIC. RangeLAN2 products operate at a data rate of 1.6 Mbps per channel, with 15 independent channels available. This multi-channel architecture allows up to 15 independent wireless LANs to operate in the same physical space providing up to 24 Mbps of aggregate network bandwidth. RangeLAN2 also features the most sophisticated mobility-centric network architecture of any wireless LAN product, including state-of-the-art seamless roaming, power management, advanced security, site survey diagnostics, and the IEEE-endorsed high-speed modulation technique (IEEE 802.11). OEM products are also WLIF (Wireless LAN Interoperability Forum)-compliant meaning that all products will interoperate. Using WLIF-compliant products, customers can choose from an even greater range of interoperable client and wireless networking solutions.
A preferred embodiment provides managed Internet access, desktop outsourcing and access to premium training, educational and other data content. AC will manage the operations of Newco under a management contract. Where appropriate, Newco will establish separate market-facing entities to deliver its offering to the various target market segments. FIG. 2 illustrates a teaching architecture in accordance with a preferred embodiment. The system provides a customized desktop environment of each level of student. Students can also access their desktops from a personal computer in the school, at home or at another remote site, like a library. Existing personal computer and Macintosh computers can be reused to provide access to the Internet utilizing a wireless LAN to avoid impacting existing communication lines. Teachers can use the system to broadcast their lessons, shadow student sessions and remotely control student's computers. Thin client technology is used to provide extended life cycles for clients, provide centralized application upgrades, Internet access, backup, security and control of existing personal computer resources.
WinFrame Server Setup in Accordance with a Preferred Embodiment
Installing WinFrame Operating System
Preparation Requirements
WinFrame installation media (Three setup diskettes and one CD-ROM).
Assuming installation of WinFrame on a Compaq Proliant server, the latest release of the Compaq Support Software diskettes (CSSD) for Windows NT 3.5x should be available (http://www.compaq.com/support/files/server/softpaqs/WINNT/NTSSD351.html). These disks will be required at different points throughout the installation.
Download any appropriate WinFrame Service Packs or HotFixes (ftp://ftp.citrix.com/winfrm17/). Ensure the PDC is running and connected prior to installing a WinFrame server as BDC or standalone server.
Installing WinFrame 1.7
Run the installation with the first of three WinFramne setup diskettes and the CD-ROM.
Install disk 2 , select new install of WinFrame.
Choose the custom installation option.
Select “S”—to skip detection.
If installing on a Proliant 5000, skip to step 12
Select “S”—to specify the SCSI adapter and array controller.
Choose “Other” and place CSSD disk # 1 in drive.
Choose “Compaq 32-Bit SCSI-2 controller for Windows NT 3.51”.
Insert the third WinFrame setup disk at the prompt.
Once WinFrame has determined the computer components, select the “Computer: MPS Multiprocessor PC”.
Select “Other” and place CSSD disk # 1 in drive.
Choose “Compaq MPS Multiprocessor for Windows NT 3.51”.
Select “No Changes: The above list matches my computer.”
Select “Unpartitioned space”.
Select “Format the partition using the NTFS file system”.
Choose the default directory “\WINFRAME”.
Press <ESC> to skip the examination.
When prompted for the “CSSD for Windows NT 3.51/4.0”, insert disk 2 of current version of the CSSD.
When prompted again for “Compaq SSD for Windows NT 3.51/4.0”, insert disk 1 of current version of Compaq SSD.
Once the reboot occurs, a WinFrame window will prompt you for the Name and Company. For Name, enter “SchoolNet”. For Company, enter “Andersen Consulting”.
In the “WinFrame Server Security Role” window, leave as standalone server or select the Backup Domain Controller radio button.
Install appropriate number of Microsoft Client Licenses necessary. For standard WinFrame server with no shared drives or remote access services, no additional client licenses are necessary. If these services are running, sufficient Microsoft Client Licenses (different from Citrix Client Licenses) must be enabled. This is a somewhat confusing issue; please contact your Microsoft reseller for additional licensing answers.
At the prompt window for the computer name, enter the WinFrame server name based on the standard naming convention (i.e. WLS-1, WLS-2, etc.)
When asked to verify the server name, check the name to ensure it is accurate.
When the “WinFrame Setup” window appears, select “Set up Only Windows Components”.
At the next window, deselect those components that are not required. While it is good practice to remove programs such as games and screen-savers, users will be prevented from running this sort of software via their profile anyway.
When the “Network Adapter Card Detection” window appears, select “Do Not Detect”.
When the “Network Adapter Card Detection” window appears, select “Continue”.
Choose “Other” and place CSSD disk # 1 in drive.
Type the path “A:\net\netflx3”.
Select the driver listed in the window. The “Windows NT Setup” window will appear and a series of files will be copied to the hard drive.
Choose TCP/IP and NetBEUI for the network protocols.
In the “Windows NT TCP/IP Installation Options”, select “TCP/IP Network Printing Support “and “Simple TCP/IP Services”.
In the “WinFrame Dial-In Support” window, select “No”.
In the “Network Settings” window, no changes are required.
In the “IP configuration” window, enter the appropriate addressing info (IP address, subnet mask, gateway, etc.) for the computer.
In the “Domain Settings” window, if the server is a standalone, (not a PDC or BDC) and it should become part of a domain, select the button next to the domain line.
Select the domain line and enter the name of the domain to enter.
Enter the administrator name and password.
Select “OK”. If the administrator password is correct, a message welcoming you to the domain will appear.
In the “Virtual Memory” window, accept the default. (The paging file should be at least 1.5 x the physical memory of the machine. A 2GB paging file is not out of the ordinary.)
In “Date/Time” window, enter the date and time.
In “Display Settings” window, adjust colors.
After adjusting, select “Test”.
When prompted to re-map the server drive letters, select “No”.
When you have joined the domain, you will be prompted to install the licenses. Insert the base license disk.
Confirm the Base License Agreement and select “OK”. Once the license is installed, you will be prompted for additional licenses. Select “No” and continue with the install.
The install will save the server installation and will ask you if you would like to make a Rescue Disk. Select “No”.
Note: A rescue disk should be made when the entire install, including service packs and hot fixes, is complete.
The system will now ask you to reboot.
In Program Manager, select ‘File|Run’
Type ‘command’
On command line, type ‘setbuild /ms’
Run ‘setup.cmd’ from CSSD disk # 1
Follow displayed directions for installing ‘Compaq MPS Multiprocessor for Windows NT 3.51’ and ‘Compaq 32-bit SCSI-2 controller’
On command line, type ‘setbuild /oem’
Installing Hotfixes
Occasionally, Citrix will release an update patch for WinFrame that corrects existing behaviors or adds new functionality. Information about these updates, as well as the actual executables, are available from Citrix's web site: http://www.citrix.com. It is a good idea to browse this site regularly for information related to WinFrame.
Create a subdirectory in “C:\hotfix\” with the name of the Hotfix to be installed.
Copy the Hotfix self-extracting archive into the newly created subdirectory.
Enter the new hotfix subdirectory.
Run the self-extracting archive.
Run “/hotfix.exe/i” to install the patch.
Reboot the server.
Run “hotfix.exe/v” to verify successful installation of the patch.
Note: The command “hotfix” provides a multitude of diagnostic and maintenance capabilities related to these operating system patches; please refer to standard Windows NT Server documentation for more information on this command.
FIG. 3 presents a list of many of the WinFrame v1.7 English hot fixes in accordance with a preferred embodiment. These fixes are applied to remedy a variety of known problems with the base application environment.
Install Network Monitor Agent
In ‘Control Panel’, choose ‘Network’ utility
In ‘Network Settings’, choose ‘Add Software’
Select ‘Network Monitor Agent’
Optimizing TCP/IP Settings for High-latency, WAN-connected WinStations
Logon to the system as an administrator
Delete all existing TCP/IP WinStations from ‘WinStation Configuration’ utility located in ‘Administrative Tools group.
From Program Manager, select ‘File|Run’
Type ‘REGEDT32’.
Select the hive: //HKEY_LOCAL_MACHINE/SYSTEM/
CurrentControlSet/Control/Citrix/Pds/tcp
Double-click on ‘OutBufDelay’.
Click on decimal.
Lower the value to anywhere between 50-100
Recreate all TCP WinStations as described in section 2.2.4. Configuring WinStation Connections
Repeat entire process until Optimal results are achieved
Changing Screen Saver Settings to Optimize Performance
Idle WinStations consume valuable system resources (CPU, memory, etc.) on a multiuser system. By changing several screen saver settings, the effects of idle terminals are greatly reduced
Logon to the system as an administrator
From Program Manager, select ‘File|Run’
Type ‘REGEDT32’.
Select the hive: ‘\\HKEY_USERS\DEFAULT\Control Panel\Destop’
Change value of ‘ScreenSaveTimeOut’ to ‘300’
Replace ‘logon.scr’ with ‘black16.scr’ in ‘SCRSAVE.EXE’
Creating Emergency Repair (‘Rescue’) Disk Set
Have at least 1 3.5”, 1.44 MB formatted disk available for each WinFrame server prior to beginning this operation.
Logon to the system as an administrator
From Program Manager, select ‘File|Run’
Type ‘rdisk’
Choose ‘Save Repair Info’
When finished, label the disk with the server name and date. Write-protect this disk and store in a safe place.
Installing Licenses
Logon to the system as an administrator
From the ‘Administrative Tools’ group run ‘WinFrame Licensing’
Choose ‘License|Add’ from menu bar.
Type Base License Serial Number into dialog box
Read and accept terms and conditions, and click ‘OK’
Add ‘Load Balancing’ and ‘5-Client’ packs as above
Highlight any user license groups you wish to ‘pool’ in a load balancing configuration
Choose ‘License|Change License Pool’ from menu bar
Type the number of licenses to pool
Repeat steps 8 & 9 for all licenses to be ‘pooled’
Activating Licenses
Open a web browser to http://www.citrix.com/misc/wfreg17.htm
Activate the registration link
Complete the registration form. When finished, a valid ‘activation code’ will be presented.
Logon to the WinFrame system as an administrator
From the ‘Administrative Tools’ group run ‘WinFrame Licensing’
Highlight license to be activated.
Choose ‘License|Activate License’ from menu bar.
Type the Activation Code for the desired license.
Configuring WinStation Connections
1. Log in as Administrator.
2. From the ‘Administrative Tools’ group run ‘WinStation Configuration’
3. Double click on the line entry for the TCP/IP protocol (“tcp#001-0xx”).
4. Inside the “Network Transport Configuration” box there will be a field for “Number of configured WinStations”; increase the number so that it equals the maximum number of client connections to accept on the server, i.e., 50.
5. Select the ‘Advanced WinStation’ button
6. Deselect all ‘inherit user config’ checkboxes
7. For ‘On a broken or timed-out connection’, select ‘disconnect’
8. For ‘Reconnect sessions disconnected’, select ‘from any WinStation’
9. For ‘Shadowing’ field, select ‘is enabled: input ON, notify OFF’
WinFrame Load Balancing
Creating a Load-Balancing Cluster
1. Log in as Administrator.
2. From the ‘Administrative Tools’ group run ‘Application Configuration’
3. Choose ‘Application|New’ from the menu bar
4. Enter ‘WLS’ for the application name
5. Choose ‘Explicit’ for the application type.
6. Select the ‘WLS’ global group and add it to the list of user groups allowed to access the application
7. Choose all available WinFrame servers and add them to the configuration list
Configuring Load-Balancing
1. Log in as Administrator.
2. From the ‘Administrative Tools’ group run ‘Application Configuration’
3. Highlight ‘WLS’
4. Choose ‘Configure|Load Balancing’ from menu bar
5. Highlight the first server and choose ‘Edit’
6. Adjust parameters. Set ‘Assume User load is 100% at:’ to 50 and click ‘Use Default Advanced Factors’
7. Repeat steps 5 & 6 for all WinFrame servers
Integrate WinFrame Servers Into WindowsNT Domain
WinFrame-specific Profile Entries
WinFrame user profiles contain all of the information stored in traditional Windows NT user profiles, plus additional, MultiWin-specific configuration entries. The standard Security Account Manager (SAM) database found on traditional WindowsNT machines has no entries for these MultiWin fields. When users log into a WinFrame host but are authenticated on an NT PDC or BDC, these MultiWin configuration details WILL NOT be correctly set.
The solution is to modify SAM databases on all NT-based PDC/BDC domains to include MultiWin specific fields. Citrix provides a utility to accomplish this.
3.1.1. Convert SAM database on WindowsNT PDC
1. Log in as Administrator.
2. From Program Manager run ‘File Run’
3. Type ‘command’
4. From command line, run ‘CNVRTUC’ against PDC
5. Reboot both WinFrame server and PDC
6. Ensure that PDC information is replicated throughout the domain
WLS User Configuration
WLS User & Group Scheme
This section will be written in cooperation with NT domain administrators at ServiceNet
WLS User Profiles
All user profiles will be ‘mandatory’ as opposed to ‘personal’; that is, students and teachers will not be able to change any desktop or configuration settings. There will be one profile for each grade level, reflecting the increased permissiveness and requirements of older children. There will be one profile for all teachers, and one profile for each administrative function (headmaster, secretary, etc.). Creation and support of profiles will be done through two administrative accounts. The first is a template account for creating new users. The second is a profile manager account for changing any configuration or desktop settings.
Creating a User Template
The user template is set up with the creation of a new User Profile. It is used to add users. All user template names should end with ‘_temp’ so that they can easily be identified in ‘User Manager for Domains’.
Login as administrator.
In “User Manager for Domains”, select “New User” from the “User” pull-down menu.
Type in the template name, ensuring that it ends with_temp.
Enter an appropriate description, so that account can easily be identified, such as “template account for the WLS 4 th Grade”.
Enter the password twice for the account.
Select the “User Cannot Change Password”, “Password Never Expires”, and “Account Disabled” boxes.
Press the “Groups” button to bring up the “Group Memberships” window and add both the “WLS” group and the specific group to which that user belongs.
Note: All users are apart of the WLS group. The WLS group should always be used when setting up a new profile or a new user. In addition, each user is also a member of a more specific group, such as 4 th Grade or Teachers, as an organizational convenience for the administrator.
Ensure that “WLS” is the Primary Group
Select “OK “to exit the Group Memberships window.
Press the “Profile” button to open the “User Environment Profile” window.
In the “WinFrame Profile Path”, enter the path “\\PDC\Profiles\<name_of_profile.man>”
In the “Connect” field select “H:” as the drive letter and enter the path “\\PDC\Home\%USERNAME%”.
Select “OK” to exit the “User Environment Profile” window.
In the “User Properties” window, select “OK” to exit.
Creating a Profile Manager
Each time a user profile is created, an accompanying profile manager should be created.
The user profile is mandatory (.man), and the profile manager is personal (.usr); other than that, the files should always duplicate each other.
Login as administrator
In “User Manager for Domains”, select the appropriate template account, such as 4th_grade_temp.
Select “Copy” from the “User” pull-down menu.
Type in the template name, ensuring that it ends with_manager.
Enter an appropriate description, so that account can easily be identified, such as “profile manager account for the WLS 4 th Grade”.
Enter the password twice.
Deselect the “Account Disabled” checkbox
Press the “Profile” button to open the “User Environment Profile” window.
In the “WinFrame Profile Path”, enter the path “\\PDC\Profiles\<name_of_profile.usr>”
Press the “Groups” button to bring up the “Group Memberships” window and add ‘Administrators’.
Select “Add”.
Logoff current WinFrame session, and login with newly created profile manager account. Create desktop groups and icons accordingly. Section 4.2.6 lists the applications that should be available to each functional group.
To modify the “Control Panel” settings for this profile, select “Run” from the “File” pull-down menu. Type “control” to bring up the “Control Panel” window and make the required modifications, such as changing the default printer connection or setting user environment variables. When the modifications in “Control Panel” are complete, exit the “Control Panel” window.
From the desktop, ensure that “Save Settings on Exit” from the “Options” pull-down menu is deselected.
Select “Run” from the “File” pull-down menu.
Type “upedit” to bring up the “User Profile Editor” window.
Ensure that the following checkboxes are checked: ‘Disable Run in File Menu’ and ‘Disable Save Settings Menu Item and Never Save Settings’,
Ensure that the following checkboxes are NOT checked: ‘Show Common Program Groups’, ‘Allow User to Connect/Remove Connections in Print Manager’, and ‘Wait for Logon Script to Complete Before Starting Program Manager’
Make all appropriate program groups Locked.
Ensure that the users in question are permitted to use the profile (make sure their group is listed, or a subgroup of the group listed, in ‘Permitted to Use Profile’)
In ‘For Unlocked Groups, Allow Users to:’, select ‘Change Program Item Properties Except Command Line’
Select “Save As File” from the “File” pull-down menu.
Select “Network” in the “Save As” window.
Save the current profile in the “\\PDC\Profiles\” directory as both a mandatory and standard profile (.man and .usr extensions, respectively).
After saving the “.man” and “.usr” profiles exit all windows to return to the main desktop.
Logoff WinFrame.
Creating a New User
Login as administrator.
In “User Manager for Domains”, select the appropriate template account, such as 4th_grade_temp.
Select “Copy” from the “User” pull-down menu.
Enter the user's full name in the “Full Name” field.
Enter the user's password twice.
Deselect the “Account Disabled” checkbox
Select “Add”.
Repeat steps 2 - 7 as necessary.
Logon with the newly added username(s) and password(s) to ensure that the profile(s) have been been correctly assigned.
Modifying an Existing Profile
The profile manager is used as the vehicle for making required changes to User Profiles as described below:
Login with the appropriate profile manager account.
Create desktop groups and icons accordingly. Modify all relevant configuration documentation.
To modify the “Control Panel” settings for this profile, select ‘File|Run’. Type ‘control’ to bring up the “Control Panel” window and make the required modifications
From the desktop, ensure that “Save Settings on Exit” from the “Options” pull-down menu is deselected.
Select “Run” from the “File” pull-down menu.
Type “upedit” to bring up the “User Profile Editor” window.
Make any required changes in the “User Profile Editor” window.
Select “Save As File” from the “File” pull-down menu.
Select “Network” in the “Save As” window.
Save the current profile in the “\\PDC\Profiles\” directory as both a mandatory and standard profile (.man and .usr extensions, respectively). Ensure that the filename is consistent with standard profile naming conventions.
When the window appears asking if you want to overwrite the existing file, select “Yes”.
After saving the “.man” and “.usr” profiles exit all windows to return to the main desktop.
Logoff WinFrame.
Common Profile Permissions for WLS Users
All User Profiles carefully limit user activity during a session. In addition, any changes made during a session, such as re-sizing a window, are not saved when the user logs off WinFrame.
Each User Profile is designed so the users cannot perform the following functions:
Create a “Personal Program Group” using the “New” command under the “File” menu.
Create a “Program Item” or “Common Program Group” using the “New” command under the “File” menu.
Use the ‘Move”, “Copy”, “Delete”, or “Run” commands under the “File” menu.
Change their passwords using the “Winframe Security” pull-down menu option under “File” and selecting “Change Password”.
“Arrange Icons” under the “Window” menu.
“Save Settings on Exit” under the “Options” menu .
“Save Settings Now” under the “Options” menu.
Each User Profile is designed so the users can perform the following functions:
View the “Program Item Properties” using the “Properties” command under the “File” menu.
Note: The user cannot modify the properties in any way.
Lock the workstation using the “Winframe Security” pull-down menu option under “File” and selecting “Lock Workstation”.
Use “Auto Arrange” and 'Minimize on Use” under the “Options” menu.
Use “Cascade” and “Tile” under the “Window” menu.
Use all help functions under the “Help” menu.
FIG. 4 is a user profile table in accordance with a preferred embodiment. The various fields are completed as the system is installed in a school or other industrial environment to define the system environment.
WLS Print Architecture
Rationale
WLS users are encouraged to print to the network attached printers located in each computer lab. These printers have higher duty cycles, require less maintenance, and will provide better performance than other devices. No additional printers can be added without contacting the Help Desk. The Help Desk does NOT have responsibility for maintaining printers, only for maintaining printer availability through the servers and network.
Many classrooms will have a single workstation capable of printing to a locally attached inkjet printer. This workstation is ‘thicker’ than a typical thin client, and should be able to support low-volume printing without experiencing debilitating performance issues. This printer is NOT shared across the network and is hence inaccessible by other thin clients. Each grade profile will include the ability to print to all network printers, and also any locally attached printers in the appropriate classrooms.
Naming Convention for Centrally Managed Printers
The naming convention used for centrally managed printers located in the WLS computer labs is as follows.
Data Center Firewall Setup
Defining SchoolNet Security Policy
Thin-Client Installation
Win95 to Thin-client Conversion
Preparation Requirements:
Win95 workstation with properly installed and configured TCP/IP connection WinFrame server IP address.
Installing WinFrame Client
Insert WinFrame client disk into drive.
Select “Start”, then “Run”.
Type “A:\setup”.
Allow all default installation parameters.
Configuring WinFrame Client for WLS
Double click on the Remote Application Manager icon on Win95 desktop. At the prompt to enter a new entry, select “No”.
Select “Options”, then “Settings . . . ”.
In the “Settings” window select the “Server Browsing” tab.
In the “TCP/IP Address:” field type the IP address of the WinFrame server you wish to connect to. If you are connecting to a cluster, choose the ICA master browser.
Click “OK”.
Select “Entry”, then “New”.
Select the “Network Connection” radio button, click on “Next”.
In the “Description:” field, enter ‘WLS’.
In the “Network Protocol:” pull down menu, select “TCP/IP”.
In the “Server” field, select the WinFrame server or Cluster name you are connecting to. Click on “Next”.
In the “Add a new Remote Application window” click on the “Change . . . ” button.
In the “Windows Properties” window, deselect “Use default” checkbox.
Select the “640×480” radio button.
Select “OK”.
Click on “Next”.
Leave the “Application:” and “Working Directory:” fields blank. Click on “Next”.
Click on “Next” and “Finish”.
Close the “Remote Application Manager” window.
Right click on the “Remote Application Manager” icon then select “Properties”.
In the “Remote Application Manager Properties” window, select the “Shortcut” tab.
The “Target” field will read: “C:\Program Files\Citrix\WinFrame Client\wfcmgr32.exe”. Edit the executable filename to: “wfcrun32.exe”.
After the second double-quote insert one space and type the name that was entered in the description field.
Note: This Must be Copied Exactly. For Example, in double-quotes, the name of “WLS” would be entered, I.e. “C:\Program Files\Citrix\WinFrame Client\wfcrun32.exe” “WLS”.
Close the “Remote Application Manager Properties” window.
Configuring the WLS Desktop
Starting the WinFrame Session
Double click on the “WLS” icon. The WinFrame session will initiate and bring you into a log on prompt. In the “From:” field will be the server name description.
Type in the userid and password.
Select “OK”. The WinFrame session will execute.
Win3.x-Thin Client Conversion
Preparation Requirements
Win3.x workstation with properly installed and configured TCP/IP connection WinFrarne server IP address.
Installing the WinFrame Client
Insert WinFrame client disk into drive.
Select “Start”, then “Run”.
Type “A:\setup”.
Allow all default installation parameters.
Configuring the WinFrame Client
Double click on “Remote Application Manager” icon. At prompt to enter a new entry, select “No”.
Select “Options”, then “Settings . . . ”
In the “Settings” window select the “Server Browsing” tab.
In the “TCP/IP Address:” field type the IP address of the WinFrame server you wish to connect to. If you are connecting to a cluster, choose the domain controller.
Click “OK”.
Select “Entry”, then “New”.
Select the “Network Connection” radio button, click on “Next”.
In the “Description:” field, enter “WLS”.
In the “Network Protocol:” pull down menu, select “TCP/IP”.
In the “Server” field, select the WinFrame server or Cluster name you are connecting to. Click on “Next”.
In the “Add a new Remote Application window” click on the “Change . . . ” button.
In the “Windows Properties” window, deselect “Use default” checkbox
Select the “640×480” radio button.
Select “OK”.
Click on “Next”.
Leave the “Application:” and “Working Directory:” fields blank. Click on “Next”.
Click on “Next” and “Finish”.
Close the “Remote Application Manager” window.
Single click on the “Remote Application Manager” icon, select “File” then “Properties”.
The “Command line:” will read: “C:\WFC16\wfcmgr.exe”. Edit the executable filename to “wfcrun.exe”.
Insert one space after the .exe extension and type the name that was entered in the description field.
Configuring the WLS Desktop
In “File Manager”, install WLS icon file (WLS.ico, located in the shared directory) into the “C:\%systemroot%\system\” directory.
Single click on the Remote Application Manager Group icon.
Select “Properties”.
In the “Description:” field type “WLS”.
Double click on the WLS group icon.
Single click on the “Remote Application Manager” icon.
Select “Properties”.
In the “Description:” field type “WLS”.
In the “Program Item Properties” click on “Change icon . . . ”.
Click on “Browse . . . ”.
Find and select the “WLS.ico” file. Select “OK”.
Select “OK” again.
Single click on the WLS icon.
Select “File” then “Copy”.
In the “Copy Program Item:” window select the pull down menu bar and select “WLS”. Click “OK”.
Single click on the “WLS” icon.
Select “File” then “Copy”.
In the “Copy Program Item:” window select the pull down menu bar and select Startup.
Click “OK”.
Configuring the Wireless Networking Parameters
Caution: By configuring the Domain and Security ID, the PMA will only communicate with access points within the same Domain and with the same Security ID.
From the shared directory on the network drive, copy “r12setup.exe” to the c:\wfw311 directory.
If Windows 3.1x is loaded, exit Windows.
Using Notepad open the autoexec.bat file
Remark the line “wfw311\net start”.
Remark the line “win”, if installed.
Save the file and exit Notepad.
Press Ctrl-Alt-Del.
At the DOS prompt type “cd wfw311”.
Type r12setup.
Using the tab key, highlight “Continue”.
If the RangeLAN2/PCMCIA Setup Window appears, continue. Otherwise skip to step 14 .
Leave all defaults
In the “Directory:” window type “c:\wfw311”.
In the “Station Type” scroll-box, use the down-arrow to select “Station”.
Using the tab key, highlight “Advanced”.
Using the tab key, highlight “Network Domain” scroll-box, use the down-arrow to select “15”.
Using the tab key, highlight “Roam Config”, use the down-arrow to select “Fast”.
Using the tab key, highlight “Ok”.
Using the tab key, highlight “Ok”.
Using the tab key, highlight “Test/Utilities”.
Using the tab key, highlight “Security ID”.
In the warning window, highlight, “Continue”.
Enter the proper Security ID.
Highlight “OK”.
In the confirmation window, ensure “OK” is highlighted.
Highlight “Done”.
Highlight “Exit”.
Edit the Autoexec.bat file and remove the two remarked lines.
Save and exit Notepad.
Press Ctrl-Alt-Del
Changing the Client Security ID
If the wireless network security must be changed, follow the below procedures:
If Windows 3.1x is loaded, exit Windows.
Using Notepad open the autoexec.bat file
Remark the line “wfw311\net start”.
Remark the line “win”, if installed.
Save the file and exit Notepad.
Press <Ctrl>-<Alt>-<Del>.
At the DOS prompt type “cd wfw311”.
Type “r12setup”.
Using the tab key, highlight “Test/Utilities”.
Using the tab key, highlight “Security ID”.
In the warning window, highlight, “Continue”.
Enter the proper Security ID.
Highlight “OK”.
In the confirmation window, ensure “OK” is highlighted.
Highlight “Done”.
Highlight “Exit”.
Edit the Autoexec.bat file and remove the two remarked lines.
Save and exit Notepad.
Backbone Configuration in Accordance with a Preferred Embodiment
The WLAN design in accordance with a preferred embodiment is comprised of 4 ‘cells’ on three domains. One domain, including the access points in the gymnasium and nurse's station will handle all mobile clients in the school, as well as desktops located inside the gym; the other domains will be reserved for wirelessly attached desktops on each wing. Note that if desktops are physically moved from one wing to the other, some trivial WLAN driver reconfiguration must be performed.
Gymnasium Radio Configuration
The access point in the gym is a repeater product, with two radios: one is configured at a station and handles the uplink to the school backbone, while the other is configured as a master and handles all wireless client devices. The configuration for the station is identical to any wireless client connecting to the Primary Wing; the configuration for the master is detailed below. FIG. 5 is a gym radio configuration in accordance with a preferred embodiment.
Nurse's Station Radio Configuration
The access point in the nurse's station handles all mobile devices in the school, and is on the same domain as the access point in the gym. This will enable mobile devices to roam seamlessly, throughout the school, the grounds, and inside the gym. FIG. 6 is a nurse's station radio configuration table in accordance with a preferred embodiment.
Wing Radio Configuration
The access point in the primary wing handles all desktops in the primary wing. FIG. 7 is a wing radio configuration table in accordance with a preferred embodiment.
Configuration Tables
Radio Configuration
Hardware Configuration
Authorization Table
Thin-Client Friendly
A fundamental premise in accordance with a preferred embodiment is delivering centrally managed capability to distributed clients via ‘thin client/server computing’ principles. This means that all solutions maximize the benefits of having centralized complexity, work in MultiWin® (WinFrame/Terminal Server) environments and deliver acceptable performance.
Transparent to end-user
The educational sector is, as a whole, relatively inexperienced with enterprise class computing solutions. Computational experience must be designed for ease of use and complexity minimized and made completely transparent to the end user. Features in accordance with a preferred embodiment include deployment of single sign-on solutions, intelligent scripting to make configuration ‘decisions’ automatically, etc.
Scalability
Business forecasts includes deployments at very large clients. Solutions must scale into the hundreds of thousands of end users, distributed across hundreds of campus locations.
License Management/Software Metering
A system in accordance with a preferred embodiment is very similar to a service bureau. The system provides managed access to data and, most importantly, applications by which this data is accessed. Most, if not all, of these applications have been developed by a third party. In accordance with a preferred embodiment, a school district may purchase the rights to an office suite running concurrently on 75% of its workstations, or a math tutor running on 3%.
Requirements
License Management
A centralized repository for managing all licensed assets is necessary to serve as a check against real-life usage criteria, both manually in the case of ‘soft’ metering, and automatically in the case of ‘hard’ metering.
Application Usage Report Generation
It is necessary to have access to application usage historical data for many reasons. First and foremost, to ensure that the agreements we have in place are sufficient. If they have not purchased sufficient access to applications, these reports will serve as a valuable tool to justify additional licenses. Secondly, the reports will document which applications are heavily used by which classes of users to improve our ability to target value-added instruction/curriculum integration. Lastly, client school administrators will want to see these sorts of reports, both to audit our pricing, to perform budgeting and license capacity planning exercises, and to enforce ‘big brother’ disciplinary policies (“What! Johnny plays ‘Solitare’ 3 hours a day? I'd better talk to him . . . ”).
Hard Metering
For key applications: ‘hard metering’ will likely be required. That is, when concurrent usage reaches a predefined threshold, no additional copies of the application will be allowed to start. This relative ease of implementing such a tool is one of the key benefits of our centralized architecture.
Technologies
Note that all of these solutions require a repository to store license information as well as usage data. This is typically an ODBC-compliant database solution, such as a SQL Server by Oracle or Sun. This sort of repository will be required to support scalable manageability across many aspects of our solution domain, and is a large and important new addition to our conceptual design and cost model.
Distributed Enterprise Management
Enterprise Management utilities, such as IBM/Tivoli TME10 or Computer Associates Unicenter, perform license management, software metering, and much more: They are intended for large, distributed corporate environments and as such are overly complex and expensive to install and administer.
Specialized Software Metering
In fact, the high degree of difficulty involved with the deployment and maintenance of a Distributed Enterprise Management solution has led 75% of companies towards deploying a parallel, separate, specialized platform to perform license management. Some packages in this class include CentaMeter, ExpressMeter, LicenseTrack, LANLicenser, and SofTrack. These packages typically integrate with other systems management utilities, such as HP OpenView or Microsoft SMS.
Thin Client/Server Metering
At least one application intended to perform license management and software metering on thin client/server computing platforms has been developed.
Managed World Wide Web Access
Requirements
Content Filtering
A key component of the AC MEN solution is the efficient. Managed browsing of educational content on the World Wide Web. Students should be denied access to content deemed unacceptable as defined by state and local legislation, community standards of acceptability, and school policies.
Variable Access Levels
Granular control of this definition of acceptability, to be applied on a per-student basis (probably under the auspices of ‘age’ or ‘grade-level’ to simplify management) should rest in the hands of school administration. For ease of use, these access levels should ideally be integrated with a user's login privilege levels to allow seamless, single-sign on capabilities.
Content Caching
A common scenario involves having an entire class of students access the same internet content as part of a classroom activity. Thus, another important element of the AC MEN solution is the caching of frequently accessed content to speed access times and reduce the bandwidth required for external internet connectivity, leading to lower overall costs.
Monitoring and Reporting
By monitoring the activity to the Internet, it will be possible to produce reports that detail usage patterns. This will be valuable in forging partnerships with content providers, in developing a knowledge-sharing mechanism by which teachers can learn from each other's experiences, and in resolving any disciplinary issues that arise from unauthorized or improper activity.
Fault-Tolerance
There should be no single point of failure with regards to managed browsing. In the event of a failure, the detailed design for the specific opportunity will determine whether the connection fails ‘open’ or ‘closed’.
Customization Potential
A custom content filtering service is provided in accordance with a preferred embodiment.
Technologies
“Standard” Browser Capabilities
Both Netscape Communicator and Microsoft Internet Explorer have built-in management functionality. They are both able to use built-in RSAC/PICS Ratings, or third party software for more granular filtering. They both maintain a cache of frequently hit sites, although maintaining separate caches for each user is not an efficient or scalable approach. The ‘open source’ approach offered by Netscape allows any imaginable customization, albeit with significant skilled effort. The Internet Administration Kit (IAK) allows moderate customization of Internet Explorer; additional customization is possible by writing a browser that employs components of Internet Explorer.
“Custom” Browser Capabilities
Web-filtering (and other kid-friendly) features can be incorporated at the browser level by using third-party and/or custom programming. SurfMonkey, for example, is a specialized browser for children based on the Internet Explorer engine (using the component-driven method mentioned above). It features built-in granular content filtering, an integrated ‘start site’ with kid-friendly content, filter chat rooms for children, and a customized interface.
IWS ChildProof Proxy
This solution is currently deployed as a component of the Test/Pilot architecture. The ChildProof proxy is a software-based content filtering proxy. It performs no caching. Developed by a small startup in Phoenix, its objective is to provide tailored content filtering for the educational sector. Currently, the solution is limited to Sun hardware and software platforms; in fact, it is the only element of the Test/Pilot architecture that runs on a non-Windows NT operating system.
In fact, all content access levels are assigned on the basis of IP address, which offers NO granularity in a thin-client environment. Furthermore, its content filtering is based on a simple list of pre-defined IP addresses or Fully Qualified Domain Names (FQDN); no keyword or image analysis filtering is implemented. Given the dynamic nature of the World Wide Web, this approach has been rejected by most major filtering solutions. It is not even possible to block access to part of a site (such as certain areas of AOL) and allow access to other areas; this is important, as many sites aimed at students are hosted by ‘amateurs’ using a web hosting service rather than corporations with their own domain names. The default list is woefully inadequate; sites as obvious as, for example, http://www.sex.com/ are not blocked automatically. This solution supports ONLY HTTP traffic (IP traffic on port 80 ); no proxying of other protocols (including HTTP-S or FTP) is performed. Lastly, this platform has suffered from reliability issues. Because it does not support load balancing among redundant peers, the proxy acts as a single point of failure: if the machine becomes unstable for any reason, users are unable to access all internet content. The immaturity of the codebase has in fact led to several such outages in the Test/Pilot environment
Standard Proxy Server Capabilities
The two industry leading firewalls are Netscape Proxy v3.5 (the current standard for Andersen Consulting's internal network) and Microsoft Proxy v2.0. In their most recent versions, these two products have very similar functionality. These products are software-based cache proxies. Their core functionality is to act as a proxy between web clients and the firewall to allow for better security, and to cache content to reduce the number of requests that must be fulfilled over the Internet. With the addition of optional components (plug-ins), it is possible to extend their functionality to perform detailed content filtering, report generation, virus scanning, and more. The Netscape product runs on Windows NT and UNIX platforms; the Microsoft product is NT-only. Both of these products support integration with the Microsoft Domain Authentication scheme, allowing access levels to be defined according to domain groups via a single sign-on. Several popular content filters (with broad brand recognition) are available as plug-ins, including SurfWatch, CyberPatrol, SmartFilter, and X-Stop; these products offer keyword-based filtering in addition to the URL filtering available as a part of the base proxy. The databases associated with these commercial products are huge and well established. Plug-ins, such as WebSense, ProxyReporter, ProxyReport, and Telemate, allow the automatic generation of reports tracking which URLs were accessed (or attempted to be accessed) by specific users. Virus-scanning plug-ins are available from TrendMicro and Network Associates. Rapid, efficient caching is a standard feature of both products. Support for many protocols, including HTTP. HTTP-S, FTP, and others is standard, as is support for SOCKS v5 proxying to allow many non-standard, application level traffic streams to be proxied. These products also support automatic configuration of browser software, to simplify implementation and maintenance. Also, both Microsoft and Netscape permit load-balanced and redundant architectures, with interproxy communication via the CARP and ICP protocols. Furthermore, each of these products has a well established API allowing for extensive customization via the coding of new plug-ins.
Comparison Matrix
FIG. 9 is a comparison matrix of various features in accordance with a preferred embodiment. In accordance with a preferred embodiment, a solution using Microsoft Proxy Server 2.0, or Netscape Proxy Server 3.5, depending on our partnerships. Use customized browser for branding (either 3 rd party, like Surf Monkey), or something homegrown (using Mozilla source code or Micrososft IAK or APIs). Leverage 3 rd party childrens ‘portal’ site, such as Disney's Dig or Yahoo's Yahooligans rather than maintaining independent lists of ‘start sites’. Not only will this reduce costs, but we can likely realize some sort of additional revenue stream by partnering with one of these providers.
Remote Access
There are several compelling sales messages associated with remote access. This allows teachers to prepare lessons from home. It might allow students to do their homework online, thereby obviating ‘the dog ate my homework’ scenarios. It also potentially provides access to educational content for children who are disabled or ill. The thin-client architecture employed in the Managed Education Network is perfectly suited to remote access scenarios. The hardware and operating system requirements for all remote access terminals are very low, enabling students, teachers, and school administrators to access modem applications with the PC they may already have at their house.
The most difficult part of enabling remote access will be ensuring adequate network connectivity between remote locations (homes, libraries, etc.) and the AC-MEN data center. Because of the relatively low bandwidth requirements, connectivity is possible over a variety of access media (albeit with varying performance); in fact, heterogenous remote access architectures can be developed, as the ICA protocol stream will run over a variety of network types. The challenge is to develop and sell a remote access solution that serves as wide a customer base as possible, is easy to implement and maintain, and is cost effective.
Requirements
“Universal” Geographic Availability
All students, teachers, administrators, and community members should have a means to access their desktop remotely, regardless of where they live or which carriers currently provide them with service.
Security
All authorized users should be able to safely and securely access educational and adminstrative data and applications remotely; no unauthorized users should be able to access these data or applications, or prevent authorized users from doing so.
Access Technologies
These include running an ICA client over a public, ISP-managed, network. We should also seek to understand the capability differences and required infrastructure between standalone and web-browser based clients. These architectures and client types potentially serve a wider customer base, with easier installation and support, for lower cost, than our current private analog dial-in solution provides.
Analog Dial-Up
The technologies that form the core of the thin-client paradigm were originally developed to enable remote control access over standard dial-up lines (at the time, operating at 14.4 Kbps). At such low connection speeds, these technologies provided all the functionality of the desktop from remote locations, but certainly not the experience. Clicking GUI widgets (particuliarly drop-down boxes) would introduce a noticable lag time. This sort of performance would be unacceptable if delivered by an application on the local desktop; in a remote control situation, users were able to overlook mediocre performance, particuliarly because the alternative was likely a long drive into the office at inopportune hours.
Since those early days, a few developments have changed the playing field. Connection speeds have slowly crept up; the adoption of the V.90 standard has meant that analog dial-up downstream rates of 40 Kbps or more are quite common. These larger pipes mean that the GUI sluggishness experienced in standard application usage is much less severe. However, in this same time period, the Internet has also emerged as the ‘killer app’. The graphically intense nature of the World Wide Web makes performance over a low bandwidth network less than ideal. This problem is exacerbated when users have to scroll down a page; this requires the screen to be redrawn and sent over the dial-up connection very frequently, increasing bandwdith requirements. The upshot is that users typically percieve worse performance when browsing the web over a dial-up connection to a MultiWin server than they would if accessing Internet content over the same dial-up connection from a local browser.
Despite these performance issues, analog dial up is still a very viable remote access option. While the experience at home is generally worse than it would be in a school, the functionality is identical. Analog Modems are inexpensive, supported by nearly every conceivable hardware and operating system platform, and relatively easy to configure. Telephone lines (at least domestically) are, by definition, universal.
ISDN Dial-up
Integrated Subscriber Digital Networking (ISDN) is a technology wherein digital signals, rather than analog, are exchanged between the residence (office, library, etc) and the phone company central office (CO). This effectively raises the throughput over a normal pair of copper wires universally deployed to 128 Kbps, which is more than adequate for several concurrent thin-client sessions.
The problems with ISDN are largely due to its limited availability. Although this technology was invented at about the same time as disco, the large infrastructure investments required by telephone companies (replacing all analog switching gear with digital equivalents) led to very slow deployment. ISDN terminal adapters are more expensive than their modem counterparts, as are the usage (per-minute) fees.
Cable Modems
Recently, efforts have begun to leverage the coaxial cable used to broadcast Cable Television to many homes as a broadband network media. Data throughput rates over typical implementations varies between 50 kbps to 1 Mbps, and hence could certainly be used to connect small schools, as well as home users, to the data center backbone.
However, widespread adoption of cable modem technology faces several large challenges. First and foremost, a high quality two-way hybrid fiber-coaxial (HFC) network needs to be run to the premises. This requires the provider to supply approximately $250 worth of equipment over and above normal one-way Cable TV (CATV) networking. Note that extremely rural areas may not even have the required CATV infrastructure. Some providers have been deploying HFC networks aggressively, but overall they are still far from commonplace; widespread distribution is likely several years away. Al so, no standard implementation yet exists: equipment, services, and pricing is still very proprietary.
Lastly, because cable modems are implemented using a shared broadband medium, there are some security concerns. It remains to be seen how severe these issues are, and what technological solutions will emerge to overcome them. Using VPN technology should provide more than adequate security for our users.
xDSL
Another recent effort to greatly improve data connectivity to the home involves leveraging the same pair of copper wires used by traditional analog and ISDN. Digital Subscriber Loop is an alternative digital standard which makes use of asymmetric data distribution properties to achieve very high downstream throughput rates.
Like cable modems, xDSL technologies face huge hurdles. The shocking lack of standardization in implementations has led to an alphabet soup (ADSL, HDSL, RADSL, VDSL, IDSL, etc.) of different, proprietary, incompatible, schemas. There are severe distance limitations between the residence and the CO. And carriers have only just begun installing the back-end, DSL access multiplexors (DSLAMs) necessary to support this service. It remains to be seen whether either cable modems and xDSL deployments (or both) will succeed, of if they will spawn another overhyped and underutilized access technology, like IDSN.
Internet
The above approaches involve leveraging a private or, more lkely, semiprivate access infrastructure, most likely built and maintained by our carrier/telco partner. It is also possible to remotely access a centralized, thin-client/server desktop over a public infrastructure, the Internet. In many cases, students and teachers already have Internet access from remote locations (sometimes, this access is subsidized/sponsored by educational agencies already). Leveraging this connectivity instead of maintaining a separate, parallel, access infrastructure is potentially a large cost savings, in addition to being much easier to install and support.
There are, of course, tradeoffs involved in using the Internet as a access medium. No performance guarantees are possible; latency will vary widely depending on ISPs, backbone providers, and instantaneous traffic conditions. Security is also a large concern; precautions must be taken to ensure that unauthorized or malicious attempts to access system resources and data or deny service to legitimate users are thwarted. Such precautions probably include careful configuration of choke routers and firewalls, and authentication via Virtual Private Networking (VPN) technologies. Note that VPN technologies are highly proprietary, and evaluation and selection will depend largely on the security architecture implemented by our carrier provider.
FIG. 10 is a comparison matrix of various communication features in accordance with a preferred embodiment.
In accordance with a preferred embodiment, Internet connectivity is used to enable users to remotely access their educational desktop remotely over the Internet. Carrier analog dial-up services are leveraged rather than installing/maintaining private POPs. In accordance with a preferred embodiment, the following dial up access functions are provided by the carriers:
PPP connection
dynamic IP address allocation,
maintenance of dial-up platform,
authentication/security implementation (RADIUS, TACACS+, etc.)
upgrade of network capacity,
support for routing private IP addresses,
disaster recovery,
p.01 Grade of service,
user account management function,
help desk support,
management reports
All customer-facing support (installation, troubleshooting, etc.)
Investigate offering alternative carrier-hosted dial-up services (such as ISDN) as a option
Use Authentication/VPN technologies to prevent abuse
Set expectations of decreased performance over Internet/Analog Dial-up with users prior to deployment
Multimedia
It has become increasingly obvious that supporting the information services needs of the educational sector is far different than supporting those same MIS needs in corporate environments. One important differentiation is the simple nature of the information services it is necessary to provide; the office suites and productivity applications that form the mainstay of the ‘traditional’ business user's computing desktop are but one (albeit important) element in an educational solution. Teachers and students also require access to specialized content and applications whose very nature presents new delivery challenges.
Objectives
Support Multimedia Rich Educational Internet Content
Many educational sites on the Internet deliver graphically rich content via ‘plug-ins’, such as Shockwave or RealAudio. While the limited throughput and relatively high latency of the Internet means that the quality of this content is relatively low, in most cases it is still much higher than the standard thin-client data stream can support. That is, multimedia Internet content viewed on a standalone workstation is of better quality than on a thin client device. In most cases, however, this content is still usable (now that audio delivery is supported in certain configurations).
Support Multimedia Rich Educational Applications
Educational software packages (including reference works like MS-Encarta) often make use of high quality multimedia content. Quality rendering of this content is often necessary to successful usage of these applications. The new breed of digital reference works include audio, video, and even ‘virtual reality’ content, in addition to the ‘stuffy’ text to which society been shackled for the last several millenmia, education packages (including learning games like ‘Math Blaster’ or ‘Carmen Sandiego’) often have lavish graphical and audio interfaces. In an effort to entice students into consumption of content, increasingly ‘flashy’ and ‘absorbing’ contexts are being developed. Studies have shown that programs that ‘reward’ correct answers or responses with a multimedia treat are rather ineffective in promoting true, lasting learning; nevertheless, these sorts of applications are very popular with teachers, parents, and students alike.
Support Distance Learning
The learning systems of tomorrow are likely to have even greater interface requirements. The concept of ‘distance learning’, wherein true content experts can remotely deliver lessons that are ignored by students irrespective of geography, is increasingly finding its way into visions that describe the schools of the future. These sorts of systems typically require full motion video delivery; in some scenarios, upstream video broadcasting is also necessary. Note that some forms of ‘distance learning’, such as training packages like those offered from CBT Systems, don't require such high-end multimedia delivery. This sort of moderation is quickly falling out of favor.
Technologies
Standard, Thin-client Architecture
The thin-client remote control technology employed by Citrix and Microsoft works by establishing a number of data channels between the client and the server. The screen display data channel uses a protocol that only allows for 256 colors, and has significant latency that is in practice often limited by network conditions. Even under ideal conditions, however, this ‘ThinWire’ protocol cannot display rapidly updating graphics, such as those found in animation or video clips. The WinFrame product from Citrix does not include an audio data channel; therefore, remote ICA clients connected to a WinFrame server cannot play sound from applications running on that server. Sound is of course an important element of any definition of multimedia. Sound is available for remote ICA clients connected to a Windows Terminal Server/Metaframe platform.
Out of Band, Parallel Video Distribution
It is possible to deliver improved multimedia capabilities via a parallel architecture; for example, the CorelVideo product from Corel. This solution is a delivery vehicle for traditional video content (NTSC/PAL). That is, any traditional analog video signal (from VCR, Cable TV, even Video Conferencing with the right equipment) can be delivered to the ‘desktop’ via an unused pair inside a Cat3/Cat5 RJ45 cable. One configuration of this solution is a Linux-based thin client with a built-in video CODEC. The thin client has both a standard data network connection, and an analog video input. A software package ‘switches’ between traditional ‘thin-client’ and ‘video’ modes. The data and video cables are both connected to a splitter, which muxes the signals’ together over the same physical RJ45. This runs (not more than 300-500 ft) to the wiring closet and into a Corel proprietary patch panel, where the data channels are demuxed and patched into the hub/switch, and the video channels run over a separate trunk line into a proprietary Corel Video Server with line cards. This server serves up MPEG encoded video, or is connected to VCRs or standard Cable Television, etc. If dark fiber is available, you can trunk servers together in multiple locations.
This solution does not fulfill our requirement to be able to serve graphically intensive applications in-band. It is not well suited to a centralized architecture, because there is no efficient way to centrally manage video content (not only would it be cost prohibitive to trunk all servers in schools to a centralized data/video center, but dark fiber is simply not available for wide area links from most carriers.) Another alternative involves using digital video sources, such as MPEG, rather than analog. This would at least enable wide-area, centrally managed content, and would obviate the need for changes to the physical infrastructure. Thin clients from vendors such as Tektronix enable this sort of solution. Unfortunately, this also would not enable graphically intensive applications in-band.
Locally Served Thin Clients (DirectICA)
In the absence of working, centrally-managed thin client solutions that enable multimedia delivery, it may be possible to enable much increased functionality via a distributed thin client architecture. This would preserve most of the simplicity of the user devices, a guiding principle towards lowering cost of ownership, but would distribute server complexity to remote sites. These servers could be locked down (logically and physically) to make them far easier to support than local desktops.
One way to accomplish this is via the DirectICA solution available via WinFrame and Metaframe. A local server running either WinFrame or WTS/Metaframe can be outfitted with several multiport VGA adapters. These adapters deliver analog video signal (in much the same way that the CorelVideo solution does) to thin client-like devices up to 300 ft away. Because these remote devices are literally nothing more than user interface terminals, they can display video output with the same fidelity as a locally attached monitor.
It may also be possible to deliver analog (NTSC) video content from sources such as broadcast and cable television, VHS VCRs, Laserdisc and DVD players, etc. Several TV Tuner & Video Capture cards are supported under Windows NT4.0, including the Hauppauge WinCast. Testing to determine compatibility under Windows Terminal Server and Metaframe, as well as interoperability with the DirectICA video cards, would be necessary to determine the overall feasibility of this solution.
Thick Multimedia Terminals
By resorting to a distributed architecture, its possible to enable nearly all conceivable multimedia functionality. However, the cost end effort required to implement and support this sort of architecture is potentially prohibitive; this is in fact the architecture that we advocate migrating away from in the first place.
FIG. 11 illustrates a comparison matrix of thin client features in accordance with a preferred embodiment. In accordance with a preferred embodiment, a locally served thin client architecture is enabled utilizing DirectICA. Local servers are used for print queues, DHCP, etc. to improve perforformance, functionality, and stability of other local ‘traditional’ thin clients. Analog (NTSC) video is delivered in accordance with a preferred embodiment over DirectICA infrastructure.
Wireless Detailed Description in Accordance with a Preferred Embodiment
Introduction
Several applications call for network access in areas where traditional wired connectivity is unsuitable. There may exist physical or economic barriers to running network cable, or users may require flexibility not afforded by wired connections. Typical scenarios include a remote building with a relatively small number of network users on a corporate campus, or a warehouse floor where inventory must be performed. In certain scenarios, these needs are met via the installation of a Wireless Local Area Network (WLAN).
A number of factors influence the design decision to institute local area wireless support, as opposed to wide-area, “cellular”-type technologies. Where business requirements allow it, local area technologies typically over greater throughput and more seamless integration into existing networks and systems. WLANs may offer greater end-user device options. Sending sensitive data over public carrier-based solutions may be unacceptable. Whatever the reasons, it is important to bear in mind the relative immaturity of wireless technologies in general. The state of the art is constantly evolving, for both local and wide area technologies, and that future developments made alleviate some of the above concerns. For example, satellite-based technologies will make global deployments extremely feasible (at the cost of increased expense and lower throughput).
Note that WLAN technologies certainly have their limitations. At present, they offer very limited throughput (less than 2 Mbps/user) at high costs (5 times the price of wired connections). Additionally, cross-vendor interoperability is non-existent, resulting in an extremely fragmented and unstable marketplace. In general, WLANs are suited only for specific, niche applications; i.e., vertical rather than horizontal deployment.
Design Methodology Guidelines
Ideally, WLAN design would be a three phase approach. A preliminary design should be produced, the conclusions should be tested in a physical on-site survey, and the survey results should be used to revise and refine the design.
Preliminary Design
The preliminary WLAN design does not necessarily require physical access to the area to be supported. Establishing good lines of communications with important user contacts, and acquiring key documentation, should enable much design work to occur from remote locations.
Determine User Requirements
A number of different wireless connectivity scenarios exist as a function of user requirements. Two examples include the highly mobile equipment maintainer who requires seamless wireless connectivity across a large contiguous area, and the small remote facility with no existing communications capability that requires LAN access. These, and other, disparate scenarios may require vastly different equipment and architectures. It is essential to accurately determine user requirements before beginning a WLAN design, and to incorporate any changing requirements in a logical and timely fashion. Note that gathering user requirements prior to beginning the design phase will enable detection of any unfeasible demands, and allow the opportunity to set realistic expectations.
Acquire Physical and Network Maps
Getting an idea of the size and shape of the area to be covered, as well as the approximate location of any major obstacles, impediments, and potential mounting locations, is essential to performing a wireless network design.
Furthermore, the WLAN will undoubtedly require integration with the existing wired network installation. The wired network topology will strongly influence WLAN design decisions. For example, wireless clients will typically only be able to roam between access points on the same LAN segment; routers will impede the seamless ‘hand-off’ to a new access point. Getting accurate network maps is a crucial step in analysis and design of the wireless/wired network interfaces.
Perform Product Evaluation and Selection
Based on user requirements, physical constraints, and network topology, it should be possible to select the WLAN vendor and products that will be implemented as a part of the total solution. Note that the current state of the art does not allow for cross-vendor interoperability; selection of a WLAN vendor will determine which client devices will be able to use the fielded network. It is also important to consider several non-technical factors when choosing a vendor; the long-term consequences of this decision will require selecting a vendor with adequate support, and who is likely to survive the market shake-out that will occur over the next few years.
Each WLAN vendor is likely to have several product offerings to meet different requirements. For example, a vendor may offer products with different transceiver strengths (100 mW vs. 500 mW) or different network interfaces (Ethernet vs. Token Ring). Early determination of all relevant and realistic products will enable administrative work and detailed design to begin.
Obtain Frequency Approval
WLAN devices utilize portions of the radio spectrum to communicate. Their use may be governed by local, regional, or national regulatory bodies or agencies. It is extremely important to coordinate with all applicable bodies before attempting to design and implement a WLAN. Note that the low power employed by typical WLAN transmitters will ease regulatory concerns. Also, most WLAN products currently shipping operate in 2.4 Ghz range, which has been set aside by many national agencies for unlicensed Industrial, Scientific, and Medical commercial utilization. Certification may require complex paperwork with lengthy approval cycles to be filed by equipment manufacturers or integrators.
Perform Initial Research and Testing
Only by learning a great deal about the theoretical and practical capabilities of the relevant access point and antenna options can efficient and accurate detailed design commence. Exact capabilities will depend a great deal on environmental conditions, but the WLAN architect should become very familiar with generalized range and throughput properties, as well as understand the strengths and limitations of the hardware and architecture in question. There is no substitute for hands-on experience with the equipment, which can be obtained prior to site surveys and implementation, at least in part, by testing the actual equipment to be used in a staging area.
Prepare Preliminary Design Document
With the above information, it is possible to produce a preliminary design showing projected locations and configurations of WLAN equipment. For example, rough templates of the approximate coverage area associated with each access point/antenna pair can be constructed to the scale of available physical maps. These templates could then be overlaid on the maps in question to assist in determination of optimal access point/antenna placement. The design goals will vary from installation to installation, but the following factors are likely to have significant impact:
1. Minimize number of access points needed to cover a given area
2. Place access points to facilitate in-field diagnostics and maintenance
3. Place antennae to minimize field effects (‘RF shadowing, ‘Multipath’, ‘Near-far’, ‘Hidden receiver’ phenomena) and improve network performance
4. Place access points to ease integration with wired network
Site Survey
After completing a preliminary WLAN design approach, the physical site should be surveyed to test and identify variances with this design.
Obtain and Coordinate Resources
Several relevant resources are required to conduct a thorough and complete site survey. Also, there are potentially several administrative functions that should be performed prior to arrival on site. Coordination may include the following steps
1. Obtain permission to enter the site, including all areas to be serviced by the WLAN or slated to host equipment
2. Schedule sufficient time with appropriate human resources, such as those individuals who will be performing the actual survey, site custodians, and network managers
3. Obtain appropriate equipment to support in-field evaluation of WLAN performance. For example, if plans call for access points/antennas to be mounted in unusual places, schedule resources to enable temporary mounting of representative equipment in these locations.
Perform Walkthrough of Planned Installation
A thorough physical inspection of the areas to be serviced by the proposed design may yield important information that will lead to design modifications. For example, areas may have unexpected vegetation that would impact radio signal propagation, or locations proposed to host access points may prove unsuitable.
Obtain Relevant Documentation
Detailed power, network, and structural documentation should be obtained to flesh out detailed design requirements. This documentation should be carefully reviewed for issues that will impact design decisions.
Perform Field Performance Testing
Representative WLAN equipment should be temporarily mounted in each location. Detailed and comprehensive performance statistics should be captured using a benchmarked test platform. The effective coverage area served by each access point/antenna pair should be mapped. Also, representative throughput information should be captured. Several scenarios can arise where strong radio signal strength does not produce correspondingly high effective throughput rates; this usually indicates the presence of undesired radio field effects, such as multipath.
Detailed Design
After conducting the site survey, a finalized detailed design can be produced. Several of these steps can occur in tandem with the site survey; preparing documentation and comparing with expected results can lead to an iterative process that produces the best design quickly.
Prepare Site Survey Report
Timely and through documentation of all information gleaned during the site survey will expedite the detailed design process. It will also prove invaluable during the implementation and testing of the WLAN.
Compare Site Survey Results With Preliminary Design
The results obtained during the site survey should be carefully compared with the expected results around which the preliminary design was based. Variances should be carefully noted. If the observed results are unsatisfactory, the preliminary design should be revised, and additional testing should be performed.
Prepare Detailed Design Document
The detailed design should be a revision and expansion of the preliminary design. If the results observed during the site survey are unsatisfactory, the preliminary design should be revisited and revised to achieve desired performance. Additional testing may be required. Additional detail should be provided with regards to physical WLAN installation requirements, WLAN-wired network integration details, and expected serviceable WLAN coverage areas and qualities.
Prepare Installation Plan Document
A detailed document to enable an efficient and flawless installation of WLAN hardware should be produced. In most cases, the personnel responsible for planning and design of the WLAN will not be responsible for performing the actual installation; in many cases, they will not even be present. Therefore, it is absolutely critical that this document be produced with great care, and with an eye towards clarity.
Optimize Channel Utilization
Most WLAN systems have several channels within the prescribed frequency band. These channels can be used to maximize the available network bandwidth. WLAN equipment tuned to the same channel will share the same bandwidth; therefore it is of great interest to minimize the number of radio units employing a given channel. Channels can be efficiently recycled with sufficient separation.
The number of available channels will depend on the WLAN vendor; note that it is not necessarily a given that a greater number of channels available will mean a greater practical throughput within a given area. For example, frequency hopping spread spectrum techniques generally rely on designating several orthogonal subsets of frequency hops from the total number available in the given bandwidth. Squeezing additional channels into the same total band will reduce the orthogonality of the channels and increase the probability that cross-channel interference will occur leading to throughput reduction. It is the responsibility of the WLAN vendor to optimize the total number of available channels, but it is the responsibility of the WLAN implementers to utilize these channels effectively.
In an optimal setup, each service area (be it user-servicing access point or wireless bridge link) would have its own channel. This is not always possible. A design criteria should be to reuse channels for area/links that are physically separated and of lesser importance. Effective channel utilization can be reduced to a relatively simple algorithm.
1. Identify all access point locations and service areas on a map of the coverage area. Note that each wireless bridge link has both a master and a station. While the channel is not configured on the station, it still receives and transmits on that channel and hence must be considered in the channel planning stage.
2. Label each service area with a unique channel identifier.
3. When channels are depleted, seek to reuse channels in service areas that are physically disparate. It may take several revisions to produce an optimal channel set up. This is a mostly trial and error process, but guidelines for efficient allocation may be available in the ‘cellular’ section of wide area wireless networking resources, as this is essentially the same problem wide area carriers deal with in their “cellular” installations.
4. Construct table of access point configuration information and check for consistency.
Design Roaming Strategy
If large contiguous areas are serviced by multiple access points, it is often necessary to ensure that efficient roaming occurs. ‘Roaming’ is the process by which a mobile WLAN user is seamlessly ‘handed-off’ from one access point to another. Several factors will influence the ability to roam: not only must the mobile WLAN unit be properly configured to communicate with all relevant access points at the physical and data link layers, but the WLAN unit must also be configured to communicate with the wired LAN at the network layer. The practical implications of this will depend on the WLAN product and network topologies involved, but it may mean that
1. All roaming radio units must have the same logical ‘domain’ and security settings, and
2. All roaming radio units must be located on the same logical network segment.
For example, if two access points are located on different network segments, it is unlikely that roaming will be possible. The network address of the mobile unit will be valid for one segment, but not the other, and correct routing will not be possible. Note that several technologies to circumvent this problem (Mobile IP, Mobile IPX, IPv6) are in development; few of these solutions are currently available on a wide-spread basis.
General Frequency Issues
Frequency issues surround nearly all details of WLAN performance and implementation, including signal propagation, maximum data throughput, and administrative licensing and coordination. A number of different and incompatible frequency ranges and modulation schemes are employed by various WLAN implementations; in fact, three are specified in the IEEE 802.11 ‘standard’. Successful WLAN design demands a thorough understanding of frequency and its myriad implications.
Signal Propagation
In general, lower frequency signals have much better propagation than higher frequency signals. Consider the typical car stereo: when sufficiently loud, the low, thumping bass propagates well outside the vehicle, whereas the high treble sounds are completely muffled by the car body. This same effect is evident in WLAN signal propagation. Radios with similar power output that operate at 900 Mhz have better range than those that operate at 2.4 Ghz, which in turn have better range than infrared devices.
Maximum Data Throughput
In general, lower frequency signals have smaller theoretical data throughputs than higher frequency signals. While part of this is attributable simply to the smaller number of bits that can be modulated over the simpler carrier wave, the problem is compounded by the relatively small spectrum bandwidth devoted to WLAN applications in the crowded, lower frequency ranges. Radios operating at 2.4 Ghz have higher throughputs than those operating at 900 Mhz, and WLAN vendors are looking to the 5 Ghz band to provide even higher speeds.
Licensing and Coordination
In general, lower frequency signals face greater danger of interference than higher frequency signals. Applications using the 900 Mhz band are actually quite common, owing largely to the low cost of the radios required to broadcast in this range. This greatly increases the effort needed to ensure that the WLAN fails to interfere with, or be interfered by, other unlicensed wireless devices, such as cordless phones. 2.4 Ghz radios have been newer to market, and have been relatively well protected by regulatory agencies; these devices face relatively low competition for airwaves. Infrared signals are employed by extremely common remote control devices; significant testing and coordination is a prerequisite to successful deployment. These factors are of course colored by the signal propagation in the relevant band (see above).
Bands and Encoding Schemes
Spread Spectrum
Direct Sequence Spread Spectrum
This is a technique by which the narrowband data signal is transformed by a wideband spreading signal known to both receiver and transmitter, resulting in a composite wideband signal which is then transmitted. The inverse operation is performed by the receiving station to regenerate the data signal. This encoding scheme allows for channels with relatively high throughput rates, typically around 10 Mbps. However, the ‘stacking’ of these channels in the frequency band is inhibited by technical and regulatory legislation, typically resulting in less aggregate data throughput than possible with other spread spectrum techniques. In addition, this technique is fairly sensitive to interference, and environmental conditions that may only lower the throughput of some radios may completely preclude the use of DSSS-based devices. Lastly, the wideband signal transmission results in high power consumption, which is often unsuitable for wireless, mobile, applications. DSSS was quite common in first generation WLAN implementations, but has generally fallen out of favor with the wireless community. Lucent is the industry-leading DSSS radio vendor.
Frequency Hopping Spread Spectrum
This is a technique by which the transmitting and receiving stations very quickly hop from narrowband frequency to frequency in a pre-orchestrated pattern. This encoding scheme allows only for relatively low per-channel throughput rates, typically less than 2 Mbps. Unlike DSSS, however, properly designed FHSS channels can be stacked fairly densely, allowing for a large number of orthogonal channel hopping patterns to fill the same composite wideband spectrum and resulting in higher aggregate data throughput rates. This technique offers much higher interference immunity than most DSSS implementations, and consumes less power. Many former DSSS radio vendors now focus on FHSS techniques.
900 Mhz
This was the first band utilized by spread spectrum WLAN implementations, ranging from 902-928 Mhz. Typical implementations utilixed DSSS encoding, and experienced ranges of 100 m with throughputs of 500-800 Kbps. The 900 Mhz band quickly became saturated by unlicensed commercial devices ranging from cordless phones to garage door openers, and the relatively small bandwidth allocated to commercial devices left little room for performance enhancements.
2.4 Ghz
As the 900 Mhz band became increasingly crowded, and the inherent throughput limitations became increasingly evident, many WLAN vendors began looking to the 2.4-2.4835 Ghz band to provide much needed room for growth and expansion. By 1996, this became the de facto standard for spread spectrum implementations. Many of the propagation issues involved in moving to a higher frequency were overcome by focusing on higher power radios, still allowed by FCC Part 15 specifications for unlicensed operation. 2.4 Ghz FHSS and DSSS physical layers are specified as part of the IEEE 802.11 standard (see below).
5 Ghz
No sooner than vendors standardized on 2.4 Ghz and products began to achieve some degree of maturity, than the industry began looking for ways to further increase throughput. It quickly became obvious that even large data modulation developments would not allow per-channel FHSS throughput of greater than 8-10 Mbps in the 2.4 Ghz band. A standard called ‘HiperLAN’ was published in Europe in 1997 aiming at providing very high data rates (˜25 Mbps) for short distances using the open 5 Ghz spectrum. Adding to the incentives, the FCC recently allocated a large portion of the spectrum, from 5.15-5.35 Ghz and 5.725-5.825 Ghz, for unlicensed consumer applications. WLAN vendors are beginning serious research and development efforts in this band, and expect to release 5 Ghz products by 1999.
Infrared
Infrared WLAN equipment operated at 350 Thz, just below visible light on the radio spectrum. As such, most of the properties associated with light are applicable to IR WLANs. Their signals do not propagate through barriers, such as walls, and require higher power to ‘spread’ over a wide angle and fill a room. As such, IR WLANs are best'suited to point-to-point links and for short distance temporary ihtra-room connectivity. Many consumer devices are equipped with IrDA ports to enable a sort of short range IR WLAN. Infrared is one of the physical layers specified in the IEEE 802.11 standard (see below).
WLAN Standards
IEEE 802.11
On Jun. 26, 1997, the IEEE approved standard 802.11, dictating physical and media access control layers for wireless LANs. This standard in development for over seven years, aims at producing the sort of interoperability present in wired LAN technologies (such as Ethernet) necessary to increase competition, lower prices, and prompt widespread adoption. Unfortunately, this standard defines 3 different physical layers (2.4 Ghz DSSS, 2.4 Ghz FHSS, and Infrared), specifies only low speed connections (less than 2 Mbps), fails to include contention management and inter-access point communications, standards, and includes several optional implementation details. The result is that IEEE 802.11 will probably not spawn true, useful, interoperability. It has, however, increased public awareness of WLAN technology, and many vendors will likely work together to ‘fill in th holes’ in the standard and work towards interoperability on their own.
OpenAir2.4
Disappointed by the results of the IEEE 802.11 effort, a coalition called the Wireless LAN Interoperability Forum (WLIF) formed to support WLAN technologies. Unlike IEEE 802.11, this is a complete end-to-end standard completely specifying everything necessary for interoperability using a 1.6 Mbps, 2.4 Ghz FHSS implementation. Also unlike IEEE 802.11, however, this is primarily a single-vendor effort with support from OEM partners.
MobileIP
Existing wireline-based LAN technologies used by WLAN implementations do not easily allow for client mobility, one of the primary reasons to implement a WLAN. For example, were a client to roam from an access point on one subnet to an access point on a different subnet, its IP address would no longer-be valid and network communication would be inhibited. A standard called MobileIP has been adopted allowing for the automatic re-direction of network traffic to mobile clients. This requires a specialized, proprietary, and expensive IP stack at the client, and the deployment of ‘foreign agents’ which sense the movement of the client and ‘forward’ all designated packets accordingly. IPv6 has built-in mobility awareness. It remains to be seen whether IPv6 will be implemented quickly enough so that most WLAN applications can avoid the complications of MobileIP altogether.
WLAN Technical Details in Accordance with a Preferred Embodiment
Product Details
Technical details for a Wireless LAN architecture are described in accordance with a preferred embodiment. All RangeLAN2 products offer 15 non-interfering OpenAir 2.4® Frequency Hopping Spread Spectrum channels in the 2.4-2.483 Ghz ISM band of the spectrum, operate at a maximum data rate of 1.6 Mbps, and meet FCC Part 15 regulations.
RangeLAN2 7510 Ethernet Access Point (AP)
This product is a transparent bridge between a wired Ethernet port and a wireless radio interface. It can be configured through a command line interface accessed via its Configuration, Ethernet, or Radio ports.
Ethernet Port:
10BaseT (RJ-45) or 10Base2 (BNC)
Antenna Port:
Reverse BNC
Configuration Port:
Serial (DB-9)
Radio Power Output:
100 mW
Operating Temperature Range:
−20 to 60 C.
Operating Humidity Range
10-90%
Weight:
1.5 lb
Size:
8.54″ × 6.54″ × 1.66″
Input Voltage:
10-18V (DC)
RangeLAN2 7520 Manageable Ethernet Access Point
This product is similar to the 7510 AP-II, but features additional memory to offer enhanced management capabilities and node-caching performance. Its command line configuration interface can also be accessed via analog phone lines through a modem direct-attached to its Configuration point; additionally, it features a Web browser interface accessible via its Ethernet or Radio ports. The 7520 also offers full SNMP compliant remote monitoring and management via its Ethernet and Radio ports using standard 802.1D and proprietary MIBs. Lastly, the 7520 can be configured to distribute software updates to other 7520 access points on the WLAN or wired Ethernet segment.
RangeLAN2 7530 Manageable Token Ring Access Point
This product is similar to the 7520 AP-II, but features a 802.3 Token Ring network interface rather than 802.2 Ethernet.
Token Ring Port: STP (DBP) or UTP (RJ-45)
RangeLAN2 7521 Extended Range (XR) Access Point
This product is not yet shipping, so information is subject to change. It is essentially similar to the 7520 AP-II, but features a 500 mW radio.
RangeLAN2 7550 Extend Point (EP)
This product is not yet shipping, so information is subject to change. It is essentially similar to the 7520 AP-II, but features two 100 mW radio interfaces rather than a radio interface and an Ethernet interface. Its expected power consumption is slightly lower than the 7520.
RangeLAN2 7551 Extended Range Extend Point
This product is not yet shipping, so information is subject to change. It is essentially similar to the 7550 EP, but features two 500 mW radio interfaces rather than 100 mW interfaces.
RangeLAN2 740x PC Card
This product is a Type II PCMCIA transceiver.
Radio Power Output:
100 mW
Operating Temperature Range:
−20 to 60 C.
Operating Humidity Range
10-90%
Weight:
31 g
Size:
3.37″ × 2.13″ × 0.20″
Input Voltage:
5V
Power Consumption:
300 mA transmit
150 mA receive
<5 mA doze
2 mA sleep
Drivers Included:
ODI
NDIS 2.1, 3.1
RangeLAN2 7100 ISA Card
This product is essentially similar to the 740x transceiver, but features an ½ length ISA bus interface rather than a PCMCIA interface.
RangeLAN2 6xxx OEM Products
These products offer similar functionality to the 740x transceiver, but in a variety of OEM integratable form factors. Exact technical specifications will vary from integration to integration, and OEM vendors must ensure adequate performance and re-certify the final product with the FCC.
Other wireless LAN implementations, in accordance with alternative embodiments include:
802.11 Compliant Access Points and NICs
Parallel Port RangeLAN2 adapters
Ethernet Port RangeLAN2 Adapters
Protocol Details
Roaming
‘Roaming’ is the process by which stations automatically and seamlessly switch to which master they are synchronized. Roaming occurs when the observed signal quality does not meet the predefined criteria. This can happen due to the station physically moving out of range, varying radio conditions, or exceptions such as power failures servicing the master. Roaming does not occur for bandwidth reasons (i.e., a station will not determine that the current channel is too crowded and attempt to synchronize with another master).
Two user definable parameters control station roaming behavior. Roaming can be wholly disabled, and the ‘Roam Speed’ can be set to ‘Fast’, ‘Normal’, or ‘Slow’. ‘Normal’ roaming occurs when a transmission error percentage threshold is exceeded, and a new master is found with significantly improved signal qualities. ‘Fast’ and ‘Slow’ roaming speeds are less selective about the new master, and have lower and higher error thresholds, respectively. The exact error thresholds and characteristics that determine a ‘significantly better signal’ are not normally user-definable.
When the number of transmission errors exceeds a certain level, the radio first ‘falls back’ into a Binary Phase Shift Keying (BPSK) modulation scheme, which effectively cuts the throughput in half the normal mode of operation is Quad Phase Shift Keying (QPSK). If conditions do not improve, or worsen (note that,the exact algorithm is proprietary), the radio eventually attempts to roam. BPSK is also used for all broadcast packets, such as ICMP notices. Because of this, ‘ping’ is not an ideal network diagnostics tool.
Roam speed should ordinarily be set to ‘Normal’; this is the only setting that ensures that any new connection is better than the one previously abandoned. In an area serviced by many masters, ‘Roam Speed’ should be set to ‘High’ to allow stations to switch immediately after the signal degrades. In an area serviced by relatively few and far between masters, the ‘Roam Speed’ should be set to ‘Slow’ to encourage the station to maintain a degree of connectivity, albeit poor, with a master. If coverage is truly sparse, stations may attempt to roam and lose all connectivity whatsoever. In accordance with a preferred embodiment, stations sample link conditions if ‘Roaming’ is enabled, transmission errors are recorded, if the transmission error rate climbs above a certain defined level, stations fall back to a reduced throughput mode. If the transmission error rate climbs above the threshold defined by roaming speed, stations look for a new master. If ‘Normal’ roaming is enabled, the new master must have improved signal qualities, or it is rejected. If ‘Fast’ or ‘Slow’ roaming is enabled, the first new master is accepted regardless of signal quality. An IPX packet is sent from the new access point to the old one informing it of the roam.
Note that access points configured as stations, as in a bridging topology, have several additional roaming parameters. An ordered list of masters with whom to attempt synchronization can be defined by setting the ‘First Master to Sync With’, ‘Second Master to Sync With’, etc. parameters. This allows default and fall-back WLAN topologies to be explicitly defined to allow for planned redundancy without compromising network performance.
Collision Avoidance (CSMA/CA)
Normal collision detection algorithms, as employed by wired 802.2 Ethernet technologies, do not lead to efficient or equitable bandwidth utilization: the presence of radio phenomena such as ‘Near/Far’ and ‘Hidden Receiver’ reduce the effectiveness of these techniques, prompting the development of a proprietary Carrier Sense Multiple Access Collision Avoidance algorithm (CSMA/CA) in which potential collisions are prevented. Note that the protocol is acknowledged wireless collisions will result in unrecieved and hence unacknowledged packets, prompting a retransmission.
The CSMA/CA algorithm works as follows. All stations are kept in synchronization by the master access point. When a station wants to transmit data, it listens on the channel and waits for an opening. It then broadcasts a Request to Send (RTS) packet, which is very short. This broadcast is heard by all other stations in range on the channel. The access point broadcasts a Cleared to Send (CTS) packet on the channel with the name of the station granted permission, and a length of time for which this clearance is valid. All stations, even those out of range, or hidden, from the original station now know to stay idle for the specified time. The original station then transmits its data in the time allotted (or until its finished, it the data is short). The data is then acknowledged by the master, and all stations are free to send RTS packets as necessary.
Contention Management and Prioritization
CSMA/CA alone does not ensure equitable distribution of bandwidth. If one radio is closer, with a stronger signal, than its peers, its RTS will be more likely to be Cleared by the access point, allowing it to speak freely while other stations' Requests are summarily ignored. A mechanism in accordance with a preferred embodiment utilizes a radio protocol to allow stations to seize the airwaves. Each RTS interval is divided into slots. The number of slots varies depending on a user definable parameter (“MAC Level Optimization”) and the number of stations synchronized to the master.
FIG. 8 is a tabular display of the optimization level and synchronization in accordance with a preferred embodiment. Stations select a slot a random from the last half of available positions (i.e., if ‘MAC Level Optimization’ is set to Medium, stations randomly select from slots 3 and 4 ). If a station's Request is ignored twice, that station is then allowed to pick from the first half of available slots, thereby virtually assuring its Request will be Cleared. The exception to this rule is when an access point is configured as a station, as in a ‘bridging’ topology (see Section 1.2.5). Access points are considered higher priority traffic than normal stations, as they are likely to be servicing multiple clients themselves. They are thus permitted to initially choose a slot randomly from the last 75% of available positions (i.e., if ‘MAC Level Optimization’ is set to Medium, access point stations randomly select from slots 2 , 3 , and 4 ).
Filtering
A wireless LAN in accordance with a preferred embodiment has the ability to perform some rudimentary packet filtering. This is largely done for throughput preservation; in general there is no need to consume the limited bandwidth offered by WLAN solutions with such chatty traffic as IPX SAP broadcasts. A preferred embodiment filters this traffic at the access point before it is propagated over the wireless network.
Most of the filters are self-explanatory, based on protocol types. One filter offers the ability to filter traffic that neither originates from nor is destined for other wireless products, as determined by the first 8 hexadecimal digits of the MAC address: this feature is enabled by setting ‘Filter Fixed Nodes’ to on. Note that in most cases, this filter should be on to maximize throughput available to wireless clients. The one exception is when wireless products are used to link two disparate wired networks, as in bridging between buildings.
Access points use the IPX protocol to communicate roaming information. To enable users to roam between access points, you must disable the IPX filter. Access points use a proprietary protocol to exchange version information.
‘Bridging’
This is actually an unfortunate term, arising out of necessity. ‘Repeaters’ are referred to as ‘Extended Points’. The term ‘bridging’ arose historically; wireless point-to-point architectures have been used to link physically disparate networks in the same fashion that ‘bridges’, were previously employed to link logically disparate networks (which, by circumstance, were usually physically disparate as well). Most WLAN products are bridges, as they all translate from standard wired protocols (such as 802.3 Ethernet) into wired protocols (such as 802.11 or OpenAir2.4). A few perform no protocol translation and merely forward packets from one radio interface to the other. In most respects, access points configured as bridges act as normal stations. Some specialized aspects of the bridging architecture are detailed above, such as the configurable roam list, traffic prioritization scheme, and wired packet filter.
WLAN Security
One argument against implementation of wireless LANs may involve security. There is no doubt that the benefits of wireless LANs come at the cost of decreased network security. In particular, WLANs are extremely susceptible to denial of service attacks by highly committed individuals. However, proper precautions should preserve wireless data and network integrity.
Spread-spectrum techniques call for the transmission of data to occur across several distinct hops in the frequency band. In addition to reducing susceptibility to interference and thereby reducing inadvertent denial of service, this mechanism makes it non-trivial to ‘eavesdrop’ on a radio channel using ‘scanner’-type equipment and intercept data transmission. The architecture utilizes Frequency Hopping Spread Spectrum (FHSS) data transmission with 75 distinct hops in the 2.4-2.4835 Ghz ISM band. Note that committed individuals could still effect a DoS attack by ‘jamming’ the entire ISM band.
If commercially available products are used in WLAN implementations, it is relatively easy (though non-trivial) to intercept a spread-spectrum channel. A slightly less clumsy DoS attack could be launched by highly skilled individuals by synchronizing to the Frequency Hopping pattern and selectively ‘jamming’ the frequency in use. Mere acquisition of the radio signal is insufficient to intercept or modify data if this signal is encoded; measures would need to be taken to provide for efficient decoding of this signal. An architecture in accordance with a preferred embodiment utilizes a 20 byte key to encode data in real time using a proprietary algorithm. Note that this encoding is not ‘encryption’.
Steps should be taken to ensure that unauthorized user devices do not attempt to access the WLAN. The architecture utilizes an authorization scheme which denies access from units whose MAC address is not listed in the Authorization Table. Attempts to authorize the network from unauthorized nodes are logged. The above steps implement security measures at the lowest levels of the network architecture (i.e., those levels specific to WLAN implementations). The WLAN is still a part of the overall network implementation, and is subject to all relevant network-level regulations and provisions. For example, network traffic originating from or destined for WLAN hosts can be carefully monitored and regulated via network level restrictions, such as packet filtering at appropriate routers. Furthermore, specific measures can be taken at the application level to ensure data integrity. For example, session-level strong encryption (based on the RC5 algorithm) is available via some application software to prevent user authentication and session data transport from being passed ‘in the clear’. It should be noted that some of the features intended to prevent unauthorized use of the WLAN, such as port-based MAC address filtering have only recently being implemented in wired networks. FIG. 12 is a table of various communication protocols in accordance with a preferred embodiment.
FIGS. 13A to 13 F illustrate various architectures in accordance with a preferred embodiment. FIG. 14 illustrates a wireless communication architecture in accordance with a preferred embodiment. FIG. 15 illustrates a load balancing cluster in accordance with a preferred embodiment.
While various embodiments have been described above, it should be understood that they have been presented by way of example only, and not limitation. Thus, the breadth and scope of a preferred embodiment should not be limited by any of the above described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents. | An interactive electronic instructional system is a teaching interface between a teacher and students where data is transmitted from the teacher's terminal to the student terminals. The data is received at the student terminals and is separated into execution data and instructional data. The student terminals are grouped into teams allowing student teams to interact with a group decision. This encourages team participation by shy or otherwise reluctant students. Team answer data is transmitted from one of the student terminals in the team to the teacher's terminal. The teacher monitors team answer data to infer class progress towards a goal. The teacher may modify the instructional data based on the progress. | 7 |
This is a division of application Ser. No. 115,918, filed Nov. 2, 1987.
BACKGROUND OF THE INVENTION
1. Field of Invention
The present invention relates to a novel method of controlling epilepsy, muscle tension, muscular spasticity, and anxiety in living mammal bodies which utilizes certain 3-amino-5-methyl-1H-pyrazole-4-carboxylic acids and esters; and novel pharmaceutical compositions therefor are disclosed.
2. Information Disclosure Statement
3-Amino-5-substituted-1H-pyrazole-4-carboxylic acids identical or similar to those useful in the novel methods of the present invention have been disclosed as herbicides in German Offer. No. 2,747,531.
5-Amino-1,3-substituted-4-pyrazolecarboxanilides having anticonvulsant activity are disclosed in U.S. Pat. No. 4,346,097 and in U.S. Pat. No. 4,393,217 as having anxiolytic and antidepressant activity. In contrast compounds of the present invention are 4-carboxylates and 4-carboxylic acids.
3-Anilido-5-substituted-1H-pyrazole-4-carboxylic acid esters have been disclosed in Japan Kokai No. 74 95,968 to be an effective remedy against smallpox virus.
OBJECTIVES AND SUMMARY OF THE INVENTION
The present invention is concerned with a novel method of treating epilepsy, muscle tension, muscle spasticity, and anxiety in a living mammal which comprises administering to a mammal in need thereof a 3-amino-5-methyl-1H-pyrazole-4-carboxylic acid or an ester thereof having the following formula: ##STR2## wherein:
R 1 is hydrogen, loweralkyl or a pharmaceutically acceptable cation;
R 2 and R 3 , same or different, are hydrogen, loweralkyl, aryl, cycloalkyl, loweralkenyl, 1-adamantyl, heterocyclicaminoalkyl, diloweralkylaminoloweralkyl or R 2 with R 3 and adjacent nitrogen forming the heterocyclic ring structure 4-morpholino, 4-substituted-1-piperazinyl, 1-piperazinyl, 1-piperidinyl, 1-pyrrolidinyl, or 1-homopiperidinyl;
and the pharmaceutically acceptable salts thereof; and the tautomeric isomers thereof.
In further definition of the symbols in Formula I and where they appear elsewhere throughout this specification and claims, the terms have the following significance:
The term "loweralkyl" as used herein include straight and branched chain radicals up to eight carbons inclusive and is exemplified by such groups as methyl, ethyl, propyl, isopropyl, butyl, sec. butyl, tert. butyl, 1,1,3,3-tetramethylbutyl, amyl, isoamyl, hexyl, heptyl, and octyl radicals and the like. The term "loweralkoxy" as used herein has the formula-O-loweralkyl.
The term "aryl" as used herein includes pyridinyl in any of its positions, naphtalenyl in any of its positions, phenyl and phenyl-loweralkyl wherein phenyl may be substituted by one to three radicals, same or different, and are halogen, methylthio, loweralkyl, loweralkoxy, or trifluoromethyl.
The term "pharmaceutically acceptable cation" as used herein refers primarily to a pharmaceutically acceptable metal such as sodium, potassium, magnesium, zinc, copper, aluminum and the like.
The term "cycloalkyl" includes primarily cyclic and polycyclic alkyl radicals of three to ten carbon atoms and includes such groups as cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, 1-adamantyl and the like.
The term "loweralkenyl" as used herein refers to a loweralkyl radical containing a carbon-carbon double bond.
The term "heterocyclicaminoalkyl" as used herein refers primarily to a heterocyclic amino radical having 5-7 ring members and exemplified by such groups as 4-morpholinyl, 1-pyrrolidinyl, 1-piperidinyl, 4-substituted-1-piperazinyl, 1-piperazinyl, 1-homopiperidinyl and the like, connected via a 1-8 carbon alkyl chain, including branched chains, to a nitrogen of the heterocyclic amino ring.
The term "heterocyclic ring structure" as used herein includes primarily the heterocyclic amino radicals 1-azetidinyl, 1-pyrrolidinyl, 1-piperidinyl, 1-homopiperidinyl, 1-piperizinyl and the like.
The term "4-substituted-1-piperazinyl" as used herein refers to a piperazine radical substituted by usual groups common in the pharmaceutical art including "aryl" and "loweralkyl" as defined above.
The term "pharmaceutically acceptable salts" as used herein refers to those acid addition salts, quarternary salts, carboxylic acid salts, alcoholates and hydrates that are physiologically compatible in mammals. The acid addition salts may be formed by either strong or weak acids. Representative of useful strong acids are hydrochloric, hydrobromic, sulfuric, phosphoric and the like. Representative of useful weak acids are fumaric, maleic, succinic, oxalic, citric, tartaric, hexamic and the like. Suitable quarternary salts include loweralkyl halides and sulfates. Suitable carboxylic acid salts are formed by such as the alkali metals, alkaline earth metals, copper, aluminum and the like.
The term "tautomeric isomers" refers to the possible existence of the compounds of Formula I, in two forms, Ia and Ib as follows: ##STR3## and it is understood the compounds may exist in one or both tautomeric forms depending on such factors as the various substituents which make up the molecule, and when in solution, on the nature of the solvent. For purposes of simplicity, the numbering system used herein corresponds to that of Formula Ia.
The compounds of Formula I of this invention are useful because of their pharmacological action on the central nervous system. This method employs the compounds of Formula I to treat a living mammal (e.g., humans) for muscle tension and spasticity (i.e., to relax muscles), to control anxiety and to treat epilepsy (control convulsions).
The procedure used for testing compounds for their muscle relaxant activity is the Morphine-Induced-Straub-Tail-Test. The procedure used for testing compounds for their anticonvulsant activity is based on evaluation of protective activity against seizures induced by electrical or chemical challenge. The procedure used for testing compounds for antianxiety activity is the Vogel Conflict Test, which is based on the shock-suppressed drinking behavior of rats. All of these evaluation techniques are described in greater detail under Pharmacological Test Procedures, hereinbelow.
It is therefore an object of the present invention to provide certain 3-amino-5-methyl-1H-pyrazole-4-carboxylic acids and acid esters thereof, as described hereinabove and as defined under Formula I which have CNS activity in a novel method of treatment for epilepsy, muscle tension, spastic muscles, and anxiety.
Additional objects and advantages of the present invention will be apparent to one skilled in the art and others will become apparent from the following description of the best mode of carrying out the invention, and from the appended claims.
DETAILED DESCRIPTION OF THE INVENTION
The novel methods of treating epilepsy, anxiety, muscle tension, and muscle spasticity in living animals comprises administering a 3-amino-5-methyl-1H-pyrazole-4-carboxylic acid or carboxylic acid ester and derivatives thereof as set forth hereinabove under Formula I and in definitions therewith, and as pharmaceutical compositions to a living animal body for anticonvulsant, muscle relaxant, or antianxiety effect in an effective amount.
The compounds of Formula I are prepared by one of three methods as outlined hereinbelow under methods A, B, and C. ##STR4## wherein:
R 1 and R 3 are as defined hereinabove under Formula I.
Generally in Method A, a primary amine of Formula V is reacted first with carbon disulfide and triethylamine in solvent, e.g., methylene chloride and treated with ethyl chloroformate and triethylamine in appropriate solvents in a procedure similar to that used by Garmaise et al., J. Amer. Chem. Soc. 80:3332 (1958), giving an isothiocyanate product of Formula IV. This product is reacted with hydrazine hydrate as in the method of Pohloudek, Fabini and Gockeritz, Pharmazie, 17, No. 9,515 (1962) to give a thiosemicarbazide of Formula III, which is reacted with a compound of Formula II as in the method of Bulka et al., Chem. Ber. 98,259 (1965) to give a compound of Formula Ic. Pharmaceutically acceptable acid addition salts may be prepared by reacting the free base with the appropriate acid. ##STR5## wherein:
R 1 , R 2 , and R 3 are as defined hereinabove under Formula I, except that when a Formula IX compound is reacted with thiophosgene R 2 and R 3 are not hydrogen, and R 2 and R 3 and adjacent nitrogen do not form the heterocyclic ring structure 1-piperazinyl in this method, but may form the heterocyclic ring structure 4-substituted-1-piperazinyl.
Generally in Method B, an amine of Formula IX is reacted in sequence with carbon disulfide, chloracetic acid, and hydrazine hydrate, as in the method of Jensen, K.A. J. Prakt. Chem. 159,189 (194) to give a thiosemicarbazide of Formula VII. Optionally, a secondary amine of Formula IX may be reacted with thiophosgene to give a compound of Formula VIII, followed by reaction with hydrazine hydrate to give the desired thiosemicarbazide of Formula VII as in the method of Jensen, et al., Acta. Chem. Scand. 22,37 (1968). In any event, reaction of the obtained thiosemicarbazide with a compound of Formula VI, by the method of Bulka, et al., Chem. Ber. 98,259 (1965) gives a compound of Formula Id. Pharmaceutically acceptable salts may be prepared by reacting the free base with the appropriate acid. ##STR6## wherein:
R 1 , R 2 , and R 3 are as defined hereinabove under Formula I, except R 1 is not hydrogen in this method.
Generally in Method C, a carboxylic acid ester of Formula I is hydrolyzed by use of a phase transfer catalyst such as tetrabutylammonium bromide in a suitable solvent such as ethyl alcohol. The reaction mixture is stirred at ambient temperature for about 24 hr, diluted with water, and extracted with an appropriate organic solvent such as isopropyl ether. Acidification of the extracted organic layer to about approximately pH 6 precipitates the desired compound of Formula Ie, which may then be purified and/or dried by the usual means known in the art. The method is illustrated more fully in Example 45. Pharmaceutically acceptable acid addition salts may be prepared by reacting with the appropriate acid.
Many of the starting compounds used in the novel methods of the present invention, i.e., starting amine compounds, compounds of Formula V and Formula IX are available commercially through Aldrich Chemical Co., Inc., 940 West Saint Paul Avenue, Milwaukee, Wi 53233. Other starting compounds useful in the methods of the present invention are readily prepared by known methods of chemical synthesis used in the art, or are obvious variations thereof. The following preparations and examples serve to illustrate methods of preparing the compounds useful in the novel methods of the present invention. The scope of the invention is not limited by the Preparations and Examples, however. Structures of the compounds of the Examples are given for reference in Table I.
Preparation 1
Utilizing Method A and the procedure of Garmaise, et al., J. Amer. Chem. Soc., 80,3332 (1958), and the procedure of Pohloudek-Fabrini and Gockeritz, Pharmazie, 17, No. 9,515 (1962) and reacting the following:
(a) aniline,
(b) 4-chloroaniline,
(c) 3-(methylmercapto)aniline,
(d) 1-aminonaphthalene,
(e) 2-(methylmercapto)aniline,
(f) 2,6-dimethylaniline,
(g) 2-methyoxyaniline,
(h) o-toluidine,
(i) 2,6-dichloroaniline,
(j) 2-chloroaniline
(k) 2,4-dimethoxyaniline,
(l) 3-chloroaniline,
(m) 2-aminopyridine,
(n) butylamine,
(o) 2,6-diethylaniline,
(p) 2,4-dimethylaniline,
(q) 4-chloro-2-methylaniline,
(r) 2,4-dichloroaniline,
(s) 2-chloro-6-methylaniline,
(t) 4-bromo-2,6-dimethylaniline,
(u) methylamine,
(v) allylamine,
(w) ethylamine,
(x) cyclohexylamine,
(y) benzylamine, and
(z) 1-adamantanamine
in sequence with
(1) carbon disulfide and triethylamine, solvent (e.g. methylene chloride)
(2) ethyl chloroformate/methylene chloride, and
(3) triethylamine/methylene chloride followed by hydrazine hydrate,
there are obtained:
(a) 4-phenyl-3-thiosemicarbazide,
(b) 4-(4-chlorophenyl)-3-thiosemicarbazide,
(c) 4-[3-(methythio)phenyl]-3-thiosemicarbazide,
(d) 4-(1-naphthalenyl)-3-thiosemicarbazide,
(e) 4-[2-(methylthio)phenyl]-3-thiosemicarbazide,
(f) 4-(2,6-dimethylphenyl)-3-thiosemicarbazide,
(g) 4-(2-methoxyphenyl)-3-thiosemicarbazide,
(h) 4-(2-methylphenyl)-3-thiosemicarbazide,
(i) 4-(2,6-dichlorophenyl)-3-thiosemicarbazide,
(j) 4-(2-chlorophenyl)-3-thiosemicarbazide,
(k) 4-(2,4-dimethoxyphenyl)-3-thiosemicarbazide,
(l) 4-(3-chlorophenyl)-3-thiosemicarbazide,
(m) 4-(2-pyridyl)-3-thiosemicarbazide,
(n) 4-butyl-3-thiosemicarbazide,
(o) 4-(2,6-diethylphenyl)-3-thiosemicarbazide,
(p) 4-(2,4-dimethylphenyl)-3-thiosemicarbazide,
(q) 4-(4-chloro-2-methylphenyl)-3-thiosemicarbazide,
(r) 4-(2,4-dichlorophenyl)-3-thiosemicarbazide,
(s) 4-(2-chloro-6-methylphenyl)-3-thiosemicarbazide,
(t) 4-(4-bromo-2,6-dimethylphenyl)-3-thiosemicarbazide,
(u) 4-methyl-3-thiosemicarbazide,
(v) 4-(2-propenyl)-3-thiosemicarbazide,
(w) 4-ethyl-3-thiosemicarbazide,
(x) 4-cyclohexyl-3-thiosemicarbazide,
(y) 4-phenylmethyl-3-thiosemicarbazide, and
(z) 5-(1-adamantyl)-3-thiosemicarbazide.
Preparation 2
Utilizing Method A and the procedure of Garmaise, et al., J. Amer. Chem. Soc., 80,3332 (1958) and the procedure of Pohloudek-Fabrini and Gockeritz, Pharmazie, 17, No. 9,515 (1962) and reacting the following:
(a) phenethylamine,
(b) heptylamine,
(c) tert-butylamine,
(d) cycloheptylamine,
(e) cyclopentylamine,
(f) cyclopropylamine,
(g) propylamine,
(h) sec-butylamine,
(i) amylamine,
(j) hexylamine,
(k) cyclooctylamine,
(l) 2-methylbutylamine,
(m) tert-octylamine,
(n) 3-dimethylaminopropylamine,
(o) 1-(2-aminoethyl)piperidine,
(p) isopropylamine,
(q) 4-(2-aminoethyl)morpholine,
(r) 4-(3-aminopropyl)morpholine, and
(s) 4-aminobenzotrifuluoride
in sequence with
(1) carbon disulfide and triethylamine, solvent (e.g., methylene chloride)
(2) ethyl chloroformate/methylene chloride, and
(3) triethylamine/methylene chloride followed by hydrazine hydrate,
there are obtained:
(a) 4-phenylethyl-3-thiosemicarbazide,
(b) 4-heptyl-3-thiosemicarbazide,
(c) 4-(1,1-dimethylethyl)-3-thiosemicarbazide,
(d) 4-cycloheptyl-3-thiosemicarbazide,
(e) 4-cyclopentyl-3-thiosemicarbazide,
(f) 4-cyclopropyl-3-thiosemicarbazide,
(g) 4-propyl-3-thiosemicarbazide,
(h) 4-(2-butyl)-3-thiosemicarbazide,
(i) 4-pentyl-3-thiosemicarbazide,
(j) 4-hexyl-3-thiosemicarbazide,
(k) 4-cyclooctyl-3-thiosemicarbazide,
(l) 4-(2-methylbutyl)-3-thiosemicarbazide,
(m) 4-(1,1,3,3-tetramethylbutyl)-3-thiosemicarbazide,
(n) 4-(3-dimethylaminopropyl)-3-thiosemicarbazide,
(o) 4-(2-(1-piperidinyl)ethyl)-3-thiosemicarbazide,
(p) 4-(1-methylethyl)-3-thiosemicarbazide,
(q) 4-[2-(4-morpholinyl)ethyl]-3-thiosemicarbazide,
(r) 4-[3-(4-morpholinyl)propyl]-3-thiosemicarbazide, and
(s) 4-[4-(trifluoromethyl)phenyl]-3-thiosemicarbazide.
Preparation 3
Utilizing Method B and the procedure of Jensen, et al., Acta Chem. Scand., 22,37 (1968) and reacting the following:
(a) dimethylamine,
(b) di-n-butylamine,
(c) morpholine,
(d) N-methylcyclohexylamine,
(e) N-methylcyclopentylamine,
(f) 1-phenylpiperazine,
(g) 1-benzylpiperazine,
(h) pyrrolidine,
(i) piperidine, and
(j) homopiperidine
with thiophosgene followed by hydrazine hydrate, there are obtained:
(a) 4,4-dimethyl-3-thiosemicarbazide,
(b) 4,4-dibutyl-3-thiosemicarbazide,
(c) 4-morpholinecarbothioic acid hydrazide,
(d) 4-cyclopentyl-4-methyl-3-thiosemicarbazide,
(e) 4-cyclopentyl-4-methyl-3-thiosemicarbazide,
(f) (4-phenyl-1-piperazine)carbothioic acid hydrazide,
(g) (4-phenylmethyl-1-piperazine)carbothioic acid hydrazide,
(h) 1-pyrrolidinecarbothioic acid hydrazide,
(i) 1-piperidinecarbothioic acid hydrazide, and
(j) 1-homopiperidinecarbothioic acid hydrazide.
EXAMPLE 1
5-Methyl-3-phenylamino-1H-pyrazole-4-carboxylic acid, ethyl ester.
A suspension of 16.7 g (0.1 mole) of 4-phenyl3-thiosemicarbazide in 60 mL of absolute ethanol was treated with 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate and the mixture stirred for 1 hr at room temperature. As the thiosemicarbazide began to dissolve the reaction mixture became exothermic and a reddish-brown solid precipitated. Alcoholic hydrogen chloride (2N, 50 mL) was added, and the reaction mixture heated at reflux for 1.0 hr. The solution was filtered while hot and the filtrate was evaporated under reduced pressure. The solid residue was triturated in cold absolute ethanol and a red solid collected by filtration. The solid was warmed in 2N hydrochloric acid (100 mL) and the suspended sulfur removed by filtration. An orange-red solid precipitated from the filtrate, was collected by filtration and air dried for ˜16 hr (14.6 g, mp 160°-4° C.). Recrystallization from benzene left 10.5 g of product, mp 165°-6° C. The material was air dried and submitted for elemental analysis.
Analysis: Calculated for C 13 H 15 N 3 O 2 : C, 63.66; H, 6.16; N, 17.13. Found: C, 63.63; H, 6.22; N, 17.13.
EXAMPLE 2
3-[(4-Chlorophenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A suspension of 20.1 g (0.10 mole) of 4-(4-chlorophenyl)3-thiosemicarbazide in 80 mL of absolute ethanol was treated with 16.5 g (0.10 mole) of ethyl 2-chloroacetoacetate and the mixture stirred for 1.0 hr at room temperature. Alcoholic hydrogen chloride (2N, 60 mL) was added and the dark precipitate dissolved while heating the mixture at reflux for 1.0 hr. The solution was filtered while hot, and the filter cake washed with absolute ethanol. The filtrate was evaporated under reduced pressure and the residue triturated in cold absolute ethanol and filtered. Both filter cakes were found to be the same compound by TLC (10% methanol in benzene on silica gel). The two were combined, dissolved in hot absolute ethanol (the hydrochloride salt was water insoluble), partially neutralized with saturated aqueous sodium bicarbonate, and the solid filtered (10.4 g, mp 212°-226° C.). A second crop was obtained by treating the filtrate with saturated aqueous sodium bicarbonate (11.5 g, mp 220°-225° C.). The second crop was recrystallized from absolute ethanol to give 3.8 g of product, mp 223°-225° C. This solid was dried at 100° C./0.1 mmHg/3 hr; then for ˜16 hr at RT/0.1 mmHg.
Analysis: Calculated for C 13 H 14 ClN 3 O 2 : C, 55.82; H, 5.05; N, 15.02. Found: C, 55.85; H, 5.08; N, 15.10.
EXAMPLE 3
5-Methyl-3-[[3-(methylthio)phenyl]amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A suspension of 10.0 g (0.046 mole) of 4-(3-methythiophenyl)-3-thiosemicarbazide and 7.72 g (0.0469 mole) of ethyl 2-chloroacetoacetate in 150 mL of absolute ethanol was stirred at room temperature for ˜16 hr. Ethanolic hydrogen chloride (2N, 50 mL) was added, the mixture refluxed for 1.0 hr, the solution filter while hot, and the filtrate evaporated under reduced pressure to give a crystalline residue which was recrystallized three times from absolute ethanol to give 6.3 g produce, mp 191.5°-194° C. The sample was dried at 56° C./4 hr/0.1 mmHg then 2 hr/25° C./0.1 mmHg.
Analysis: Calculated for C 14 H 17 N 3 O 2 S: C, 57.71; H, 5.88; N, 14.42. Found: C, 57.97; H, 5.94; N, 14.58.
EXAMPLE 4
5-Methyl-3-(1-naphthalenylamino)-1H-pyrazole-4-carboxylic acid, ethyl ester.
A suspension of 15.0 g (0.069 mole) of 4-(1-naphthalenyl)-3-thiosemicarbazide and 11.4 g (0.069 mole) of ethyl 2-chloroacetoacetate in 100 mL of absolute ethanol was stirred at room temperature for 1 hr. Alcoholic hydrogen chloride (2N, 50 mL) was added, the mixture refluxed for 1 hr, filtered while hot and the filtrate evaporated under reduced pressure. The residue was recrystallized twice from 190 ethanol then twice from absolute ethanol to give 6.2 g of product, mp 199°-202° C. The sample was dried at 56° C./4 hr/0.1 mmHg then at 25° C./0.1 mmHg/for ˜16 hr.
Analysis: Calculated for C 17 H 17 N 3 O 2 : C, 69.14; H, 5.80; N, 14.23. Found: C, 69.05; H, 5.86; N, 14.23.
EXAMPLE 5
5-Methyl-3-[[2-(methylthio)phenyl]amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A mixture of 15 g (0.07 mole) of 4-[2-(methylthio)phenyl]-3-thisemicarbazide and 11.96 g (0.07 mole) of ethyl 2-chloroacetoacetate (97%) in 100 mL of absolute ethanol was stirred under nitrogen atmosphere for 1 hr at room temperature. The reaction was slightly exothermic and the mixture took on a yellow color as most of the solid dissolved. The mixture was treated with 50 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1.5 hr. The mixture had darkened to a deep, clear, orange color, with only a trace of insoluble material which was removed by filtering through a sintered glass filter. The solvent was removed in vacuo giving a yellow-orange solid (18.6 g). The solid was recrystallized from acetone, 17.4 g (85% yield), mp 135°-158° C. Thin layer chromatography indicated two impurities (10% methanol/benzene on silica gel). This crude product was recrystallized from benzeneligroin to give 12.1 g (59% yield), mp 126° -128° C. (some solid remained and melted at 158°-160° C.). Thin layer chromatography indicated that one of the two impurities had been removed. The solid was dissolved in methylene chloride and chromatographed on a 250 g column of Florisil® (60-100 mesh). The column was eluted with methylene chloride. The solid obtained was recrystallized from benzene-ligroin giving 4.6 g (22.5%) of product, mp 140.5°-142° C.
Analysis: Calculated for C 14 H 17 N 3 O 2 S: C, 57.71; H, 5.88; N, 14.42. Found: C, 57.87; H, 5.89; N, 14.35.
EXAMPLE 6
5-Methyl-3-[(2,6-dimethylphenyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A mixture of 9.8 g (0.05 mole) of 4-(2,6-dimethylphenyl)-3-thiosemicarbazide and 8.48 g (0.05 mole) of ethyl 2-chloroacetoacetate (97%) in 75 mL of absolute ethanol was stirred under nitrogen atmosphere for one hour at room temperature. The reaction was slightly exothermic and the mixture changed from a white slurry to a yellow slurry as most of the solid dissolved. The mixture was treated with 40 mL of 2N ethanolic hydrogen chloride and allowed to stir at room temperature for 16 hr. The reaction mixture was heated at reflux for two hours; during this time it took on a dark orange color which cleared later as all the material dissolved (a small amount of insoluble material was also present). The reaction mixture was filtered and the solvent removed under reduced pressure leaving a yellow-orange solid. The solid was triturated with acetone which dissolved most the orange color. Filtration gave 12.6 g of pale yellow crystals, mp 131°-137° C. Recrystallization of the yellow solid from acetone gave two crops of soft, fluffy, white product. Both crops were combined and analyzed, yield 8.5 g (62%), mp 142°-144° C.
Analysis: Calculated for C 15 H 19 N 3 O 2 : C, 65.91; H, 7.01; N, 15.37. Found: C, 65.82; H, 6.93; N, 15.37.
EXAMPLE 7
5-Methyl-3-[(2-methoxyphenyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A suspension of 10.0 g (0.0507 mole) of 4-(2-methoxyphenyl)-3-thiosemicarbazide and 8.35 g (0.0507 mole) of ethyl 2-chloroacetoacetate in 150 mL of absolute ethanol was stirred for ˜16 hr at room temperature. Alcoholic hydrogen chloride (2N, 50 mL) was added, the mixture heated at reflux for 1.0 hr, and the solution filtered while hot to remove the precipitated sulfur. The filtrate was evaporated under reduced pressure, and the residue dissolved in hot ethanol, treated with charcoal and filtered through Celite®. The solution deposited 10.0 g of product, mp 162°-172° C. A similar recrystallization from absolute ethanol left 8.1 g, mp 155°-175° C. This product was dissolved in absolute ethanol, treated with charcoal, and filtered through Celite® 3 times. The filtrate deposited 4.3 g of product while standing for ˜16 hr, mp 155.5°-159° C. which was a mixture of free base and hydrochloride salt. This last filtrate was left open to the atmosphere, and after approximately 50% of the solvent had evaporated, a solid precipitated and was collected by filtration: 1.4 g, mp 184°-191° C.
Analysis: Calculated for C 14 H 17 N 3 O 3 : C, 61.08; H, 6.22; N, 15.26 Found: C, 60.98; H, 6.19; N, 15.16
EXAMPLE 8
5-Methyl-3-[(2-methylphenyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 4-(2-methylphenyl)-3-thiosemicarbazide, 15.3 g (0.08 mole), in 100 mL of absolute ethanol was treated under nitrogen atmosphere with ethyl 2-chloroacetoacetate, 13.61 g (0.08 mole). After stirring for 1 hr the slurry had turned from white to yellow with most of the material going into solution. The reaction mixture was treated with 50 mL of 2N ethanolic hydrogen chloride and stirred for 18 hr., after which the reaction mixture was heated at reflux for 2 hours. A clear orange solution was decanted from some residual material. The hot solution was filtered through a sintered glass filter and the filtrate concentrated in vacuo to give a yellow solid residue. This residue was dissolved in 500 mL of acetone and 50 mL methanol. After filtering, the volume of the filtrate was concentrated to 125 mL under nitrogen atmosphere. The product was allowed to crystallize at ˜7-10° C. for ˜72 hr. Some sulfur crystals separated and were removed by filtration. The filtrate was again concentrated in vacuo to a solid. The solid was dissolved in hot acetone and upon cooling at ˜7-10° C., long needle-like crystals formed and redissolved on warming to room temperature. The solution was treated with water and overnight gave pale, yellow needle-like crystals which, after drying, weighed 15 g, mp 156°-160° C. After 3 recrystallizations from benzene/ligroin a fine white crystalline solid was obtained (8.6 g, mp 160°-161° C.).
Analysis: Calculated for C 14 H 17 N 3 O 2 : C, 64.85; H, 6.61; N, 16.21. Found: C, 64.88; H, 6.59; N, 16.33.
EXAMPLE 9
3-[(2,6-Dichlorophenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A slurry of 9.4 g (0.04 mole) of 4-(2,6-dichlorophenyl)-3-thiosemicarbazide in 75 mL of absolute ethanol was stirred under nitrogen atmosphere while 6.8 g (0.04 mole) of ethyl 2-choroacetoacetate was added. The reaction mixture became yellow as it stirred for 1 hr at room temperature. Then 40 mL of 2N ethanolic hydrogen chloride was added and the reaction mixture heated at reflux for 3 hr. Insoluble sulfur was removed by filtration and the filtrate concentrated in vacuo to give an orange solid, which when triturated with hot acetone yielded 11.3 g of pale yellow crystals, mp: plastic 175°-191° C., degasses at 195° C., and forms a clear melt at 215° C. Recrystallization from acetonitrile gave 6.5 g of product, mp 180°-190° C. Additional material was obtained from the reaction mixture filtrate upon setting. The filtrate was then concentrated to a solid. All crude materials were combined and dissolved in 125 mL of benzene, treated with charcoal, filtered, and the volume reduced to 40 mL. The benzene solution was treated with 25 mL of ligroin and the product crystallized from the hot solution to give 9.7 g of crystalline product which had a pink color, mp 191°-192° C.
Analysis: Calculated for C 13 H 13 N 3 O 2 Cl 2 : C, 49.70; H, 4.17; N, 13.38. Found: C, 49.50; H, 4.21; N, 13.26.
EXAMPLE 10
3[(2-Chlorophenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A solution of 10.05 g (0.05 mole) of 4-(2-chlorophenyl)-3-thiosemicarbazide in 75 mL of absolute ethanol was treated with 8.48 g (0.05 mole) of ethyl 2-choroacetoacetate and stirred under nitrogen atmosphere at room temperature for 1 hr. The reaction mixture was treated with 40 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1 hr, during which time the yellow slurry became a clear, deep orange solution. The characteristic insoluble amorphous sulfur was removed by filtration. The filtrate began to solidify. It was allowed to cool for approximately 16 hr to yield 10.1 g of yellow crystalline product. The filtrate was concentrated in vacuo to yield an additional 3 g of yellow product. The 2 solids were combined and recrystallized from benzene to give 10.4 g of white crystalline product, mp 188°-189° C.
Analysis: Calculated for C 13 H 14 N 3 O 2 Cl: C, 55.82; H, 5.05; N, 15.02. Found: C, 55.45; H, 5.01; N, 14.98.
EXAMPLE 11
3-[(2,4-Dimethoxyphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 18.2 g (0.08 mole) of 4-(2,4-dimethoxyphenyl)-3-thiosemicarbazide in 120 mL of absolute ethanol was treated with 13.6 g (0.08 mole) of ethyl 2-chloroacetoacetate, and the slightly exothermic reaction was allowed to stir at room temperature for 2 hr. Most of the solid material dissolved and the solution became yellow. The reaction mixture was treated with 40 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1 hr. At this time point, previous reaction mixtures had become clear solutions. The reaction mixture was diluted with an additional 200 mL of absolute ethanol and heated to reflux. The reactants dissolved and the reaction mixture became orange, and amorphous sulfur separated. The reaction mixture was filtered hot. Some products precipitated in the filter while filtering and were washed out with 100 mL of hot absolute ethanol. The combined reaction mixture volume, now 600 mL, was reduced under a stream of nitrogen, and on cooling overnight yielded 23 g of crystalline product with a yellow color. Recrystallization from ethanol gave 18 g of yellow crystalline product but TLC showed the presence of sulfur. The compound was dissolved in 50 mL of methanol and 100 mL of benzene was added. The volume was reduced to 75 mL, and 50 mL of ligroin was added. After 5 days, filtration yielded 11.4 g of white powder with a pink color, mp 199°-200° C. Elemental analysis indicated that it was the hydrochloride salt.
Analysis: Calculated for C 15 H 20 N 3 O 4 Cl: C, 52.71; H, 5.90; N, 12.29. Found: C, 52.69; H, 5.86; N, 12.39.
EXAMPLE 12
3-[(3-Chlorophenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 8 g (0.04 mole) of 4-(3-chlorophenyl)-3-thiosemicarbazide in 75 mL of absolute ethanol was treated with 6.8 g (0.04 mole) of ethyl 2-choroacetoacetate. The reactants quickly dissolved but a precipitate soon formed. After stirring at room temperature for 2 hr the reaction mixture was treated with 40 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1 hr, then filtered while hot to remove the insoluble sulfur. The filtrate on cooling yielded 3.5 g of yellow solid and an additional 4.7 g was obtained when the filtrate was concentrated in vacuo. Recrystallization from benzene/ligroin gave 4.2 g of pale yellow brown product. Additional ligroin added to the filtrate gave, upon cooling at ˜7-10° C. for ˜16 hr, additional crystals but also some oil; this tri-phase mixture was filtered to yield 1.5 g of additional product. Both solids had identical mass spectra. They were combined and recrystallized twice from benzene/ligroin and finally from benzene by dissolving the solids and reducing the volume until crystallization began. Upon cooling, 3.93 g of beige plate-like crystals were collected, mp 159.5°-160° C.
Analysis: Calculated for C 13 H 14 N 3 O 2 Cl: C, 55.82; H, 5.05; N, 15.02. Found: C, 55.86; H, 5.07; N, 15.20.
EXAMPLE 13
5-Methyl-3-[(2-pyridinyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 4.4 g (0.03 mole) of 4-(2-pyridyl)-3-thiosemicarbazide in 50 mL of absolute ethanol was treated with 5.3 g (0.03 mole) of ethyl 2-chloroacetoacetate and after 2 hr at room temperature the solution had become yellow. The reaction mixture was then treated with 25 mL of 2N ethanolic hydrogen chloride and stirred over the weekend at room temperature. The reaction mixture was heated at reflux for 2 hr, filtered hot and the filtrate concentrated in vacuo to give a yellow-orange oil (8.1 g) which failed to crystallize. After 2 weeks no crystalline product was evident. The oil was dissolved in ethanol/water, made basic with sodium bicarbonate solution, and extracted with 3×100 mL of methylene chloride. The extracts were combined, washed with 20 mL of water, dried over magnesium sulfate, and concentrated in vacuo to a yellow oil which solidified on standing overnight. Recrystallization 3 times from benzene/ligroin, each time reducing the volume, gave 1.45 g of cream-colored powder, mp 155°-156° C. Elemental analysis gave a high carbon analysis and NMR showed the presence of benzene. The sample was dried at 100° C. in vacuo for 2 hr and resubmitted for elemental analysis.
Analysis: Calculated for C 12 H 14 N 4 O 2 : C, 58.53; H, 5.73; N, 22.75. Found: C, 58.58; H, 5.73; N, 22.78.
EXAMPLE 14
3-Butylamino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred solution of 14.7 g (0.1 mole) of 4-butyl-3-thiosemicarbazide in 150 mL of absolute ethanol was treated with 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate. The reaction mixture while stirring at ambient temperature became progressively cloudy within 1 hr, then unexpectedly became clear. The reaction mixture was treated with 60 mL of 2N ethanolic hydrogen chloride and stirred at ambient temperature over the weekend. The reaction mixture was now cloudy, but cleared as the reaction mixture was heated to reflux. After 1 hr, the hot reaction mixture was filtered and concentrated in vacuo to give a yellow oil. Trituration of this oil with benzene/ligroin (50:50) gave 10.7 g of off-white solid. Recrystallization from benzene/ligroin gave 10.5 g of white power, mp 138°-139° C. TLC (10% methanol/benzene; silica gel) showed 4 major spots and nmr analysis showed the presence of excess butyl radical. The reaction mixture product was then recrystallized from methanol/water (6.1 g). The filtrate was made basic with 3N sodium hydroxide solution and an addition 8 g (wet) of material was obtained. The 2 fractions were combined and recrystallized from benzene to give 11.2 g of fine white crystals which were dried at 82° C. under high vacuum, mp 109°-110° C.
NOTE: It was found that the hydrochloride salt of this compound is formed in nonaqueous solvents but dissociates in aqueous solution.
Analysis: Calculated for C 11 H 19 N 3 O 2 : C, 58.65; H, 8.50; N, 18.65. Found: C, 58.14; H, 8.54; N, 18.79.
EXAMPLE 15
3-Butylamino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, sulfate[1:1].
A solution of 3-butylamino-5-methyl-1-H-pyrazole-4-carboxylic acid ethyl ester (2 g in 20 mL of isopropyl ether) was treated dropwise with 1N sulfuric acid in 2-propanol. A turbid solution formed and an oil slowly separated and solidified. Recrystallization from isopropyl alcohol/isopropyl ether gave 2 g of fine white crystals, mp 81°-83° C. The sulfate salt, like the hydrochloride, dissociates in aqueous solution.
Analysis: Calculated for C 11 H 21 SN 3 O 6 : C, 40.86; H, 6.55; N, 12.99. Found: C, 40.62; H, 6.56; N, 12.91.
EXAMPLE 16
3-[(2,6-Diethylphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 9.4 g (0.05 mole) of 4-(2,6-diethylphenyl)-3-thiosemicarbazide in 75 mL of absolute ethanol was treated with 8.25 g (0.05 mole) of ethyl 2-chloroacetoacetate. The reaction mixture was stirred at ambient temperature as the color changed from white to yellow then to a greenishwhite. The reaction mixture was treated with 40 mL of 2N ethanolic hydrogen chloride, heated at reflux for 1 hr then filtered hot. The filtrate upon cooling yielded a pale yellow solid, 16 g. Recrystallization from benzene/ligroin gave 15.5 g of white granular solid which was dried at 82° C. under high vacuum for 3 hr, mp 167°-170° C. Elemental analysis and its 1H NMR spectrum indicated the product was a hydrochloride salt.
Analysis: Calculated for C 17 H 24 N 3 O 2 Cl: C, 60.44; H, 7.16; N, 12.44. Found: C, 60.59; H, 7.16; N, 12.60.
EXAMPLE 17
3-[(2,4-Dimethylphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 10.8 g (0.06 mole) of 4-(2,4-dimethylphenyl)-3-thiosemicabazide in 90 mL of absolute ethanol was treated with 9 g (0.066 mole) of ethyl 2-chloroacetoacetate. The mixture was stirred at ambient temperature for 1 hr under nitrogen atmosphere, then treated with 45 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1 hr. The reaction mixture was filtered to remove amorphous sulfur and the filtrate concentrated in vacuo to give a yellow solid. Trituration with benzene gave 13.6 g of crude product which was recrystallized from benzene/methanol (90:10) by reducing the volume in half while heating under a nitrogen atmosphere, to give 4.6 g of solid, mp 148°-171° C. Addition of ligroin to the filtrate gave, after 3 days, an additional 6.3 g of solid, mp 127°-129° C. Mass spectra of both samples were identical except that one showed hydrogen chloride present. Both compounds were dissolved in methanol/water and made basic with 3N sodium hydroxide. The solution became milky then a solid separated, 17 g (wet). After air drying for 3 days its final weight was 10.8 g. Recrystallization from benzene/ligroin have 9.3 g of fine white crystals, mp 174.5°-176° C.
Analysis: Calculated for C 15 H 19 N 3 O 2 : C, 65.91; H, 7.01; N, 15.37. Found: C, 65.35; H, 6.99; N, 15.55
EXAMPLE 18
3-[(4-Chloro-2-methylphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 11.4 g (0.053 mole) of 4-(4-chloro-2-methylphenyl)-3-thiosemicarbazide in 80 mL of absolute ethanol was treated with 9.6 g (0.0583 mole) of ethyl 2-chloroacetoacetate then stirred for 1 hr at ambient temperature. The reaction mixture was treated with 40 mL of 2N ethanolic hydrogen chloride, heated to reflux, then allowed to stir ˜16 hr at ambient temperature. The reaction mixture was again heated to reflux to dissolve most of the material and filtered hot to remove the amorphous sulfur. The filtrate was concentrated in vacuo. The yellow solid obtained was recrystallized from methanol/benzene to give 9.5 g of crystalline product, mp 146°-177° C. Addition of ligroin to the filtrate gave after 6 hr an additional 3.8 g, mp 170°-183° C. Both fractions were combined in acetone/water and made basic with 3N sodium hydroxide. The milky mixture was heated until a clear solution was obtained and upon cooling, the product crystallized, 34 g (wet). The product was air dried and recrystallized from benzene to give 9 g of fine white crystals, mp 156°-187° C.
Analysis: Calculated for C 14 H 16 N 3 O 2 Cl: C, 57.24; H, 5.50; N, 14.30. Found: C, 57.23; H, 5.49; N, 14.36.
EXAMPLE 19
3-[2,4-Dichlorophenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A slurry of 9.5 g (0.04 mole) of 4-(2,4-dichlorophenyl)-3-thiosemicarbazide in 60 mL of absolute ethanol was treated with 6.7 g (0.04 mole) of ethyl 2-chloroacetoacetate then stirred for 1.5 hr at ambient temperature. The reaction mixture was treated with 30 mL of 2N ethanolic hydrogen chloride, heated at reflux for 2 hr and allowed to cool ˜16 hr. The reaction mixture was heated to reflux to dissolve most of the material and filtered to remove the amorphous sulfur. Upon cooling the filtrate yielded 3.7 g of tan product. The residue was concentrated in vacuo to give 4.2 g of crude yellow solid. All the reaction mixture materials were dissolved in methanol, treated with 3N sodium hydroxide, then diluted with water until a curd-like material separated. This crude yellow-tan solid, 28 g (wet) was allowed to air dry then recrystallized from 2-propyl alcohol to give two batches of solid, 4.3 g of fine white needles, mp 215°- 217° C. and 2.2 g of fine pale beige needles, mp 214°-215° C. Comparison TLC of both compounds (10% methanol/benzene; silica gel) showed them to be identical. They were combined for analysis.
Analysis: Calculated for C 13 H 13 N 3 O 2 Cl 2 : C, 49.70; H, 4.17; N, 13.38. Found: C, 49.72; H, 4.17; N, 13.49.
EXAMPLE 20
3-[(2-Chloro-6-methylphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A slurry of 21.5 g (0.1 mole) of 4-(2-chloro-6-methylphenyl)-3-thiosemicarbazide in 100 mL of absolute ethanol was treated with 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate and stirred ambient temperature for 1 hr. The yellow mixture was treated with 50 mL of 2N ethanolic hydrogen chloride and heated at reflux until the reaction mixture was a clear red-brown color (2.5 hr). The reaction mixture was filtered and the filtrate concentrated in vacuo to give 43 of crude yellow solid. The crude solid was dissolved in acetone, made basic with 40 mL of 3N sodium hydroxide, filtered to remove some insoluble material and diluted with water to precipitate the product, 38 g (wet). After air drying, it was recrystallized from acetone to give 14.6 g of white crystalline product, mp 158°-159° C.
Analysis: Calculated for C 14 H 16 N 3 O 2 Cl: C, 57.24; H, 5.50; N, 14.30. Found: C, 57/26; H, 5.50; N, 14.45.
EXAMPLE 21
3-[(4-Bromo-2.6-dimethylphenyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A mixture of 14.6 g (0.06 mole) of 4-(4-bromo-2,6-dimethylphenyl)-3-thiosemicarbazide and 9.93 g (0.06 mole) of ethyl 2-chloroacetoacetate in 60 mL of absolute ethanol was stirred under nitrogen atmosphere for 2 hr, treated with 30 mL of 2N ethanolic hydrogen chloride and heated at reflux until the reaction mixture cleared (3 hr). The reaction mixture was filtered hot then concentrated in vacuo to give an orange solid which, when triturated with warm benzene/ligroin (50:50) and filtered gave 10.8 g of slightly orange crystalline product. The filtrate upon standing for ˜16 hr gave an additional 4.4 g of yellow crystals which became white when washed with warm acetone. The 2 fractions were combined and recrystallized from benzene/ligroin to give 10.35 g of fine white crystalline rods, mp 171°-199° C. (with degassing). An NMR analysis showed the solid to be a salt with some solvent present; mass spectra confirmed the presence of hydrogen chloride. After drying at 82° C. under high vacuum, there was left 9.56 g, mp 168°-196° C. A broad melting point range suggested that it may be a mixture of free base and salt; therefore, it was dissolved in methanol/water along with other reaction mixture material, made basic with 3N sodium hydroxide and extracted with 5×60 mL of methylene chloride. The extracts were combined, washed with water, dried over magnesium sulfate and concentrated in vacuo to give a dark yellow solid. Recrystallization from benzene/ligroin then from benzene gave 10.7 g of white granular power, mp 184°-185° C.
Analysis: Calculated for C 15 H 18 N 3 O 2 Br: C, 51.15; H, 5.15; N, 11.93. Found: C, 51.19; H, 5.09; N, 12.09.
EXAMPLE 22
5-Methyl-3-(methylamino)-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred mixture of 42 g (0.4 mole) of 4-methyl-3-thiosemicarbazide and 65.8 g (0.4 mole) of ethyl 2-chloracetoacetate in 200 mL of absolute ethanol became exothermic after mixing, warming the mixture nearly to reflux. After stirring for 1 hr the reaction mixture was cooled to ambient temperature. The yellow-green slurry was treated with 200 mL of 2N ethanolic hydrogen chloride and was allowed to stir at ambient temperature for ˜72 hr. The orange-red slurry was heated to reflux and diluted with 1200 mL of hot absolute ethanol leaving only amorphous sulfur which was removed by filtration. The solvent was evaporated in vacuo leaving a crude orange solid which was triturated with refluxing acetone to give 45.6 g of white granular product. Recrystallization from absolute ethanol gave upon cooling a fine granular precipitate; however, after 5 hr fine white needles formed, suggesting the presence of 2 different products. The solid material as well as reaction mixture residues were combined in methanol/water and made basic with 3 N sodium hydroxide. The basic mixture was extracted with 3×200 mL of methylene chloride. The extracts were combined, washed with water (50 mL), dried over magnesium sulfate and concentrated on a rotary evaporator to give a yellow solid. Recrystallization from acetone gave 19.2 g of fine white needles, mp 161°-162° C. A second crude crop of 9 g was obtained from the filtrate.
Analysis: Calculated for C 8 H 13 N 3 O 2 : C, 52.45; H, 7.15; N, 22.94. Found: C, 52.71; H, 7.24; N, 23.25.
EXAMPLE 23
5-Methyl-3-[(2-propenyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A mixture of 26.24 g (0.2 mole) of 4-(2-propenyl)-3-thiosemicarbazide and 32.9 g (0.2 mole) of ethyl 2-chloroacetoacetate in 150 mL of absolute ethanol was stirred under nitrogen atmosphere for 1.5 hr, treated with 100 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1.5 hr. The reaction mixture was stirred at ambient temperature for ˜72 hr, heated to reflux and filtered to remove the amorphous sulfur. The filtrate was concentrated in vacuo to give a deep red oil which crystallized on trituration with acetone to give 29 g of product. Recrystallization from acetone gave 21 g of needle-like crystals tinted with yellow. A second recrystallization from benzene gave 15.8 g of fine white needles, mp 133°-134° C. A rework of the filtrates from both recrystallizations gave an additional 7 g of crude product.
Analysis: Calculated for C 10 H 16 N 3 O 2 Cl: C, 48.88; H, 6.56; N, 17.10. Found: C, 49.20; H, 6.61; N, 17.35.
EXAMPLE 24
3-(Ethylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A mixture of 47.68 g (0.4 mole) of 4-ethyl-3-thiosemicarbazide and 65.8 g (0.4 mole) of ethyl 2-chloracetoacetate was stirred under nitrogen atmosphere for 1.5 hr at ambient temperature then treated with 200 mL of 2N ethanolic hydrogen chloride. The mixture was stirred for ˜72 hr, filtered to remove the amorphous sulfur, and the solvent was removed in vacuo to give a deep amber oil which solidified. Recrystallization from acetone gave 27 g of crude product which was recrystallized from benzene/petroleum ether to give 23.5 g of fine white crystals, mp 140°-148° C. Rework of the filtrate gave an additional 17.5 g of crude product.
Analysis: Calculated for C 9 H 16 N 3 O 2 Cl: C, 46.26; H, 6.90; N, 17.98. Found: C, 46.40; H, 6.91; N, 18.37.
EXAMPLE 25
3-(Cyclohexylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A mixture of 34.7 g (0.2 mole) of 4-cyclohexyl-3-thiosemicarbazide and 32.9 g (0.2 mole) of ethyl 2-chloroacetoacetate in 350 mL of absolute ethanol was stirred under nitrogen atmosphere at ambient temperature for 2 hr, treated with 100 mL of 2N ethanolic hydrogen chloride and heated at reflux for 2 hr. The hot reaction mixture was filtered to remove an amorphous solid. The product persistently crystallized in the filter. The product was recrystallized from acetone and recovered by decating off hot acetone solvent and washing the residue with cold acetone to give 27 g of large, off-white crystals, mp 178-182° C.
Analysis: Calculated for C 13 H 22 N 3 O 2 Cl: C, 54.26; H, 7.71; N, 14.60. Found: C, 54.27; H, 7.71; N, 14.75.
EXAMPLE 26
5-Methyl-3-[(phenylmethyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A mixture of 18 g (0.106 mole) of 4-phenylmethyl-3-thiosemicarbazide and 18 g (0.11 mole) of ethyl 2-chloroacetoacetate in 200 mL of absolute ethanol was stirred at ambient temperature for 1.5 hr then heated at reflux for 2 hr. The clear red-orange reaction mixture was filtered hot to remove amorphous sulfur and concentrated in vacuo to give a crude yellow paste. Trituration with acetone gave 22.8 g of yellow crystalline product. Recrystallization of a 6 g portion from acetone gave 2 products with melting points of 138°-140° C. and 200°-205° C. A sample was dissolved in methanol/water and converted to the free base with 3N sodium hydroxide. The resulting solid was recrystallized from acetone to give 3.3 g f fine white crystals which were dried at 98° C. for 18 hr under reduced pressure (mp 149°-159° C.).
Analysis: Calculated for C 14 H 17 N 3 O 2 : C, 64.84; H, 6.61; N, 16.21. Found: C, 64.45; H, 6.58; N, 16.24.
EXAMPLE 27
3-Amino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred mixture of 9.1 g (0.1 mole) of 3-thiosemicarbazide and 1 mL of concentrated hydrochloride acid in 150 mL of absolute ethanol was cooled to 0° C. in an ice bath and 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate was added dropwise. The thiosemicarbazide dissolved as the reaction mixture was allowed to slowly come to ambient temperature, it then became yellow and a new precipitate formed. The reaction mixture was heated at reflux for 3 hr. All the material had not dissolved so the reaction mixture was diluted with water and made acidic with 3N hydrochloric acid to dissolve all the solids but sulfur. After filtering, the filtrate was concentrated in vacuo leaving an orange-red oil which slowly crystallized when acetone was added to give 11.5 g of orange powder, mp 186°-188° C., with decomposition.
Analysis: Calculated for C 7 H 11 N 3 O 2 : C, 40.89; H, 5.88; N, 20.43. Found: C, 40.64; H, 5.54; N, 20.59.
EXAMPLE 28
3[(1-Adamantyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A mixture of 11.26 g (0.05 mole) of 4-(1-adamantyl)-3-thiosemicarbazide and 8.2 g (0.05 mole) of ethyl 2-chloroacetoacetate in 100 mL of absolute ethanol was stirred at ambient temperature for 2 days, heated at reflux for 2 hr, filtered hot to remove the sulfur, and concentrated in vacuo to give 19 g of white solid residue. The solid was dissolved in methanol/benzene and washed with 3N sodium hydroxide to convert all the material to the free base. The benzene layer was separated, washed with water, dried over magnesium sulfate and concentrated to give a solid residue. After trying to recrystallize the residue from various solvents and solvent mixtures, all 9.5 g was dissolved in acetic acid and treated with concentrated hydrochloric acid which gave 6.8 g of hydrochloride salt when concentrated in vacuo. Recrystallization from acetone/diethyl ether gave 2.5 g of fine white crystals, mp 151°-180° C. Rework of the filtrate gave 5 additional fractions. TLC (10% methanol/benzene; silica gel) showed that only 2 fractions were pure. They were combined (7.6 g) and recrystallized from ethyl acetate to give 4.2 g of fine white crystals, mp 190°-203° C. (red melt).
Analysis: Calculated for C 17 H 26 ClN 3 O 2 : C, 60.08; H, 7.71; N, 12.36. Found: C, 60.31; H, 7.74; N, 12.57.
EXAMPLE 29
3-Dimethylamino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 2.5 g (0.013 mole) of 4,4-dimethyl-3-thiosemicarbazide in 50 mL of absolute ethanol was treated with 2.1 g (0.013 mole) of ethyl 2-chloroacetoacetate added at a rapid rate under nitrogen atmosphere. The reaction mixture turned yellow immediately, cleared, became cloudy and finally became a clear orange solution within 5 minutes. The reaction mixture was stirred at ambient temperature for ˜72 hr, heated to reflux, filtered hot, and concentrated in vacuo to give a yellow oil which solidified. Trituration with benzene gave 3 g of tan solid. After 3 recrystallizations from benzene, 1.8 g of fine pale beige crystalline product was obtained, mp 135°-139° C. After drying at 98° C. under reduced pressure for 3 hr, mp 137-139° C. Analysis: Calculated for C 9 H 16 ClN 3 O 2 : C, 46.26; H, 6.90; N, 17.98. Found: C, 46.05; H, 6.91; N, 18.09.
EXAMPLE 30
5-Methyl-3-[(2-phenylmethyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred slurry of 33.1 g (0.17 mole) of 4-phenylethyl-3-thiosemicarbazide in 500 mL of absolute ethanol under nitrogen atmosphere was treated with 29 g (0.17 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for ˜72 hr, heated to reflux to dissolve most materials, and filtered hot. The filtrate was concentrated in vacuo to give a reddish oil, 71 g. The residue was chromatographed on 800 g Florosil® and eluted first with benzene to remove a yellow band (sulfur) followed by an acetone/benzene gradient which gave two main fractions. These two fractions were combined, and concentrated to give a yellow oil which solidified. Recrystallization (twice) from ligroin gave a fluffy white crystalline product, with small spots of green-yellow color, 12.1 g, mp 138°-139° C.
Analysis: Calculated for C 15 H 19 N 3 O 2 : C, 65.91; H, 7.01; N, 15.37. Found: C, 65.78; H, 6.99; N, 15.42.
EXAMPLE 31
3-Heptylamino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 30.3 g (0.16 mole) of 4-heptyl-3-thiosemicarbazide in 500 mL of absolute ethanol under nitrogen atmosphere was treated with the rapid addition of 26.3 g (0.16 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for ˜16 hr, heated at reflux for 3 hr and filtered hot. Concentration of the filtrate in vacuo gave a deep red oil. The oil solidified on standing for ˜16 hr and was recrystallized from 2-propyl alcohol to give 15 g of fine white crystals, mp 83°-84° C.
Analysis: Calculated for C 14 H 26 ClN 3 O 2 : C, 55.35; H, 8.63; N, 13.83. Found: C, 55.47; H, 8.64; N, 13.91.
EXAMPLE 32
3-[(1,1-Dimethylethyl)amino]-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
A solution of 25 g (0.17 mole) of 4-(1,1-dimethylethyl)-3-thiosemicarbazide in 85 mL of 2N ethanolic hydrogen chloride was cooled to 0° C. with an ice bath and while stirring under nitrogen atmosphere, 28 g (0.17 mole) of ethyl 2-chloroacetoacetate was added dropwise. The reaction mixture was allowed to come to room temperature while stirring for 16 hr. The pale yellow solution was then refluxed for 2 hr during which a film of sulfur deposited on the sides of the flask. The reaction mixture was cooled to room temperature and the sulfur removed by filtration. The filtrate was concentrated in vacuo to give 39 g of pale yellow oil which was dissolved in ligroin and, after standing at ˜7-10° C. for ˜60 hr, yielded 20.5 g of large crystals, mp 118°-119° C. An additional 6.1 g of crude material was obtained by reworking the residues.
Analysis: Calculated for C 10 H 19 N 3 O 2 : C, 58.65; H, 8.50; N, 18.65. Found: C, 58.66; H, 8.54; N, 18.72.
EXAMPLE 33
3-(Cycloheptylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A solution of 11.6 g (0.0619 mole) of 4-cycloheptyl-3-thiosemicarbazide in 100 mL of tetrahydrofuran was stirred under nitrogen atmosphere while 10.2 g (0.062 mole) of ethyl 2-chloroacetoacetate was added. The reaction mixture quickly turned yellow and slowly became exothermic to boiling. The reaction mixture was refluxed for 1.5 hr, filtered (to remove amorphous sulfur), and concentrated in vacuo to give a yellow granular solid, 19.7 g. Several attempts at recrystallization of the material from various solvents resulted in 4 fractions all having melting points in the range of 157°-160° C. These were combined (12 g) and recrystallized from methyl isobutyl ketone, after treating with charcoal, to give 10.3 g of product. After drying at 82° C. under vacuum for 15 hr the weight was reduced to 9.8 g with mp 155°-161° C.
Analysis: Calculated for C 14 H 24 N 3 O 2 Cl: C, 55.71; H, 8.02; N, 13.92. Found: C, 55.85; H, 7.94; N, 13.89.
EXAMPLE 34
3-(Cyclopentylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester hydrochloride [1:1].
A stirred slurry of 8.3 g (0.052 mole) of 4-cyclopentyl-3-thiosemicarbazide in 50 mL of absolute ethanol under nitrogen atmosphere was treated with 8.6 g (0.052 mole) of ethyl 2-chloroacetoacetate. The reaction mixture which, after filtering, turned pale yellow, as stirred for 18 hr at ambient temperature, treated with 20 mL of 2N ethanolic hydrogen chloride and heated at reflux for 1 hr. The reaction mixture was filtered hot and the filtrate concentrated in vacuo to a yellow-orange solid. Most of the solid was dissolved in 100 mL of hot absolute ethanol. The mixture was filtered, and when the filtrate was treated with dipropyl ether (150 mL) a precipitate formed which was collected by filtration to give 11.7 g of crude product. Recrystallization from benzene/ligroin with charcoal treatment gave 7.6 g of fine white fluffy needles, mp 175°-177° C.
Analysis: Calculated for C 12 H 20 N 3 O 2 Cl: C, 52.65; H, 7.36; N, 15.35. Found: C, 52.83; H, 7.33; N, 15.41.
EXAMPLE 35
3-(Cyclopropylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester hydrochloride [1:1].
A stirred slurry of 10.4 g (0.079 mole) of 4-cyclopropyl-3-thiosemicarbazide under nitrogen atmosphere was treated with 13 g (0.079 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 1 hr, treated with 30 mL of 2N ethanolic hydrogen chloride and heated to reflux. The reaction mixture was allowed to cool to ambient temperature while stirring for ˜72 hr. The sulfur residue was removed by filtration and the filtrate concentrated in vacuo to an orange oil which solidified. Recrystallization twice from acetone gave 7.4 g of large blade-like crystals, after drying for 2 hr at 98° C. under reduced pressure, mp 147°-148.5° C. The filtrates gave an additional 6 g of crude product. The 2 solids were combined ad recrystallized from methyl ethyl ketone to give 6.3 g of white crystalline power, mp 151°-152° C.
Analysis: Calculated for C 10 H 16 N 3 O 2 Cl: C, 48.88; H, 6.56; N, 17.10. Found: C, 48.72; H, 6.55; N, 17.28.
EXAMPLE 38
5-Methyl-3-(propylamino)-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 10.1 g (b 0.076 mole) of 4-propyl-3-thiosemicarbazide in 50 mL of absolute ethanol under nitrogen atmosphere was treated with 12.5 g (0.076 mole) of ethyl 2-chloroacetoacetate. After stirring at ambient temperature for 3 hr, it was treated with 20 mL of 2N ethanolic hydrogen chloride, heated at reflux for 45 minutes and cooled to ambient temperature while stirring for ˜72 hr. The reaction mixture was filtered to remove the amorphous sulfur and the filtrate concentrated in vacuo to give an orange paste. Recrystallization from a small amount of cold acetone gave the crude product, which was recrystallized from methyl ethyl keton to give 11.8 g of fine pale beige needles, mp 154°-161° C. TLC (20% methanol/benzene; silica gel) showed one major spot and 2 minor ones. Recrystallized from toluene gave 9.5 g of fine white crystals, mp 155°-161° C.
Analysis: Calculated for C 10 H 18 N 3 O 2 Cl: C, 48.49; H, 7.32; N, 16.96. Found: C, 48.76; H, 7.36; N, 17.19.
EXAMPLE 37
5-Methyl-3-[(1-methylpropyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 5.1 g (0.035 mole) of 4-(2-butyl)-3-thiosemicarbazide in 40 mL of absolute ethanol was treated with 5.7 g (0.035 mole) of ethyl 2-chloroacetoacetate and stirred at ambient temperature for 3 hr. The mixture was treated with 20 mL of 2N ethanolic hydrogen chloride, heated at reflux for 1 hr and stirred for ˜16 hr at ambient temperature. The reaction mixture after filtering and concentrating in vacuo gave a crude orange solid. A second reaction mixture was prepared with 8.0 g (0.054 mole) of crude 4-(2-buytl)-3-thiosemicarbazide, 50 mL of absolute ethanol, 8.9 g (0.054 mole) of ethyl 2-chloroacetoacetate, and 25 mL of 2N ethanolic hydrogen chloride as described above and gave a crude orange solid. The TLC of both crude products (10% methanol/benzene; silica gel) were identical. Recrystallization of the first batch from acetone/isopropyl ether gave 4 g of fine white crystals, mp 147°-148.5° C. Recrystallization of the second batch from benzene/ligroin gave 2.5 g of pale yellow crystalline product, mp 146°-148.5° C. The 2 solids were combined (6.5 g) and recrystallized from 200 mL of acetone/isopropyl ester (3:1) to give 3.6 g of white fluffy crystals, mp 147°-149° C.
Analysis: Calculated for C 11 H 20 N 3 O 2 Cl: C, 50.48; H, 7.70; N, 16.05. Found: C, 50.63; H, 7.70; N, 16.19.
EXAMPLE 38
5-methyl-3(pentylamino)-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred solution of 25.8 g (0.16 mole) of 4-pentyl-3-thiosemicarbazide in 150 mL of tetrahydrofuran was treated with 26.4 g (0.16 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 2 hr, heated at reflux for 4 hr, and stirred for ˜16 hr at ambient temperature. The reaction mixture contained amorphous material and large yellow crystals, which dissolved on heating at reflux for 1 hr. Upon cooling, large yellow crystals separated and were removed by filtration (sulfur). The filtrate was diluted with ice water, made acidic with 6N sulfuric acid and filtered to remove additional sulfur. The filtrate was adjusted to pH 6 with sodium carbonate and a total of 32.2 g of precipitated product was collected in 3 fractions. All the material was chromatographed twice on silica gel without purification, first by eluting with methylene chloride and the second time by eluting with benzene. A third column of 800 g of silica gel was eluted with isopropyl ether to give an orange oil which was not the product, then eluted with 50/50 isopropyl ether/methylene chloride. The product crystallized from the second eluent to give 7.8 g of white crystalline product after washing with isopropyl ether to remove a yellow color, mp 117°-119° C.
Analysis: Calculated for C 12 H 21 N 3 O 2 : C, 60.78; H, 8.85; N, 17.56. Found: C, 60.24; H, 8.88; N, 17.59.
EXAMPLE 39
3-(Hexylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 15.8 g (0.091 mole) of 4-hexyl-3-thiosemicarbazide in 150 mL of absolute ethanol under nitrogen atmosphere was treated with 14.8 g (0.091 mole) of ethyl 2-chloroacetoacetate, stirred for 2.5 hr at ambient temperature, treated with 50 mL of 2N ethanolic hydrogen chloride, heated at reflux for 1 hr, and stirred at ambient temperature ˜16 hr. The reaction mixture was heated to dissolve most of the solids, filtered to remove the insoluble sulfur and concentrated in vacuo to give a deep red-orange oil. After standing for 3 weeks at ambient temperature, the oil began to crystallize. Trituration with ethyl acetate and filtration gave 13 g of crude product, which was recrystallized from acetone/diethyl ether to give 7.5 g of white granular product, mp 108°-109° C.
Analysis: Calculated for C 13 H 24 N 3 O 2 Cl: C, 53.88; H, 8.35; N, 14.50. Found: C, 53.71; H, 8.38; N, 14.71.
EXAMPLE 40
3-(Cyclooctylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 18.7 g (0.093 mole) of 4-cyclooctyl-3-thiosemicarbazide in 150 mL of absolute ethanol under nitrogen atmosphere was treated with 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 1.5 hr, treated with 50 mL of 2N ethanolic hydrogen chloride and heated at reflux for ˜16 hr. The yellow-brown reaction mixture was filtered and concentrated in vacuo to a dark oil which solidified. Trituration of the crude product with warm acetone removed most of the color to give 17.9 g of product. Recrystallization from methyl ethyl ketone/isopropyl ether followed by recrystallization from methyl ethyl ketone gave 7.1 g of crystalline product, mp 161°-166° C. which was dried at 82° C. under reduced pressure for 3 hr (mp, 168°-171° C.).
Analysis: Calculated for C 15 H 26 N 3 O 2 Cl: C, 57.04; H, 8.30; N, 13.30. Found: C, 56.98; H, 8.33; N, 13.48.
EXAMPLE 41
5-Methyl-3-[(2-methylbutyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred pale yellow solution of 14.3 g (0.089 mole) of 4-(2-methylbutyl)-3-thiosemicarbazide in 50 mL of absolute ethanol was cooled to -10° C. in an ice/methanol bath and treated under nitrogen atmosphere with 15 g (0.09 mole) of ethyl 2-chloroacetoacetate. The reaction mixture was stirred for 2 hr at 15° C., heated to reflux, treated with 50 mL of 2N ethanolic hydrogen chloride and after 1 hr at reflux, filtered to remove the amorphous sulfur. The filtrate was concentrated in vacuo to give a deep red oil, 26.8 g, which failed to crystallize. The TLC (10% methanol/methylene chloride; silica gel) showed at least 10 spots. A sample (9 g) of the oil was dissolved in isopropyl ether, and extracted with 6N sulfuric acid. The combined aqueous acid portions were cooled in an ice bath and neutralized with base to give a yellow oil. This oil was extracted into methylene chloride which was dried over magnesium sulfate and concentrated to give 5.7 g of yellow oil. The oil was dissolved in benzene, treated with 30 g of Florisil®, stirred for ˜16 hr, and filtered. The Florisil® was washed with methylene chloride until the effluent was clear, and then washed with methanol until clear. The methanol fractions were combined, concentrated in vacuo to give 3.5 g of pale yellow oil which was dissolved in diethyl ether, cooled to -50+ C. and filtered to remove some insoluble Florisil®. The filtrate was treated with ethereal hydrogen chloride to give a fine crystalline product, 4.1 g. Recrystallization from isopropyl ether gave 2.8 g of silver plate-like crystals, mp 130-133° C.
Analysis: Calculated for C 12 H 22 N 3 O 2 Cl: C, 52.26; H, 8.04; N, 15.24. Found: C, 52.23; H, 8.09; N, 15.43.
EXAMPLE 42
5-Methyl-3-[(1,1,3,3,-tetramethylbutyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 19.5 g (0.096 mole) of 4-(1,1,3,3-tetramethylbutyl)-3-thiosemicarbazide in 100 mL of absolute ethanol under nitrogen atmosphere was treated with 16.5 g (0.1 mole) of ethyl 2-chloroacetoacetate (slightly exothermic). The reaction mixture was stirred at ambient temperature for 1 hr, treated with 50 mL of 2N ethanolic hydrogen chloride, heated at reflux for 1 hr and stirred for ˜72 hr at ambient temperature. A precipitate of amorphous sulfur indicated that the reaction was complete. The sulfur was removed by filtration, the filtrate concentrated in vacuo and the residue when triturated with hot acetone gave a pale yellow insoluble crystalline solid. The supernate fractions were combined and yielded 3.5 g of fine white crystals on cooling, mp 167°-168° C. After 24 hr an additional crop of crystals was obtained from the acetone filtrate. Mass spectra showed all the solids to be expected product. TLC (10% methanol/benzene; silica gel) showed 1 major spot for each fraction.
Analysis: Calculated for C 15 H 28 N 3 O 2 Cl: C, 56.68; H, 8.88; N, 13.22. Found: C, 56.68; H, 8.85; N, 13.33.
EXAMPLE 43
3-(Dibutylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred solution of 14.3 g (0.07 mole) of 4,4-di-n-butyl-3-thiosemicarbazide in 100 mL of absolute ethanol was cooled to 10° C. under nitrogen atmosphere, treated with 11.6 g (0.07 mole) of ethyl 2-choroacetoacetate, warmed to 60° C., then cooled to ambient temperature and stirred for 18 hr. The reaction mixture was heated to reflux in order to dissolve the precipitate, filtered to remove amorphous sulfur and concentrated in vacuo to give a solid. The solid was recrystallized from acetone to yield 8 g of white crystalline product, mp 159°-162° C., as the hydrochloride salt.
Analysis: Calculated for C 15 H 28 ClN 3 O 2 : C, 56.68; H, 8.88; N, 13.22. Found: C, 56.67; H, 8.97; N, 13.25.
EXAMPLE 44
5-Methyl-3-(4-morpholinyl)-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 6.3 g (0.039 mole) of 4-morpholinecarbothioic acid hydrazide in 75 mL of absolute ethanol under nitrogen atmosphere was treated with 6.43 g (0.039 mole) of ethyl 2-chloroacetoacetate and the exothermic reaction mixture stirred at ambient temperature for 18 hr. The major portion of reaction mixture solids were dissolved by heating to reflux, the sulfur residue removed by filtration and the filtrate concentrated in vacuo to a solid, which was crystallized from 2-propyl alcohol to yield 5.5 g of white crystalline needles, mp 165°-173° C., as the hydrochloride salt.
Analysis: Calculated for C 11 H 18 N 3 O 3 Cl: C, 47.92; H, 6.58; N, 15.24. Found: C, 47.68; H, 6.60; N, 15.28.
EXAMPLE 45
3-(Cyclohexylamino)-5-methyl-1H-pyrazole-4-carboxylic acid.
A solution of 2 g (0.007 mole) of 3-cyclohexylamino-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester hydrochloride [1:1] in 30 mL of ethanol was treated with 5 mL of 50% sodium hydroxide solution, 20 mg of tetrabutylammonium bromide and stirred rapidly while heating at reflux. After 20 hr the reaction mixture was diluted with ice water, extracted with 6×100 mL of isopropyl ether, the pH adjusted to 7 with concentrated sulfuric acid and to pH 5.5 with 10 g of sodium dihydrogen phosphate. The fine precipitate was collected by filtration to give 0.6 g of beige power, mp 162°-163° C. (degasses).
Analysis: Calculated for C 11 H 17 N 3 O 2 : C, 59.17; H, 7.68; N, 18.82. Found: C, 59.13; H, 7.67; N, 18.72.
EXAMPLE 46
3-(Cyclohexylmethylamino)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 11.6 g (0.062 mole) of 4-cyclohexyl-4-methyl-3-thiosemicarbazide in 60 mL of absolute ethanol under nitrogen atmosphere was treated with 10.2 g (0.062 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 4 hr, treated with 35 mL of 2N ethanolic hydrogen chloride, and head at reflux until clear. The hot reaction mixture was filtered to remove amorphous sulfur and the red filtrate concentrated in vacuo. The oily residue which crystallized when triturated with acetone gave 14 g of crude product. Recrystallization from 2-propyl alcohol/2-propyl ether gave 7.9 g of crystalline product, mp 156°-158° C., as the hydrochloride salt.
Analysis: Calculated for C 14 H 23 N 3 O 2 Cl: C, 55.71; H, 8.02; N, 13.92. Found: C, 55.66; H, 8.04; N, 13.94.
EXAMPLE 47
3-(Cyclopentylmethylamino)-5-methyl1H-pyrazole-4-carboxylic acid, ethyl ester hydrochloride [1:1].
A stirred slurry of 8.4 g (0.049 mole) of 4-cyclopentyl-4-methyl-3-thiosemicarbazide in 50 mL of absolute ethanol was treated with 8.1 g (0.049 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 18 hr, treated with 25 mL of 2N ethanolic hydrogen chloride and heated at reflux for 2 hr. The hot solution was filtered to remove amorphous sulfur and concentrated to a red oil which gave a crude solid product when triturated with acetone. After four recrystallizations, methyl ethyl ketone/2-propyl ether (twice), acetonitrile/acetone and finally from acetonitrile, there was obtained 3.2 g of crystalline product, mp 144°-146° C., as the hydrochloride salt.
Analysis: Calculated for C 13 H 22 N 3 O 2 Cl: C, 54.26; H, 7.71; N, 14.60. Found: C, 54.06; H, 7.70; N, 14.59.
EXAMPLE 48
3-[[3-(Dimethylamino)propyl]amino]-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester hydrochloride [1:2].
A stirred solution of 7.05 g (0.04 mole) of 4-(3-dimethylaminopropyl)-3-thiosemicarbazide in 50 mL of absolute ethanol under nitrogen atmosphere was treated with 40 mL of 2N ethanolic hydrogen chloride and then with 6.6 g (0.04 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 2 hr and heated at reflux for 5 hr. The reaction mixture was filtered hot to remove some crystalline sulfur and the filtrate solidified on cooling to give 8.3 g of crude product. After 5 recrystallizations from methyl ethyl ketone/methanol with charcoal treatment of the final recrystallization, a crystalline product was obtained, 3,4 g, mp 195°-196° C. After drying at 82° C. under reduced pressure, it was submitted for elemental analysis.
Analysis: Calculated for C 12 H 24 N 4 O 2 Cl 2 : C, 44.04; H, 7.39; N, 17.12. Found: C, 43.94; H, 7.39; N, 17.20.
EXAMPLE 49
5-Methyl-3-[[2-(1-piperidinyl)ethyl]amino]-1H-pyrazole-4-carboxylic acid ethyl ester, hydrochloride [1:2].
A stirred solution of 6 g (0.03 mole) of 4-(2-piperidinoethyl)-3-thiosemicarbazide in 30 mL of 2N ethanolic hydrogen chloride was diluted to 60 mL with absolute ethanol, treated with 4.9 g (0.03 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 3 hr, and heated at reflux for 2 hr. The reaction mixture was filtered hot to remove amorphous sulfur and the filtrate concentrated to an orange oil. Trituration with refluxing 2-propyl ether and cooling gave a plastic mass with crystals. The 2-propyl ether was decanted and the residual material recrystallized from 2-propyl alcohol/2-propyl ether to give 8 g of crude product. A second recrystallization from 2-propyl alcohol/2-propyl ether gave 5.3 g of beige crystalline product, mp 198°-200° C. as the dihydrochloride salt.
Analysis: Calculated for C 14 H 26 N 4 O 2 Cl 2 : C, 47.60; H, 7.42; N, 15.86. Found: C, 47.49; H, 7.48; N, 15.88.
EXAMPLE 50
5-Methyl-3-[(1-methylethyl)amino]-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:1].
A stirred slurry of 10.5 g (0.079 mole) of 4-(2-propanyl)-3-thiosemicarbazide in 100 mL of tetrahydrofuran under nitrogen atmosphere was treated with 13 g (0.079 mole) of ethyl 2-chloroacetoacetate. After 30 minutes the reaction mixture became suddenly exothermic, turning green-yellow and amorphous sulfur separated. The reaction mixture was stirred at ambient temperature for 2 hr, diluted with water, made acidic with 3N hydrochloric acid and filtered to remove the insoluble sulfur. The filtrate was adjusted to pH 8 with sodium carbonate and extracted with 3×50 mL of methylene chloride. The extracts were combined, washed with water, dried over magnesium sulfate and the filtrate concentrated in vacuo. The oily residue in acetone was treated with ethereal hydrogen chloride and diluted with an equal volume of isopropyl ether to five the crude product. Recrystallization from acetone gave 6.6 g of large beige crystals, mp 158°-159° C., as the hydrochloride salt.
Analysis: Calculated for C 10 H 18 N 3 O 2 Cl: C, 48.49; H, 7.32; N, 16.96. Found: C, 48.57; H, 7.34; N, 17.13.
EXAMPLE 51
5-Methyl-3-[[2-(4-morpholinyl)ethyl]amino]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred solution of 10 g (0.049 mole) of 4-[2-(4-morpholino)ethyl]-3-thiosemicarbazide in 50 mL of absolute ethanol under nitrogen was treated with 25 mL of 2N ethanolic hydrogen chloride and 8.1 g (0.05 mole) of ethyl 2-chloroacetoacetate, stirred at ambient temperature for 2 hr and heated at reflux for 3 hr. The reaction mixture was filtered hot to remove amorphous sulfur and concentrated to an orange oil, 23 g. Trituration of the residue with refluxing acetone gave upon cooling a three-phase mixture consisting of solid, oil, and acetone. The solid material could not be separated from the oil. All the reaction mixture material was stirred in methanol/water and filtered through Celite® to remove sulfur. The filtrate was extracted with 100 mL of benzene, and adjusted to pH 8 with sodium carbonate, extracted with 2×100 mL of 2-propyl ether (no product) and extracted with 4×100 mL of methylene chloride. The methylene chloride extracts were combined, dried over magnesium sulfate and concentrated in vacuo to give a paste-like solid. Trituration of the residue with 2-propyl ether gave a yellow powder, 4.2 g, mp 124°-125° C. Recrystallization from 2-propyl ether gave 3.9 g of yellow power, mp 124°-125° C.
Analysis: Calculated for C 13 H 22 N 4 O 3 : C, 55.30; H, 7.85; N, 19.84. Found: C, 55.48; H, 7.93; N, 19.58.
EXAMPLE 52
5-Methyl-3-(4-phenyl-1-piperazinyl)-1H-pyrazole-4-carboxylic acid, ethyl ester.
A solution of 9 g (0.038 mole) of 4-(4-phenyl-1-piperazine)carbothioic acid hydrazide in 50 mL of 2N ethanolic hydrogen chloride was treated while stirring under nitrogen atmosphere with 6.3 g (0.038 mole) of ethyl 2-chloroacetoacetate. After stirring for 2 hr at room temperature the reaction mixture slurry was heated at reflux until it became clear (˜4 hr). The reaction mixture was allowed to stir for ˜16 hr without heating. The resulting solid product was dissolved by adding an additional 50 mL of absolute ethanol and heating to reflux. The hot solution was filtered to remove amorphous sulfur and upon cooling the product crystallized from the filtrate. Filtration gave 9.3 g of a pale beige power, mp 164°-169° C. All the product was dissolved in warm water and converted to the free base by the addition of 3N sodium hydroxide to pH 10. The oil which separated crystallized slowly and after isolation by filtration it was recrystallized from ethanol/water to five 3.7 g of silver plate-like crystals, mp 137°-138° C.
Analysis: Calculated for C 17 H 22 N 4 O 2 : C, 64.95; H, 7.05; N, 17.82. Found: C, 64.97; H, 7.07; N, 17.82.
EXAMPLE 53
5-Methyl-3-[3-(4-morpholino)propylamino]-1H-pyrazole-4-carboxylic acid, ethylester, oxalate [1:2].
A solution of 10 g (0.46 mole) of 4-[3-(4-morpholino)propyl]-3-thiosemicarbazide in 150 mL of tetrahydrofuran was treated with 4.1 mL (0.05 mole) of concentrated by hydrochloric acid. The curd-like material was stirred while 7.6 g (0.046 mole) of ethyl 2-chloroacetoacetate was added. The reaction mixture was stirred for 18 hr at room temperature, then heated at reflux for 3 hr. Upon cooling, the solid was removed by filtration, dissolved in water, and the insoluble sulfur removed by filtration. The filtrate was made basic with sodium carbonate and extracted with 3×25 mL of methylene chloride which upon drying and concentrating gave 5.8 g of orange oil. The basic aqueous phase was saturated with salt, but further extractions with methylene chloride gave no additional material. After the water had evaporated from the brine solution the resulting solids were triturated with 5×100 mL of boiling isopropyl alcohol. The alcohol portions were combined and concentrated to an orange oil. TLC indicated that a majority of the residues were the starting thiosemicarbazide. All the residual oils were combined, dissolved in 150 mL of 2N ethanolic hydrogen chloride, and then treated with 7.6 g (0.046 mole) of ethyl 2-chloroacetoacetate. The reaction mixture was heated at reflux for 2 hr and the amorphous sulfur formed was removed by filtration. The filtrate was concentrated on a rotary evaporator to give an orange semi-solid residue. This material was dissolved in hot isopropyl alcohol and upon cooling 7 g of fine yellow powder was collected by filtration. The next day the yellow power had changed to an orange oil (hydroscopic). This oil was dissolved in 100 mL of isopropyl alcohol and washed with 50% sodium by hydroxide (25 mL). The 2-propyl alcohol solution was treated with oxalic acid and after heating to dissolve the solid material, filtration and cooling gave in 2 crops a total of 4.4 g of pale yellow granular product, mp, plastic 141°-143° C., and degasses at 155°-157° C.
Analysis: Calculated for C 18 H 28 N 4 O 10 : C, 45.38; H, 5.92; N, 11.76. Found: C, 45.23; H, 5.91; N, 11.59.
EXAMPLE 54
5-Methyl-3-[4-(phenylmethyl)-1-piperazinyl]-1H-pyrazole-4-carboxylic acid, ethyl ester.
A stirred solution of 89 g (0.36 mole) of 4-(methylphenyl)piperazinecarbothoic acid hydrazide in 500 mL of 2N ethanolic hydrogen chloride under nitrogen atmosphere was treated with 58.5 g (0.36 mole) of ethyl 2-chloroacetoacetate. The reaction mixture turned yellow quickly and was stirred at ambient temperature for 4 hr, heated at reflux for 1 hr and stirred for ˜16 hr at ambient temperature. The yellow-white precipitate could not be dissolved in the reaction mixture solvent by heating, or after adding 700 mL of additional ethanol and heating to reflux. The reaction mixture was cooled and the solid removed by filtration, yielding 158.8 g of mostly white product tinged with yellow sulfur. A sample was recrystallized 3 times from ethanol, mp 218°-222° C. (degasses). A 12 g portion was recovered from a second reaction mixture as the crystalline free base and recrystallization of this material from 2-propyl ether/ligroin with aid of a soxhlet extraction gave 8.3 g of white crystalline product, mp 124-126° C.
Analysis: Calculated for C 18 H 24 N 4 O 2 : C, 65.83; H, 7.37; N, 17.06. Found: C, 65.96; H, 7.39; N, 17.13.
EXAMPLE 55
5-Methyl-3-(1-piperazinyl)-1H-pyrazole-4-carboxylic acid, ethyl ester, hydrochloride [1:2].
A slurry of 10 g (0.03 mole) of 5-methyl-3-[(4-phenylmethyl)-1-piperazinyl]-1H-pyrazole-4-carboxylic acid ethyl ester in 150 mL of ethanol was treated with 50 mL of 3N hydrochloric acid then with 1 g of 5% palladium on carbon. This mixture was hydrogenated on a Parr apparatus with 43 psi of hydrogen gas at ˜60° C. After 3 hr, the reaction mixture was cooled, filtered to remove the catalyst, and the filtrate concentrated in vacuo to give a solid residue. Recrystallization from absolute ethanol yielded 6.8 g of white crystalline product, mp 254°-256° C., with degassing.
Analysis: Calculate for C 11 H 20 N 4 O 2 Cl 2 : C, 42.45; H, 6.48; N, 18.00. Found: C, 42.46; H, 6.44; N, 17.93.
EXAMPLE 56
5-Methyl-3-[4-(trifluoromethyl)phenylamino]-1H-pyrazole-4-carboxylic acidethyl ester.
When in the procedure of Example 1 and utilizing Method A, reacting the following in sequence:
(1) 4-[4-(trifluoromethyl)phenyl-3-thiosemicarbazide, and
(2) ethyl 2-chloroacetoacetate, the title compound is obtained.
EXAMPLE 57
When in the procedure of Example 45 and substituting the following for 4-morpholine carbothioic acid hydrazide:
(a) 1-pyrrolidinecarbothioic acid hydrazide
(b) 1-piperidinecarbothioic acid hydrazide
(c) 1-homopiperidinecarbothioic acid hydrazide
there are obtained:
(a) 5-methyl-3-(1-pyrrolidinyl)-1H-pyrazole-4-carboxylic acid, ethyl ester
(b) 5-methyl-3-(1-piperidinyl)-1H-pyrazole-4-carboxylic acid, ethyl ester
(c) 3-(1-homopiperidinyl)-5-methyl-1H-pyrazole-4-carboxylic acid, ethyl ester.
__________________________________________________________________________ ##STR7## Formula IExample MeltingNumber R.sup.1 NR.sup.2 R.sup.3 Salt Point__________________________________________________________________________1 C.sub.2 H.sub.5 NHC.sub.6 H.sub.5 -- 165-166° C.2 C.sub.2 H.sub.5 NH[4-Cl(C.sub.6 H.sub.4)] -- 223-225° C.3 C.sub.2 H.sub.5 NH[3-SCH.sub.3 (C.sub.6 H.sub.4)] -- 191.5-194° C.4 C.sub.2 H.sub.5 (1-naphthalenyl)amino -- 199-202° C.5 C.sub.2 H.sub.5 NH[2-SCH.sub.2 (C.sub.6 H.sub.4)] -- 14.5-142° C.6 C.sub.2 H.sub.5 NH[2,6-(CH.sub.2).sub.2 (C.sub.6 H.sub.3)] -- 142-144° C.7 C.sub.2 H.sub.5 NH[2-OCH.sub.3 (C.sub.6 H.sub.4)] -- 184-191° C.8 C.sub.2 H.sub.5 NH[2-CH.sub.3 (C.sub.6 H.sub.4)] -- 160-161° C.9 C.sub.2 H.sub.5 NH[2,6-Cl.sub.2 (C.sub.6 H.sub.3)] -- 191-192° C.10 C.sub.2 H.sub.5 NH[2-Cl.sub.2 (C.sub.6 H.sub.4)] -- 188-189° C.11 C.sub.2 H.sub.5 NH[2,4-(OCH.sub.3).sub.2 (C.sub.6 H.sub.3)] HC[1:1] 199-200° C.12 C.sub.2 H.sub.5 NH[3-C(C.sub.6 H.sub.4)] -- 159.5-160° C.13 C.sub.2 H.sub.5 (2-pyridinyl)amino -- 155°-156° C.14 C.sub.2 H.sub.5 NH[CH.sub.2).sub.3 CH.sub.3 ] -- 109-110° C.15 C.sub.2 H.sub.5 NH[CH.sub.2).sub.3 CH.sub.3 ] sulfate[1:1] 81-83° C.16 C.sub.2 H.sub.5 NH[2,6-(C.sub.2 H.sub.5 ).sub.2 (C.sub.6 H.sub.3) HC[1:1] 167-170° C.17 C.sub.2 H.sub.5 NH[2,4-(CH.sub.3).sub.2 (C.sub.6 H.sub.3)] -- 174.5-176° C.18 C.sub.2 H.sub.5 NH[2-CH.sub.34-C](C.sub.6 H.sub.3) -- 156-187° C.19 C.sub.2 H.sub.5 NH[2,4-Cl.sub.2 (C.sub.6 H.sub.3)] -- 214-217° C.20 C.sub.2 H.sub.5 NH[2-Cl,6-CH.sub.3 (C.sub.6 H.sub.3)] -- 158-159° C.21 C.sub.2 H.sub.5 NH[2,6-(CH.sub.3).sub.2,4-Br(C.sub.6 H.sub.2)] -- 184-185° C.22 C.sub.2 H.sub.5 NHCH.sub.3 -- 161-162° C.23 C.sub.2 H.sub.5 NH(CH.sub.2 CHCH.sub.2) HCl[1:1] 133-134° C.24 C.sub.2 H.sub.5 NH(C.sub.2 H.sub.5) HCl[1:1] 140-148° C.25 C.sub.2 H.sub.5 NH(C.sub.6 H.sub.11) HCl[1:1] 178-182° C.26 C.sub.2 H.sub.5 NH[CH.sub.2 (C.sub.6 H.sub.5)] -- 149-150° C.27 C.sub.2 H.sub.5 NH.sub.2 HCl[1:1] 186-188° C.28 C.sub.2 H.sub.5 (1-adamantyl)amino -- 190-203° C.29 C.sub.2 H.sub.5 N(CH.sub.3).sub.2 HCl[1:1] 137-139° C.30 C.sub.2 H.sub.5 NH[(CH.sub.2).sub.2C.sub.6 H.sub.5 ] -- 138-139° C.31 C.sub.2 H.sub.5 NH[(CH.sub.2).sub.6CH.sub.3 ] HCl[1:1] 83-84° C.32 C.sub.2 H.sub.5 NH[C(CH.sub.3).sub.3 ] -- 118-119° C.33 C.sub.2 H.sub.5 NH[C.sub.7 H.sub.13 ] HCl[1:1] 155-161° C.34 C.sub.2 H.sub.5 NH[C.sub.5 H.sub.9 ] HCl[1:1] 175-177° C.35 C.sub.2 H.sub.5 NH[C.sub.3 H.sub.5 ] HCl[1:1] 151-152° C.36 C.sub.2 H.sub.5 NH[(CH.sub.2).sub.2CH.sub. 3 ] HCl[1:1] 155-161° C.37 C.sub.2 H.sub.5 (1-methylpropyl)amino HCl[1:1] 147-149° C.38 C.sub.2 H.sub.5 NH(CH.sub.2).sub.4CH.sub.3 ] -- 117-119° C.39 C.sub.2 H.sub.5 NH(CH.sub.2).sub.5 CH.sub.3 ] HCl[1:1] 108-109° C.40 C.sub.2 H.sub.5 NH[C.sub.8 H.sub.15 ] HCl[1:1] 168-171° C.41 C.sub.2 H.sub.5 (2-methylbutyl)amino HCl[1:1] 130-133° C.42 C.sub.2 H.sub.5 (1,1,3,3-tetramethylbutyl) HCl[1:1] 167-168° C. amino43 C.sub.2 H.sub.5 N[(CH.sub.2).sub.3 CH.sub.3 ].sub.2 HCl[1:1] 159-162° C.44 C.sub.2 H.sub.5 4-morpholinyl Hcl[1:1] 165-173° C.45 H NH(C.sub.6 H.sub.11) -- 162-163° C.46 C.sub.2 H.sub.5 N(CH.sub.3)(C.sub.6 H.sub.11) HCl[1:1] 156-158° C.47 C.sub.2 H.sub.5 N(CH.sub.3)(C.sub.5 H.sub.9) HCl[1:1] 144-146° C.48 C.sub.2 H.sub.5 NH[(CH.sub.2).sub.3N(CH.sub.3).sub.2 ] HCl[1:2] 195-196° C.49 C.sub.2 H.sub.5 [2-(1-iperidinyl)ethyl- HCl[1:2] 198-200° C. amino50 C.sub.2 H.sub.5 NH[CH(CH.sub.3).sub.2 ] HCl[1:1] 158-159° C.51 C.sub.2 H.sub.5 [2-(4-morpholinyl)ethyl]- -- 124-125° C. amino52 C.sub.2 H.sub.5 4-phenyl-1-piperazinyl -- 137-138° C.53 C.sub.2 H.sub.5 [3-(4-morpholino)propyl]- oxalate [1:2] 155-157° C. amino54 C.sub.2 H.sub.5 4-(phenylmethyl)-1- -- 124-126° C. piperazinyl55 C.sub.2 H.sub.5 1-piperazinyl HCl[1:2] 254-256° C.56 C.sub.2 H.sub.5 NH[4-CF.sub.3(C.sub.6 H.sub.4)] -- --57a C.sub.2 H.sub.5 1-pyrrolidinyl -- --57b C.sub.2 H.sub.5 1-piperidinyl -- --57c C.sub.2 H.sub.5 1-homopiperidinyl -- --__________________________________________________________________________
PHARMACOLOGICAL TEST PROCEDURES MUSCLE RELAXANT TEST
The test procedure used to indicate positive muscle relaxant activity is the Morphine-Induced Straub Tail Test described by G. D. Novak in Drug Development Research (1982) 2:383-386, except 8 animals per group were used rather than 10 per test. The test is summarized as follows: the test drug, reference drug, and control articles to be administered are prepared in saline, 0.5% aqueous methylcellulose suspension, or other solvent depending on solubility, in such concentration that the volume administered is 10 mL/kg. The initial screening dose of the test drug is usually 100 mg/kg. Groups of 8 mice are given an intraperitoneal dose of a compound or vehicle prepared as described above. After 15 min, mice are administered morphine sulfate, 60 mg/kg, subcutaneously. Fifteen minutes after administration of morphine (i.e., 30 min after test compound administration), mice were scored for presence of Straub Tail, defined as an elevation of the tail at least 90 degrees from the horizontal. An ED 50 value may be determined from at least three logarithmically spaced doses, using the method of Litchfield and Wilcoxon (1949), J. Pharmacol. Exp. Ther. 96:99-113. Illustratively, some of more active compounds such as those prepared in Examples 39 and 43 exhibited ED 50 values of 15-50 mg/kg in the foregoing Straub Tail Test.
Anticonvulsant activity was determined for compounds of Formula I as evidenced by using chemical or electrical challenge as follows:
Metrazole Chemical Challenge
(Swinyard Method)
Groups of 8 adult female mice were randomly assigned to dosage groups according to the method of Steel, R. G. C., and Torrie, J. H. (1960) in "Principles and Procedures of Statistics," McGraw-Hill Book Company, Inc., pp 99-100, pp 428-31. Each mouse was identified with a color code on its tail. The test compounds were administered as solutions or suspensions in 10 mL/kg mouse body weight of 0.5% aqueous methylcellulose suspension within 15 minutes of preparation of the suspension. Metrazole® (pentylenetetrazol) was prepared as a solution in physiological saline. The mice were not fasted prior to the test. Eight mice were tested at each dosage level.
Each mouse received one dose of the test drug (usually 100 mg/kg for screening) in 0.5% aqueous methylcellulose or the control article (0.5% aqueous methylcellulose alone) intraperitoneally. Metrazole (80 mg/kg S.C.) was then given in a loose fold of skin on the back of the neck 0.5 hr after the test compound or control article was given. Injections were given with a 1 mL glass tuberculin syringe with appropriate size hypodermic needle (27 gauge for solutions; 23 gauge for suspensions). All injections were given in a volume of 10 mL/kg mouse body weight. Each mouse was observed for 30 minutes following Metrazol injection. Failure of the animals to exhibit a threshold seizure (a single episode of clonic spasms at least 5 seconds in duration) was defined as protection. Anticonvulsant data were tabulated as the percent protection, i.e., ##EQU1## The ED 50 , 95% confidence limits and potency ratio may be ascertained by the computer-based probit analysis ascribed to Finney, D. J., Statistical Method in Biological Assay, 2nd Ed., Hefner Publishing Co., New York (1964). Illustratively, some of the more active compounds such as those of Examples 14, 25, 33, 40, and 42 exhibit ED 50 values of 20-50 mg/kg in the foregoing metrazole test.
Electrical Challenge
Adult female mice in groups of eight were administered the test drug intraperitoneally (usually 100 mg/kg initially for screening) in liquid carrier, usually physiological saline, water or 0.5% aqueous methylcellulose suspension as described above. Animals were challenged electrically by placing brass electrodes on the corneas and applying an electrical stimulus (60 Hz, 5 m sec. pulse width, 34 mA intensity) for 0.2 seconds by way of a Grass Stimulator® and constant current unit and a Hunter Timer®. The absence of tonic seizures upon cessation of the stimuli was scored as protection in that animal. The number of animals protected from tonic seizures at a given dose of test drug was determined. The ED 50 , 95% confidence limits and potency ratio may be ascertained by the method of J. T. Litchfield and F. Wilcoxon (1949) J. Pharmacol. Exp. Ther. 96, 99-113. Illustratively, some of the more active compounds such as those of Examples 15, 25, 33, 34, 35, 36, 37, 40, 42, 44, 47, and 50 exhibit ED 50 values in the range of 10-50 mg/kg.
Antianxiety Test
The test screening procedure used on to indicate positive antianxiety response is a modification of the Vogel Conflict Test which is based on shocksuppressed drinking behavior in rats outlined by J. R. Vogel, et al., in Psychopharmacology 21:1-7 (1971). The procedure used is as follows: the test, reference, and control articles are administered intraperitoneally in physiological saline, 0.5% aqueous methylcellulose, or other solvent depending on a solubility in such concentration that the volume administered is 5 mg/kg. The initial screening dose of the test article is usually 100.0 mg/kg.
Prior to dosing, rats are housed 2 per cage and deprived of water for 48 hr and thereafter randomized into treatment groups of five. Feed is available ad libitum. Thirty minutes after dosing, each rat is placed individually in a plexiglass cage measuring 18 cm in width, 13 cm in height, and 29.5 cm in length and equipped with a stainless-steel grid floor. The cage is covered with a plastic lid containing holes to facilitate introduction of a water bottle (30 mL plastic centrifuge tube) with a rubber stopper and metal drinking tube. A Drinkometer circuit (Omniteck Electronics, Inc., 3000 Cortona Road, Columbus, Ohio 43204) is connected between the drinking tube and the grid floor of the apparatus so that the rat completes the circuit whenever it licks the tube. The procedure is to allow the rat to find the drinking tube and complete 20 licks as displayed on the Drinkometer digital readout) prior to the start of the experimental session. Rats not reaching this criterion are discarded. A three minute experimental session is initiated by a 0.25 mA shock at the 20th lick. Rats that continue drinking will experience a shock at each successive 20th lick. The total number of shocks during the experimental session are as follows: ##EQU2## Statistical analysis is performed by the Dunn's Multiple Comparison Test described by O. J. Dunn, Technometrics, 6(3):241-52 1964). The mean number of shocks experienced by the control group is compared with those of each drug-treated group. Significance is considered at P<0.1. The higher the total shocks compared to control, the more active is the compound. Active compounds may then be similarly tested at reduced dosages. Five rats were tested at a given dosage level and 5 rats were used as controls. Illustratively, some of the more active compounds such as those of Examples 14, 33 and 35 exhibited MED (Minimum Effective Dose) values of 3-100 mg/kg in the foregoing Vogel Conflict Test.
Pharmaceutical Compositions
The methods of treating anxiety, muscle tension, and spasticity in mammals are best carried out by administering as active ingredients in a pharmaceutical composition at least one of the compounds of Formula I in association with a pharmaceutically acceptable carrier or excipient. The compounds are thus presented in a therapeutic composition suitable for oral, rectal, parenteral, subcutaneous, intramuscular, intraperitoneal, or intravenous administration. Thus, for example, the composition for oral administration can take the form of elixirs, capsules, tablets, or coated tablets containing carriers or excipients conveniently used in the pharmaceutical art. Suitable tableting excipients include lactose, potato, and maize starches, talc, gelatin, stearic and silicic acids, magnesium stearate and polyvinyl pyrrolidone.
For parenteral administration the carrier can be comprised of a sterile parenterally acceptable liquid; e.g., water or arachis oil contained in ampoules.
In compositions for rectal administration, the carrier or excipient can be comprised of a suppository base; e.g., cocoa butter or glyceride.
Advantageously, the compositions are formulated as dosage units, each unit being adapted to supply a fixed dose of active ingredient. Tablets, coated tablets, capsules, ampoules and suppositories are examples of preferred dosage forms according to the invention. It is only necessary that the active ingredient constitute an effective amount; i.e., such that a suitable effective dosage will be consistent with the dosage form employed. The exact individual dosages as well as daily dosages will, of course, be determined according to standard medical principles under the direction of a physician or veterinarian.
Animal testing suggests that the more active compounds of Formula I such as those cited above in the Vogel test will be effective in humans for relief from anxiety at 3 to 100 mg/kg body weight per day. Thus an active compound such as Example 14 may be administered to control anxiety in unit dosage form to an adult human at 70-1,000 mg once, twice or three times a day.
Animal testing suggests that the more active compounds of Formula I will be effective in humans for muscle relaxant effects at 15 to 100 mg/kg body weight per day. Thus, an active compound such as that of Example 33 may be administered to effectively control muscle spasms in unit dosage form to an adult human at 300-1,000 mg once, twice or three times a day.
The compounds of Formula I have anticonvulsant property as exhibited by activity against seizures caused by electrical or chemical challenge. The animal data suggest the more active compounds of Formula I, such as those cited above under Electroshock Experiments and metrazole chemical challenge are projected to be effective against all types of epilepsy. The animal data suggests the more active compounds of Formula I will be effective in humans at 5-15 mg/kg body weight per day. Thus an active compound such as that of Example 42 may be administered to effectively control all types of epilepsy, both grand mal and petit mal, seizures. For example, oral daily doses of 100-1,000 mg of active agent once, twice or three times a day are projected for treatment of epilepsy.
The active ingredients of the invention may be combined with other pharmacologically active agents as previously indicated, or with buffers, antacids or the like, for administration and the proportion of the active agent in the composition may be varied widely.
Capsules
Capsules of 5 mg, 25 mg, and 50 mg of active ingredient per capsule are prepared; with higher amounts of ingredient reduction may be made in the amount of lactose.
______________________________________Typical Blend for Encapsulation Per Capsule (mg)______________________________________Active Ingredient 5.0Lactose 296.7Starch 129.0Magnesium Stearate 4.3Total 435.0______________________________________
Uniformly blend the selected active ingredient with lactose, starch, and magnesium stearate and encapsulate the blend.
Additional capsule formulations preferably contain a higher dose of active ingredient and are as follows:
______________________________________ 100 mg per 250 mg per 500 mg perIngredients Capsule Capsule Capsule______________________________________Active Ingredient 100.0 250.0 500.0Lactose 231.5 126.5 31.1Starch 99.2 54.2 13.4Magnesium Stearate 4.3 4.3 5.5Total (mg) 435.0 435.0 550.0______________________________________
Uniformly blend the selected active ingredient with Lactose, Starch and Magnesium Stearate and encapsulate the blend.
Tablets
A typical formulation for a tablet containing 5.0 mg to 50.0 mg of active ingredient per tablet follows. The formulation may be used for other strengths of active ingredient by adjustment of weight of dicalcium phosphate and active ingredient.
______________________________________Ingredients Per Tablet (5 mg) Per Tablet (50 mg)______________________________________(1) Active Ingredient 5.0 50.0(2) Corn Starch 13.6 13.6(3) Corn Starch (paste) 3.4 3.4(4) Lactose 79.2 79.2(5) Dicalcium Phosphate 68.0 23.0(6) Calcium Stearate 0.9 0.9Total 170.1 170.1______________________________________
Uniformly blend 1, 2, 4, and 5. Prepare 3 as a 10 percent paste in water. Granulate the blend with the starch paste and pass the wet mass through a number eight mesh screen. The wet granulation is dried and passed through a number twelve mesh screen. The dried granules are blended with calcium stearate and compressed.
Additional table formulations preferably contain a higher dosage of the active ingredient and are as follows:
______________________________________ 100 mg per 250 mg per 500 mg perIngredients Tablet Tablet Tablet______________________________________Active Ingredient 100.0 250.0 500.0Lactose 180.0 150.0 200.0Corn Starch 116.0 100.0 100.0Calcium Stearate 4.0 5.0 8.0Total (mg) 400.0 505.0 808.0______________________________________
Uniformly blend the active ingredient, lactose, and corn starch. The blend is granulated, using water as a granulating medium. The wet granules are passed through an eight mesh screen and dried at 140 to 160 degrees Fahrenheit overnight. The dried granules are passed through a number ten mesh screen and blended with the proper amount of calcium stearate and this blend is then converted into tablets on a suitable tablet press.
Various modifications and equivalents will be apparent to one skilled in the art and may be made in the compounds, methods, processes and pharmaceutical compositions of the present invention without departing from the spirit and scope thereof; and it is therefore to be understood that the invention is to be limited only by the scope of the appended claims. | A novel method of controlling epilepsy, muscle tension, muscular spasticity, and anxiety in living animal bodies by administering compounds of the formula: ##STR1## wherein: R 1 is hydrogen, loweralkyl or a pharmaceutically acceptable cation;
R 2 and R 3 , same or different, are hydrogen, loweralkyl, aryl, cycloalkyl, loweralkenyl, 1-adamantyl, heterocyclicaminoalkyl, diloweralkylaminoloweralkyl, or R 2 with R 3 and adjacent nitrogen may form a heterocyclic ring structure; and the pharmaceutical acceptable acid salts, and tautomeric isomers thereof; and novel pharmaceutical compositions therefor are disclosed. | 2 |
This is a continuation of co-pending application Ser. No. 07/120,022 filed on Nov. 13, 1987, now abandoned.
BACKGROUND
This invention relates generally to the conversion of amorphous or polycrystalline semiconductor materials to substantially single crystal semiconductor material by a process known as zone-melting-recrystallization (ZMR).
The development of silicon-on-insulator (SOI) technology has been complemented by the use of ZMR processing to produce single crystal silicon for solid state devices exhibiting reduced parasitic capacitance, simplified device isolation and design, and radiation hard circuits for space applications.
Present ZMR processes require a well controlled mechanical system to translate a hot zone created by a moving strip heater across the surface of a heated silicon wafer. This system is elaborate, expensive, and has a number of mechanical parts that could degrade in time. U.S. Pat. No. 4,371,421 entitled "Lateral Epitaxial Growth by Seeded Solidification" describes such a system.
A sample to be recrystallized is placed on a heater which raises the temperature of the sample close to its melting point. A strip heater positioned above the sample is then energized to induce melting of a zone on the sample directly beneath the strip heater element. The strip heater is then translated past the surface of the sample, causing the melting zone to move in unison with the heater to induce melting then solidification of the sample to achieve lateral epitaxial growth thereby transforming the sample into a single crystal material.
SUMMARY OF THE INVENTION
The present invention comprises a new heating system that accomplished the same task with no moving parts. A moving heat zone is electrically provided using a heater block fabricated from Alumina, Zirconia, or some other refractory material in such a way as to support a large number of small heating elements. In order to keep these heating elements separated during the process and prevent them from shorting out, they are placed in small grooves machined into the refractory block. Each of these wire elements is supplied with electrical current through a control circuit. With such a circuit, it is possible to provide any combination of heated elements at any desired temperature. When sufficient current is provided to a heating element, it will become hot due to its resistivity. The refractory block is machined in such a way as to provide support of a silicon wafer. The wafer is centered over the hot zone. The heating element lengths could be adjusted so that they do not extend beyond the edges of the wafer. This provides a significant advantage to current ZMR processes by limiting edge heating.
The above, and other features of the invention, including various novel details of construction and combination 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 zone-melt recrystallization method and apparatus embodying the invention is shown by way of illustration only and not as a limitation of the invention. The principal features of this invention may be employed in various embodiments without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the zone melt recrystallization apparatus of the present invention; and
FIG. 2 is a schematic diagram of the control circuit for the apparatus of FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
A preferred embodiment of the invention is illustrated in the perspective view of FIG. 1. In operation, the entire block 10 would be raised to the temperature for ZMR operation just below the melting point of a semiconductor material 11. Then individual elements 13 are heated to a temperature required to melt the semiconductor 11. To create a hot zone 80 mils in width for example requires four heating elements with a 25/1000 inch spacing between each element. These individual heating elements can be provided with enough additional current above their bias current to melt the silicon material. To move the hot zone, the power would be provided to an adjacent heating element, to one side of the four presently being heated, while the element on the opposite side of the four hot elements would be provided only its bias current. In this way, the hot zone would be shifted over by one heating element. This process could be continued at any desired rate to move the zone across the wafer.
In a preferred embodiment, it is possible to provide varying degrees of current to individual wires. This permits gradual heating at the edge of the moving zone.
Through proper control, the heating elements could be heated in a more analog or continuous way in order to produce a much smoother transition as the heating zone is translated.
Through proper design, this heater concept provides a way of significantly reducing the mechanical strains in the ZMR processing system. The moving zone could be made to move more uniformly and more smoothly than any mechanical system and at a significant reduction in overall system complexity and cost. In the configuration of FIG. 1, a silicon wafer 11 is placed top side down on the plate 12 which is in thermal contact with elements 13.
Instead of picking up a wafer with pins as is done in current systems, it would be much more desirable to use a vacuum in this system.
A further advantage is that in order to view the molten zone in the present system, we use a video camera which must be placed at exactly the right angle with respect to the upper heater, which limits the field of view as it permits viewing of only a fraction of the molten zone. With the new system, the camera 14, which is sensitive to infrared light, would view the entire melt zone through the backside of the wafer 11. The infrared image can be used to provide a feedback signal to the control circuit to insure that heating rates are within predetermined tolerance.
FIG. 2 shows a schematic diagram of the control elements of a preferred embodiment of the invention. The resistors R 1 , R 2 , and R 3 represent individual heating elements. There are about 300 of these elements in the present embodiment. Only three are shown for purposes of illustration. A first DC current source I B provides power to bring the heater close to the melting temperature of the wafer. A second DC current source I P supplies power to bring each heater element to the melting temperature of the wafer when commanded by computer. Each element has a pair of transistors, one to connect the positive side of the I P source, and the second to connect the negative terminal of the I P source, to the desired element or elements. This allows both icnreasing and decreasing the current of the selected elements around the I B value.
The computer tells the multiplexer which elements will be effected by the Ip source. The computer also establishes the set points for the controlled elements which in combination with the video cameral provide the control of the pulse width modulator.
Another preferred embodiment utilizes a heater element wherein the elements are portions of a single wire wound about the block such that each portion is controlled by the circuit as shown in FIG. 2.
Yet another embodiment uses carbon or graphite elements deposited on the plate, which may be made from alumina, zirconia, or some other refractory material. These elements can be formed into a sequence of parallel lines, each individually controlled. The elements can also be configured in a dot matrix type configuration. | The improved zone-melt recrystallization apparatus is comprised of a heating element having a plurality of individually controllable heating elements. The elements are heated in sequence to generate a melted zone within a semiconductor material which is translated across the material by heating then cooling adjacent heating elements to recrystallize the material. | 2 |
BACKGROUND OF THE INVENTION
This invention relates to a wind turbine system and more particularly to a composite vertical axis wind turbine system that utilizes a lower wind speed vertical axis wind turbine to start the rotation of a higher wind speed wind turbine.
Wind energy is rapidly emerging as one of the most cost-effective forms of renewable energy with an ever-increasing installed capacity around the world. One of the widely recognized types of turbines used for electricity generation is the well-recognized Horizontal Axis Wind Turbine (HAWT). This type of turbine features a high blade tip velocity ratio, relatively high power generation efficiency, and low start-up torque. The second major group of wind turbines is the Vertical Axis Wind Turbines (VAWT), which possess several inherent advantages over HAWTs: VAWTs do not have to be yaw-adjusted to follow the changing direction of prevailing wind, and consequently handle gusts more efficiently; the power generator can be integrated into the system at ground level, reducing the structural requirements of the support tower, are much quieter in operation, lower in vibration and bird-friendly. However, a major disadvantage of most VAWT configurations is that they require a relatively high start-up torque. An omnidirectional vertical wind turbine electric generator system has been disclosed in U.S. Pat. No. 7,109,599 to Watkins. The contents of this patent are incorporated herein by reference.
Because of typical blade configurations and mechanical stiction in vertical axis wind turbines, it is known that starting a vertical axis wind turbine requires a higher wind speed than is necessary to keep the turbine rotating once it is in motion. Relatively smaller vertical axis wind turbines will start at lower wind speeds such as, for example, 3 miles per hour, whereas larger-sized units would require a higher wind speed (say 8 miles per hour) to start but might continue to rotate, once having been started, at, for example, 5 miles per hour.
It is an object of the present invention to address this major deficiency of VAWT by proposing a double-vertical-axis-turbine system with a torque-amplifying cascade arrangement. This system features a small vertical axis turbine that starts at a relatively lower wind speed which, once up to speed, subsequently starts a relatively higher wind speed vertical axis wind turbine.
SUMMARY OF THE INVENTION
In one aspect, the wind turbine system according to the invention includes a lower wind speed vertical axis turbine operatively connected to a first electrical motor/generator. A higher wind speed vertical axis wind turbine is provided and is operatively connected to at least one second electrical motor/generator. Electrical power from the first electrical motor/generator is directed to at least one second electrical motor/generator to start the higher wind speed turbine. In a preferred embodiment, the lower wind speed vertical axis wind turbine is disposed on top of the higher wind speed vertical axis wind turbine. It is preferred that the higher wind speed vertical axis wind turbine be operatively connected to two second electrical motor/generators.
In another preferred embodiment, the system includes an anemometer to measure wind speed such that the output of the anemometer is operatively connected to the first electrical motor/generator to direct power to the at least one second electrical motor/generator when measured wind speed reaches a selected level. Power electronics are provided to distribute electrical power from the first and second electrical motor/generators.
In one embodiment, the lower wind speed turbine includes five blades and the higher wind speed turbine includes three blades. It is preferred that the lower wind speed turbine be designed to begin rotating at a wind speed of approximately 3 miles per hour. A suitable higher wind speed turbine is designed to “self-start” turning at a wind speed of 8 miles per hour but once started, can run at say 5 miles per hour.
The wind turbine system disclosed herein is designed for mounting on building rooftops although other locations are appropriate. It is preferred that the turbines be selected to provide power in the range of 10 kW to 30 kW. The lower wind speed turbine and the higher wind speed turbine may share a common shaft. The blades of the turbines may be conventional wings with a high performance cambered airfoil configuration, featuring high lift-to-drag ratios. The blades may include regions with different surface textures and treatments.
An auxiliary blade that deploys at an angle to the main blades by use of a passive tail to serve as a wind directing and accelerating scoop blade that can swerve at an angle of say 30° to 40° off the prevailing wind may be provided, as in a sailboat's jib changing the mainsails' apparent wind and increasing the surface area of the overall “sail” area.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective, schematic view of an embodiment of the invention disclosed herein.
FIG. 2 is a perspective view of another embodiment of the invention.
FIG. 3 is a block diagram showing the power electronics arrangement.
FIG. 4 is a schematic illustration (plan view) of an auxiliary accelerator blade according to another embodiment of the invention.
FIGS. 5 a and 5 b are perspective views of turbine blades showing surface treatments including micro vortex generators and dimples to cause the wind to be “stickier” on portions of the blade closer to the center of the hub to equalize and maximize pressure on the blade surface.
DESCRIPTION OF THE PREFERRED EMBODIMENT
As shown schematically in FIG. 1 , the wind turbine system 10 includes a lower wind speed vertical axis wind turbine 12 mounted above a higher wind speed vertical axis wind turbine 14 . An anemometer 18 is mounted on the lower wind speed vertical axis turbine 12 brace system, out of the way of the turbine's exhaust flow.
An embodiment of the invention is shown in greater detail in FIG. 2 . The lower wind speed turbine 12 includes five blades but it should be understood that more or fewer than five blades may be utilized. The lower wind speed turbine 12 is operatively connected to a motor/generator 20 . The turbine 12 sits above a relatively higher wind speed turbine 14 that is operatively connected to a generator 22 . The higher wind speed turbine 14 is also operatively connected to another generator 24 . In this embodiment, the wind turbines 12 and 14 are supported on a brace 26 that also supports the anemometer 18 . As shown in FIG. 3 , the output of the motor/generators 20 , 22 and 24 are delivered to the power electronics (P/E) module 30 and ultimately to a load 32 that may be the electrical grid or an on-site storage system for either local use or as a power reservoir to be either a back-up system or for use at peak demand/peak utility pricing.
The five bladed lower wind speed vertical axis wind turbine 12 is designed to start in light winds of, for example, approximately 3 miles per hour and begin producing usable power at, say 5 MPH, producing 40% of generator's 20 rated capacity. The larger, higher wind speed vertical axis turbine 14 requires a higher start-up torque to operate. For example, the higher wind speed turbine 14 may not start in winds lighter than 8 miles per hour, but once rotating, it can sustain rotation at a lower speed such as 5 miles per hour. Suitable light wind vertical axis wind turbines are available from PacWind, Inc. of Torrance, Calif. See, U.S. Pat. No. 7,109,599 mentioned above.
Therefore under this scenario, when the anemometer 18 detects a 5 mile per hour wind speed, electrical energy from the generator 20 (since the lower wind speed turbine 12 is already rotating) is directed to the motor/generator 22 which subsequently starts the turbine 14 . Once the higher wind speed vertical axis turbine 14 is sustainably rotating, electrical energy from both the generator 20 and the generator 22 is distributed to the load 32 .
An aid to start-up and braking in an “over-speed” condition may be a pair of Neodymium magnets (not shown) mounted on the turbine 14 's input and on generator 24 's output shaft with generator 24 's magnet wrapped with one or more copper coils connected to the P/E circuit 30 . The Neodymium magnets are positioned to lift turbine 14 off generator 24 's bearings a few centimeters to reduce the start-up stiction and bearing wear. In an “over-speed” event, the excess current of generator 24 can be switched through the P/E controls to charge the coils wrapping the magnet on generator 24 thereby reversing the magnet's polarity and acting as an “electric brake” on turbine 14 output shaft until a transient gust has passed, as determined by the anemometer 18 . Anemometer 18 may also “chop” generators 20 and 24 's variable voltage output being sent to the P/E to not exceed acceptable voltage. The same system will be applied on a smaller scale to turbine 12 's blades to control its peak torque output.
In effect, the smaller turbine 12 and its motor/generator 20 act as a starter motor for the larger, higher wind speed turbine 14 , with the added assistance of the Neodymium magnet system. More importantly, an additional generator 24 is also operatively connected to the higher wind speed turbine 14 . In higher winds or during gusts, the power electronics 30 will engage the third generator 24 at the bottom of the larger unit 14 , creating a third level of counteracting torque against which the turbine blades will engage. This arrangement will thereby serve as both another source of electrical production and, in effect, another electronic “brake” on the turbines' shaft and therefore on the blades' rotational speed. In an “over-speed” event, the excess current of generator 24 can be switched through the P/E controls to charge the coils wrapping the magnet on 24 thereby reversing the magnet's polarity. This change of polarity acts as an “electric brake” on blade 14 's output shaft until the transient gust has passed or as a means to lock down the turbine, as determined by anemometer 18 .
There are thus three possible load set points (blades of turbines 12 and 14 are scaled to match to local environmental conditions) created by the sizing and choice of the three generators 20 , 22 and 24 . The three generators effectively create an electronic transmission with three gears sized to: 1) light wind; 2) start up to average geographic wind speed; and 3) maximum wind speed. These three generators 20 , 22 and 24 are all direct drive units sitting on/under the output shaft, eliminating any output loss that would accompany the use of belts, gears and clutches in conventional transmissions.
By using three smaller generators rather than one large generator, the usable power output will start at lower speeds; stay on the power profile of generators found on the market (which have narrow/high rpm power bands for effective conversion to and from mechanical to electrical power); and, be able to produce power in gales and high winds which would cause conventional units either to clip their power output, veer out of the wind, break their unit, or just have to shut down.
The blades on the turbines 12 and 14 may be conventional wings or more advanced high lift-to-drag ratio cambered airfoil blades. The tips and connection points of the blades may receive a shape treatment to assist in energy production and lift generation, and the center shaft may be shaped to allow wind flow to pass with minimal disturbance, as would the support structure, brace 26 , which may be composed of one or more supports.
If the turbine system of the invention were to be used in, for example, Boston, Mass., the smaller turbine 12 would likely kick in at approximately 3 miles per hour and produce enough power/torque to move the larger bladed unit 14 at a wind speed of 5 miles per hour. At this point, the motor/generator 22 will come on-line and will max out at approximately 13 miles per hour, the average regional wind speed, and continue to generate its maximum voltage/output throughout the generator 24 start and run-up to 29 miles per hour or greater. Above this wind speed, both generators 22 and 24 would likely have their output clipped and maintained at a constant level so as not to damage the power electronics. It should be noted that the three generators 20 , 22 and 24 may be coupled mechanically on two shafts, one for the light wind generator and one for the larger turbine, coupled with a clutch between a small output shaft and the larger turbine's shaft, or preferably electrically controlled through the power electronics resulting in a much higher output and broader power band at lower wind speeds than a conventional unit. It is preferred that the units be electrically coupled because a clutch system is both more expensive to manufacture and requires constant monitoring and maintenance and potential failure, leading to catastrophic unit failure.
With reference now to FIG. 4 either one or both of the turbines 12 or 14 may include an auxiliary accelerator blade or airfoil 40 that can swerve into a pre-set angle to the prevailing wind (say 30° to 40° off the wind) by the counter action of an orienting tail 42 .
As shown in FIGS. 5 a and 5 b , blades 50 and 52 or regions/sections thereof, may contain micro vortex generators 54 or dimples 56 to result in greater extraction of energy from the prevailing wind.
It is recognized that modifications and variations of the present invention will be apparent to those of ordinary skill in the art and it is intended that all such modifications and variations be included within the scope of the appended claims. | Wind turbine system. The system includes a lower wind speed vertical axis wind turbine operatively connected to a first electrical motor/generator and a higher wind speed vertical axis wind turbine operatively connected to at least one second electrical motor/generator. Electrical power from the first electrical motor/generator is directed to the at least one second electrical motor/generator and mag-lev system to cause the higher wind speed turbine to begin turning. | 8 |
CROSS-REFERENCE TO PARENT APPLICATION
This application is a continuation application of U.S. patent application Ser. No. 10/117,781 filed on Apr. 4, 2002, now issued as U.S. Pat. No. 7,421,693 which is incorporated by reference herein in its entirety.
CROSS-REFERENCE TO COMPUTER PROGRAM LISTING APPENDIX
Note that a computer program listing Appendix A originally filed in U.S. patent application Ser. No. 10/117,781 (see above) is hereby expressly incorporated by reference herein in its entirety.
Appendix A contains the following two files in IBM-PC format and compatible with MS-Windows which form a part of the present disclosure and this appendix A is incorporated by reference herein in its entirety:
Date
Time
Size
File Name
Mar. 28, 2002
02:31p
365,686
MEMCOP.TXT
Mar. 28, 2002
02:33p
219,262
UCEXEC.TXT
The two files of Appendix A form source code of computer programs and related data of an illustrative embodiment of the present invention, as follows:
UCEXEC.TXT file describes the behavioral model of circuitry in a microcontroller's execution unit to decode and execute an instruction to provide a store-and-load command to a memory co-processor; and
MEMCOP.TXT file describes the behavioral model of circuitry of the memory co-processor, which is also known as a special processing unit (SPU).
COPYRIGHT NOTICE
A portion of the disclosure of this patent document contains material that is subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.
CROSS REFERENCE TO RELATED APPLICATIONS
This application is related to and incorporates by reference herein in their entirety the following U.S. patent application(s):
(U.S. patent application Ser. No. 10/103,436) entitled “Dynamic Allocation of Packets to Tasks,” Nathan Elnathan et al., filed on Mar. 20, 2002, issued as U.S. Pat. No. 7,245,616;
U.S. patent application Ser. No. 10/103,393 entitled “Reordering of Out-of-Order Packets,” Nathan Elnathan, filed on Mar. 20, 2002, issued as U.S. Pat. No. 7,072,342;
U.S. patent application Ser. No. 10/103,415 entitled “Asymmetric Coherency Protection,” Ilan Pardo, filed on Mar. 20, 2002 now issued as U.S. Pat. No. 7,424,496;
U.S. patent application Ser. No. 10/117,394 entitled “Method and Apparatus to Suspend and Resume on Next Instruction for a Microcontroller,” Alexander Joffe, filed on Apr. 4, 2002, issued as U.S. Pat. No. 7,155,718;
U.S. patent application Ser. No. 10/117,452 entitled “Method And Apparatus For Issuing A Command To Store An Instruction And Load Resultant Data In A Microcontroller,” Alexander Joffe et al., filed on Apr. 4, 2002 now abandoned (see its divisional U.S. Pat. No. 7,437,535);
U.S. patent application Ser. No. 10/117,779 entitled “Memory Co-Processor for a Multi-Tasking System,” Alexander Joffe et al., filed on Apr. 4, 2002, issued as U.S. Pat. No. 6,938,132; and
U.S. patent application Ser. No. 10/117,780 entitled “Sequencing Semaphore,” Alexander Joffe et al., filed on Apr. 4, 2002, issued as U.S. Pat. No. 6,978,330.
BACKGROUND OF THE INVENTION
A number of tasks executing in a microcontroller 20 (see FIGS. 1A and 1B ) may take different paths (also called “code paths”) even if such tasks execute the same software program (also called “code”) 10 . For example, Task 0 may make a jump in executing code 10 after performing a first policing function at a location S 0 , thereby to define a first code path 11 . Once Task 0 makes the jump, Task 0 does not need to perform the remaining policing functions S 1 and S 2 that are otherwise required during in-line (i.e. no jump) execution of software program 10 .
In the example of FIG. 1A , another task, namely Task 1 does not jump immediately after location S 0 in software program 10 , and instead continues with in-line execution (e.g. executes a number of instructions immediately following location S 0 ). However, Task 1 may eventually make a jump after performing a second policing function at a location S 1 in the software program 10 , thereby to define code path 12 . In a similar manner, Task 2 may simply execute software program 10 without making any jumps immediately after locations S 0 and S 1 , thereby to define code path 13 .
In the example being discussed, at various locations in the respective code paths, a decision to make a jump depends on the value of data that is shared among such tasks, Task 0 -Task 2 . For example, in a networking application, the policing functions performed at locations S 0 and S 1 may require that a packet that is being processed be dropped, for example if the rate exceeds a predefined bandwidth allocated to a channel to which the packet belongs.
Therefore, it is important for such tasks, Task 0 -Task 2 to ensure that the data being used in the policing functions is accurate and updated properly. Access to such data may be arbitrated by use of a semaphore as a synchronization mechanism, to access a common location in memory, to ensure that data at that common location is not changed by one task while that data is being used by another task. Use of such a semaphore ensures, for example, that a packet counter is properly incremented (or a database entry is properly accessed) by each of a number of tasks that execute concurrently or simultaneously in the microcontroller.
In using a semaphore, when one task, e.g. Task 0 in FIG. 1B , is accessing a memory location at a location S 0 in the code, other tasks, e.g. Task 1 , Task 2 , and Task 3 , that also need to access that same memory location are suspended (i.e. are made to wait). While such other tasks are waiting, Task 0 may be activated from sleep, may issue a read request on being awakened, may again be put to sleep while waiting for a response from memory, may again be awakened on receiving the memory response, perform a read operation, and finally release the semaphore. Only at this point is the semaphore for code location S 0 available for use by the next task, Task 1 .
Therefore, use of a semaphore effectively single threads the access to a common memory location in all of the tasks, even though a microcontroller (such as a network processor) may support multitasking. Such single threading causes the latency of each task to affect all subsequently-performed tasks.
U.S. Pat. No. 5,790,881 granted to Nguyen on Aug. 4, 1998 entitled “Computer system including coprocessor devices simulating memory interfaces” suggests (see abstract) “coupling a coprocessor to a master device, in which the coprocessor emulates an memory interface to the master device, like that of a memory device . . . . The coprocessor is disposed to receive data written from the master device, perform a coprocessing function on that data, and respond to a read data command from the master device with processing results.”
See also U.S. Pat. No. 6,338,108 granted to Motomura on Jan. 8, 2002 entitled “Coprocessor-integrated packet-type memory LSI, packet-type memory/coprocessor bus, and control method thereof” which states (see abstract) that “[a] memory section and coprocessor sections in a coprocessor-integrated packet-type DRAM are provided with unique memory device ID and coprocessor device IDs respectively . . . ”
SUMMARY
The present invention relates to logic (also called “synchronizing logic”) that receives a signal (called a “declaration”) from each of a number of tasks, based on an initial determination of one or more paths (also called “code paths”) in an instruction stream (e.g. originating from a high-level software program or from low-level microcode) that a task is likely to follow. An initial determination by a task may be based on any information available prior to generation of the initial signal, including, for example, information in a header (of a packet or a cell) in the case of a networking application (wherein each task processes a packet/cell).
In some embodiments, each of the declarations identifies, for each of a number of predefined locations in a software program (e.g. one or more of locations S 0 -S 2 in FIGS. 1A and 1B ), whether or not that task expects to access data (also called “shared data”) that is also to be accessed by other tasks (e.g. on executing the same instructions in the instruction stream).
A task that indicates in the declaration a likely future need to access a shared data may decide at a later time that access to that shared data is no longer needed, and may indicate this to the synchronizing logic (via another declaration). However, in some embodiments, the opposite is not permitted, i.e. a task that has previously declared no need to access a shared data cannot change its no-need decision (e.g. due to changed circumstances), to declare that it now needs to access that shared data.
Once a task (also called “no-need” task) declares its lack of a future need to access a shared data (regardless of whether this happens in a first synchronization request or in a subsequent synchronization request), the synchronizing logic allows that shared data to be accessed by other tasks (also called “needy” tasks) that have indicated their need to access the same. Moreover, the synchronizing logic also allows the shared data to be accessed by the other needy tasks on completion of access of the shared data by a current task (assuming the current task was also a needy task).
In some embodiments, commands (such as a “store and load” command) to access the shared data from needy tasks are handled in order (so that allowing a no-need task to change its decision may result in out-of-order processing of access requests, which defeats the premise of in-order processing). In several such embodiments, each task is assigned a sequence number depending on the order in which the data being processed therein (e.g. a packet or a cell) is received, relative to the other tasks. Therefore, the synchronizing logic grants access to the shared data, based on the sequence number (and for this reason such a synchronizing logic is hereinafter called a “synchronizing sequencer”).
Such a synchronizing logic may be implemented in either hardware or in a microprocessor programmed with software in different embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B illustrate code paths of tasks in the prior art, wherein the tasks need to synchronize their access to shared data at various synchronization points.
FIG. 2A illustrates each task issuing a “declaration” signal in accordance with the invention, to a synchronizing logic, followed by issuance of instructions to change shared data.
FIG. 2B illustrates a table of states maintained in accordance with the invention for use in providing access to shared data.
FIG. 3A illustrates, in a block diagram, use of a memory co-processor to interface a microcontroller to external memory, in accordance with the invention.
FIG. 3B illustrates, in a flow chart, acts performed by a task in a microcontroller for accessing shared data in one embodiment.
FIG. 3C illustrates, in a timing chart, a sequence of events when a task accesses shared data at a specific location in one embodiment.
FIG. 4A illustrates, in a state diagram, transitions between various states of each task in accessing shared data in one embodiment.
FIGS. 4B and 4C illustrate, in flow charts, acts performed by a synchronizing sequencer of one embodiment.
FIGS. 5A-5L illustrate exemplary transitions that occur in a synchronization request array of the type illustrated in FIG. 2B .
FIG. 6A illustrates, in a block diagram, circuitry for a single synchronization point used to identify a sequence number of an instruction to be executed in one embodiment.
FIG. 6B illustrates, in a block diagram, replication of the circuitry of FIG. 6A to implement a number of synchronization points in accordance with the invention.
FIG. 6C illustrates, in a high-level block diagram, a memory co-processor of one embodiment, in which a sequencer of the type illustrated in FIGS. 6A and 6B is implemented.
DETAILED DESCRIPTION
In accordance with the invention, on startup or a short time thereafter prior to accessing any shared data, a number of tasks Task 0 -TaskM (wherein 0≦J≦M, M being the total number of tasks) issue signals (called “declarations”) to a logic (called “synchronizing logic”) as illustrated in FIG. 2A , to identify whether or not the tasks expect to access shared resources at certain predefined synchronization points SA-SN (wherein A≦I≦N, N being the total number of synchronization points) in their instruction streams. If access to a shared resource is expected at a synchronization point SA, then this synchronization point SA is indicated as having a state “enabled” and otherwise indicated as having the state “disabled.”
The synchronizing logic receives such state signals from each task “TaskJ”, for each synchronization point SI, and stores the state locally in a buffer (e.g. in a two-dimensional table as illustrated in FIG. 2B ). The synchronizing logic uses the states in deciding whether or not to allow an instruction from a task to access the shared data. When an instruction affecting a shared resource is received from a task for any specific synchronization point SI, the synchronizing logic changes a state associated with the task from “enabled” to “pending.”
If a task's state is “pending” and if it is now this task's turn, then the synchronizing logic issues any instructions from this task (such as a read-modify-write instruction) to the execution unit. Specifically, the synchronizing logic maintains a current pointer for each synchronization point SI, and this current pointer indicates which task's instruction (for accessing shared data) is to be now executed.
If the current pointer points to a task that has not yet provided an instruction and if the task is “enabled” then any instructions from other tasks that are received are made to wait until the current task's instruction is received and executed. If a task does not expect to issue such an instruction (and the state is “disabled”), then the current pointer is incremented to identify the next task that is current for this synchronization point SI.
Therefore, if a number of tasks do not expect to access a particular resource, then these tasks are assigned the state “disabled”. In providing access to that particular resource, all disabled tasks are skipped over, thereby to speed up the arbitration. The tasks just described as being “disabled” may expect to access one or more other shared resources, and indicate this need in their respective declarations.
If an instruction is received from a task “TaskJ” for a specific synchronization point SI, and if the current pointer for this synchronization point SI is pointing to TaskJ, then that instruction is immediately executed.
Moreover, in some embodiments, the current pointer is incremented (or increased) to point to the next task from which an instruction is to be executed.
In certain embodiments, the increment (or increase) is unconditional (i.e. automatic), and alternatively in other embodiments the increment (or increase) depends on a specific signal from the task. The just-described signal (also called “lock current pointer” signal) may be activated by a task, to allow any number of instructions from the task to be executed for the current synchronization point SJ, prior to execution of an instruction from another task.
Use of such “lock current pointer” signal (and a version of this signal is called “update sequence number” signal) implements a critical section of any length while the signal is active, thereby causing the synchronizing logic to act as a semaphore of the type described in detail in a related U.S. patent application Ser. No. 10/117,780 that has been incorporated by reference above.
Increment of the current pointer described above may be optimized in some embodiments to be sufficiently large to skip over all tasks that do not expect to provide any instructions for accessing or changing the shared data for this synchronization point SI. In several embodiments, operation of a current pointer and allocation of a shared resource at one synchronization point SI is independent of the corresponding operation and allocation at another synchronization point SJ. Therefore, there may be no sequence relation between, for example, two policing operations (which may be used to control the flow of packets in a network, for example). For this reason the two policing operations may be identified as two synchronization points SI and SJ.
In one specific embodiment, the synchronizing logic selectively provides access to a number of shared data (e.g. eight shared data) among multiple tasks that execute in a microcontroller 301 ( FIG. 3A ), such as a network processor. Microcontroller 301 is coupled to and controls the operation of one or more channel processors that process packets and/or cells, as described in, for example, U.S. Pat. No. 6,330,584 granted to Joffe that is incorporated by reference herein in its entirety. Each of the channel processors assigns a sequence number to each packet according to their order of arrival, and the sequence number along with a pointer to the packet is supplied to microcontroller 301 .
The sequence number that is assigned to each packet may be any monotonically changing number (e.g. a number that is incremented or decremented by 1 for each packet arrival), and depending on the embodiment the sequence number is unique globally across all channel processors or alternatively the sequence number is unique only within a channel processor (or only in one direction of one channel processor).
On receipt of a packet pointer and its associated sequence number, microcontroller 301 assigns the packet to a task executing therein (an assignment may be performed by, for example, a request unit). The task generates a declaration followed by one or more instructions to the co-processor, to change shared data in memory. The just-described signals generated by a task are handled by a synchronizing logic which is hereinafter referred to as a synchronizing sequencer, by virtue of its use of sequence numbers in deciding the order of access.
A synchronizing sequencer of the type described herein can be implemented off-chip, i.e. outside of microcontroller 301 in which various tasks are executing. In one such embodiment illustrated in FIG. 3A , a synchronizing sequencer 305 B is implemented in hardware in a separate co-processor 305 that is used in one embodiment to access external memory (as described in, for example, U.S. patent application Ser. No. 10/117,779 concurrently filed herewith and incorporated by reference above).
Memory co-processor 305 includes, in addition to synchronizing sequencer 305 B, a number of buffers 305 A in which are stored tables 305 A (of the type described above; also called “synchronization request arrays”). There is one table among tables 305 A for each synchronization point S 0 -SN. As noted above, multiple tables 305 A identify the state of access of shared data by various tasks (which in this example are identified by sequence numbers, because each task is assigned to a sequence number and works on a packet of that sequence number).
Each table 305 A holds the state of a group of (e.g. all) sequence numbers that identify which one of the tasks currently needs to supply a command to memory co-processor 305 . When a task has either indicated no need to access the shared data or the task's instruction (such as a read-modify-write instruction) to change the shared data has been executed, the sequence number is incremented (assuming the “update sequence number” signal is enabled with the read-modify-write instruction), after setting the synchronization point's state for the current sequence number (prior to incrementing) to “invalid”.
Soon after startup, each task compares one or more items of information in its packet header to predetermined values, thereby to classify the packet (see act 311 in FIG. 3B ). Next, the task identifies (see act 312 ) synchronization points at which processing of the packet is likely to access data shared with other tasks, e.g. at points S 0 , S 1 and S 2 illustrated in FIGS. 1A and 1B . For any given software program, synchronization points are known ahead of time, based on packet type.
Next, the task issues (see act 313 in FIG. 3B ) a “declare” command to a synchronizing sequencer. In some embodiments, each “declare” command identifies, in addition to predefined synchronization points, an identifier of the task that processes the packet (as per FIG. 3C ; also see bus 302 in FIG. 3A ).
After issuing a declare command, each task simply continues, e.g. executes software to process the packet (see act 314 in FIG. 3B ), until a synchronization point is reached. When a synchronization point is reached, each task-goes to act 315 ( FIG. 3B ) to check if it is necessary to modify the shared data in memory. Under normal circumstances, this is true, and therefore the task goes to act 316 to issue an instruction to change the data (e.g. increment a packet counter). Alternatively, the task may go to act 317 (from act 315 ), e.g. if on performance of a policing function it is decided to drop the packet being processed. If so, the task indicates its change in expectation, about not needing to use shared data at one or more synchronization points that were previously marked “enabled”.
A synchronizing sequencer receives each instruction issued by each task, and uses a buffer (of the type described above in reference to FIG. 2B ) to determine the action to be taken. For example, synchronizing sequencer temporarily stores each instruction in a buffer (also referred to as an “out of sequence” buffer), unless the following two conditions are met: (1) the task is currently enabled to access the shared data for this synchronization point and (2) it is now the current task's turn (as noted above in reference to FIG. 2B ) to access the shared data.
In one example, the signals exchanged between a microcontroller-based task and coprocessor-based synchronizing sequencer are illustrated in FIG. 3C . Specifically, in this example, a task first assembles and issues a declare command for each of a number of synchronization points that it expects to encounter when processing the just-received packet. Thereafter, the task assembles and issues a command to change shared data at a first synchronization point SA.
The issued command may be, for example, a “store-and-load” command (of the type discussed in the related U.S. patent application Ser. No. 10/980,141 incorporated by reference above), and if so, the memory co-processor returns a result to the microcontroller, indicating, for example, the task that issued the command and optionally a register in which the result is to be stored. Any number of such store-and-load commands or alternatively store commands may be issued by the task, based on synchronization points SA-SN identified in the declaration.
On receipt of a declare command identifying a particular synchronization point S 1 as being “enabled”, the synchronizing sequencer changes a value in the above-described table from “invalid” (which is a default value) to “enabled”, as illustrated by branch 401 ( FIG. 4A ). Thereafter, when the synchronizing sequencer receives a store-and-load (or store) command, the synchronizing sequencer changes an “enabled” value in the table to “pending” (as illustrated by branch 402 ). When a task's command has been executed, the synchronizing sequencer changes a “pending” value in the table to “invalid” (as illustrated by branch 403 ).
When a task indicates its change in expectation, about not needing to use shared data at one or more synchronization points that were previously at the state “enabled”, the synchronizing sequencer changes an “enabled” state in the table to “disabled” (as illustrated by branch 404 ). Branch 404 is only a unidirectional branch, meaning that a state “disabled” is not to be changed to “enabled”. A task may also indicate at the inception that it does not expect to participate in changing data at a specific synchronization point, and in this case, the synchronizing sequencer changes an “invalid” state in the table to “disabled” (as illustrated by branch 405 ).
The synchronizing sequencer changes a “disabled” state in the table to “invalid” (as illustrated by branch 406 ) when incrementing a current pointer (beyond the sequence number for the current task). The synchronizing sequencer never changes an “enabled” state in the table to “invalid”.
In one embodiment, the synchronizing sequencer is implemented by a number of processes that execute in parallel with one another. Specifically, one process 410 (illustrated in FIG. 4B ) receives and handles all commands from the various tasks, while other processes 420 (illustrated in FIG. 4C ) issue to an execution unit, instructions received from these tasks if so indicated by the state of each task. Therefore, in this embodiment, a single process 410 ( FIG. 4B ) handles all commands, for all synchronization points (i.e. for all request arrays).
Initially, process 410 simply waits for a command (as per act 411 ), and on receipt of a command from a task in a microcontroller, goes to act 412 to check if the command was a “declare” command. If so, process 410 goes to act 413 to copy enable/disable states for this task from the command into all request arrays (for all synchronization points), and thereafter returns to act 411 .
If in act 412 the command received is not a declare command, then the command contains an instruction for changing the shared data (such as a store-and-load instruction or a store instruction). If so, process 410 goes to act 414 and changes a state value of a location in the request array corresponding to the task that generated the command (e.g. for a specific sequence number), for the current synchronization point from “enable” to “pending”, and thereafter returns to act 411 .
As noted above, a number of processes 420 ( FIG. 4C ) execute in the synchronizing sequencer, one for each request array. Specifically, the sequencer retrieves in act 421 the state of a location (in the request array) that is identified by the current pointer. If the retrieved state is “invalid” (see act 422 ), then the sequencer simply returns to act 421 (after the current clock cycle has completed). If the state is not “enabled” (see act 424 ), the sequencer simply resets the state to “invalid” (see act 425 ), and then increments the current pointer (see act 426 ), and returns to act 421 .
If the state is “enabled” then the sequencer waits for the state to change (see act 427 ), and this may take several clock cycles, depending on the code path of a task (associated with the current location in the request array). When the state changes, the sequencer checks (in act 428 ) if the state is “pending” and if not, goes to act 425 (discussed above). If the state is “pending” then the sequencer supplies the instruction to the execution unit (see act 429 ), thereby to allow access to shared data.
FIG. 5A illustrates two arrays: (1) a two-dimensional array 501 (which is 4×4 in size in this example) that functions as a synchronization request array for a specific synchronization point (e.g. the first synchronization point S 0 ) and (2) a one-dimensional array 502 (which is 1×4 in size in this example) that is used to navigate to the next location in array 501 , as discussed below.
In FIG. 5A , array 501 has a row pointer Rptr pointing to the bottom-most row and a column pointer Cprt pointing to the left-most column, so that the two pointers together point to a first location in array 501 , in column 0, row 0, which is labeled as “00”. For example, based on certain number of high order bits of the sequence number, an entire row may be read in hardware, and the remaining low order bits of the sequence number are used to select one value from the row.
In one example illustrated in FIGS. 5A-5L , all possible sequence number values are mapped to one of the locations in array 501 . For example, the sequence numbers may be mapped sequentially from left to right in the bottom row, followed by left to right in the row adjacent to the bottom row and so on (with the top right corner location of array 501 representing the largest possible sequence number).
In one example, a task that processes a packet with sequence number 0 does not expect to change the data (at the first synchronization point S 0 ), and for this reason the “00” location in array 501 is initially set to value “0” which indicates “disabled” state (e.g. as a result of a “declare” command). The synchronizing sequencer resets the value in the first location “00” of array 501 to the value “x” which indicates “invalid” state, and moves the column pointer to point to the next column on the right (see FIG. 5B ). Note that the row pointer remains the same until the column pointer reaches the right-most location of array 501 .
The synchronizing sequencer notes that the second location “01” of array 501 is currently set to value “x” and therefore, a declare command has not yet been received (see FIG. 5C ) from a task with sequence number 1, for the first synchronization point S 0 . At some time, a declare command from a task with sequence number 2 is received, and the value “1” received therefrom is loaded into array 501 , in the location “02”. Next, a declare command from a task with sequence number 5 is received (for the first synchronization point S 0 ), and the value “1” received therefrom is loaded into array 501 , in the location “11”. Then, at a later time, a declare command from a task with sequence number 1 is received (for the first synchronization point S 0 ), and the value “1” received therefrom is loaded into array 501 , in the location “01”, as shown in FIG. 5D .
Next, a “store-and-load” command is received for the first synchronization point S 0 , from a task with sequence number 2. So the synchronizing sequencer loads the value “2” into array 501 (see FIG. 5E ), in the third location “02”. Since it is not yet the turn of sequence number 2 (because the current pointer is still pointing to the second location “01” of array 501 ), the synchronizing sequencer simply places the received command in a buffer (called “out-of-sequence” buffer).
An out-of-sequence buffer which is used may be, for example, dedicated to holding instructions only for the first synchronization point S 0 (so that there are multiple such buffers, one for each synchronization point), although a larger buffer to hold instructions for all synchronization points, may be used in other embodiments.
In view of this disclosure, the to-be-executed instructions being held in out-of-sequence buffers may be handled in a manner similar or identical to the prior art handling of “flows” of packets, with one flow for each synchronization point. Hence, each flow will have a task (and sequence number) that is identified by a current pointer.
Thereafter, at some point, a task with sequence number 1 issues a “store-and-load” command for the first synchronization point S 0 . The synchronization point for which a command has been issued is identified in the command, e.g. as the value of an operation number OPN (e.g. one of OP 0 -OP 7 as per FIG. 6B ). As a result of receiving a store-and-load command, the synchronizing sequencer loads the value “2” into array 501 (see FIG. 5F ), in the second location “01”.
Since the current pointer is also pointing to the second location “01”, it is now the turn of the task with sequence number 1. Therefore, the synchronizing sequencer immediately passes an instruction in the just-received command for execution by an execution unit in the memory co-processor. For details on the memory co-processor, see the related U.S. patent application Ser. No. 10/117,779 concurrently filed herewith and incorporated by reference above.
After supplying the instruction to the execution unit, the synchronizing sequencer resets the value in the second location “01” of array 501 (see FIG. 5F ) to the value “x” which indicates “invalid” state, and moves the column pointer to point to the next column on the right (see FIG. 5G ), while the row pointer remains stationary.
At this point, the current pointer is pointing to a location “02” of array 501 , with value “2” which means an instruction is pending (e.g. in the out-of-sequence buffer). The synchronizing sequencer sends this instruction for execution, and changes the value to “x” to indicate that this sequence number has been now processed for the first synchronization point S 0 .
At this point ( FIG. 5H ), the synchronizing sequencer notes that the next location has value “0” (meaning “disabled”), and changes this to value “x”. Then synchronizing sequencer moves the current pointer up to the next row, to location “10” (which represents sequence no. 4). Since the values for location “10” is “0” (meaning “disabled”), the synchronizing sequencer changes this to value “x” and moves the pointer by one location to the right (not shown).
The location “11” (which represents sequence no. 5) has a value “2” which means an instruction is pending (e.g. in the out-of-sequence buffer), and the synchronizing sequencer supplies this instruction to the execution unit, changes this location to value “x” and moves the pointer by one location to the right (see FIG. 5I ).
At this stage, the pointer is pointing to the location “12”, which has a value “2” indicating that an instruction is pending (e.g. in the out-of-sequence buffer). Again, the synchronizing sequencer supplies this instruction to the execution unit, changes this location to value “x” and moves the pointer by one location to the right (not shown). The location “13” has value “0” thereby to indicate this sequence number is “disabled” and therefore the value is changed to “x” and the pointer is moved up the next row (see FIG. 5J ).
In a similar manner, the upper-most row is eventually reached as illustrated in FIG. 5K , and the first two locations “30” and “31” are skipped because of the value “0” indicating that these sequence numbers are “disabled” and these values are changed to “x”. The pointer now points to the location “32” which has a “pending” instruction which is thereafter executed, thereby to yield the array illustrated in FIG. 5L .
In the above-described manner, whenever the synchronizing sequencer receives a command from a task, it identifies and updates an appropriate array 501 associated with the specified synchronization point and sequence number. The synchronizing sequencer also (independently in one embodiment) evaluates the value at a location identified by the current pointer, and moves the current pointer if appropriate.
Some embodiments sequentially increment a row pointer until the right-most location of array 501 is reached.
However, in other embodiments combinational logic is used to determine the next state to be processed, hence skipping a number of disabled states. Also, in some embodiments, another array 502 (also called “navigation array”) is used to identify the next row that has a location to be evaluated (e.g. all intermediate rows in which all locations are disabled are skipped).
Specifically, in one embodiment, an entire row of array 501 is read simultaneously (in hardware). Values in the row are simultaneously evaluated by combinational logic, and as a result of evaluation, the row may be updated (e.g. by changing the state to “invalid”) if execution is to proceed to another row. Also as a result of evaluation navigation array 502 may be updated.
The evaluation result can have one of the following three values: value 0 if all locations in a row are “disabled” (in which case this row in array 501 will be completely skipped by the synchronizing sequencer when issuing instructions to the execution unit), value 1 if at least one location in the row is “pending” (in which case the synchronizing sequencer will read the row and possibly issue an instruction; issuance of an instruction can happen under the following two conditions (1) if no intermediate sequence number is “enabled” i.e. waiting to become “pending” or “invalid” and (2) if no intermediate sequence number is “invalid” i.e. waiting for state to become “enabled” or “disabled”), and value x if all locations in a row are not disabled and there is no instruction pending (in which case the synchronizing sequencer may not even read the row).
Therefore, in a single clock cycle, the synchronizing sequencer skips one or more rows that do not have relevant values. The synchronizing sequencer also avoids processing a row that doesn't have any pending instruction.
The number of locations in a row of array 501 is limited only by the number of values that can be evaluated in a single clock cycle, e.g. evaluating 32 values needs more time than evaluating 16 values (e.g. 8 nanoseconds may be required for 16 values to be evaluated). In one specific implementation, array 501 is 16×16 in size, with 2 bits of value per location.
FIG. 6A illustrates, in a block diagram, circuitry (also called “synchronizer element”) for a single synchronization point used to extract a sequence number indicative of a pending instruction to be executed, from a request array 501 , using a navigation array 502 (both arrays are illustrated in FIGS. 5A-5L ). The synchronizer element of FIG. 6A also includes combinational circuitry 503 to implement state transitions, as described above in reference to, for example, FIG. 4A . The synchronizer element of FIG. 6A also includes circuitry 504 to perform the process described above in reference to, for example, FIG. 4C . Also illustrated in FIG. 6A are various combinational logic elements and storage elements to perform various acts of the type described in general herein and in detail in the attached Appendix A (filed electronically, but incorporated by reference herein in its entirety).
In one embodiment (see FIG. 6A ), the sequencer maintains a table with a 2 bits of state per sequence number. These 2 bits indicate if the entry has a valid pending request to be issued to the execution unit or has an entry which could be skipped. The arrangement of this table is not in an array of 256*2 bits but in an array of 16 entries*16 consecutive states thus covering the 256 sequence numbers.
FIG. 6B illustrates, in a block diagram, replication of the synchronizer element of FIG. 6A in blocks op 0 -op 7 , to implement a number of synchronization points, and using arbitration (e.g. round-robin) to select one of the sequence numbers across all blocks, and use of that sequence number to pass to a decoder an instruction to be executed. In the implementation illustrated in FIG. 6B , all parameters for an instruction are stored in a parameters table that is indexed by a task number. The task number is supplied from a task number table that in turn is indexed by a sequence number. As noted above, each synchronizer element of FIG. 6A provides a sequence number, and one of these numbers is selected by arbitration. Although there may be a large number of values for a sequence number, the number of tasks is limited, and for this reason one level of indirection saves storage space in the parameters table (which holds, e.g. 32 entries, one entry for each task number).
FIG. 6C illustrates, in a high-level block diagram, a memory co-processor in which a sequencer of the type illustrated in FIGS. 6A and 6B is implemented. A memory co-processor illustrated in FIG. 6C also contains an input control block 601 that directs commands received on a bus 602 either to a sequencer 603 or to a command FIFO 604 that holds various instructions (along with a memory address and a task identifier) for decoding by decode unit 606 and execution by execution unit 608 .
Such a decision is made based on the type of command received, e.g. if the command type is not “SPU” (which is an name for the memory co-processor of one embodiment), then the command is written directly to the FIFO. If the command type is “SPU” and if the “enable sequencing” signal (which is in a field in the command that has been received) is inactive then the command is written directly to the FIFO. In all other cases, the command is passed to the sequencer. As noted elsewhere herein, the sequencer buffers commands that are received out of sequence, and after the next command (based on a previously processed command's sequence number) is received, then as many commands as can be issued in sequence are issued to the command FIFO.
FIG. 6C also contains a decode unit 606 that decodes each instruction in the FIFO, and passes the decoded instruction and parameters to the execution unit 608 . The execution unit in turn executes the instruction, e.g. performs a read-modify-write operation to read data from memory, change the data based on the specified modify function (such as policing) and writes the data back to memory.
Note that in some embodiments, there is one sequencer for eight ingress ports and another sequencer for eight egress ports. Moreover, in some embodiments, a cross-connect (called “XMAU”) connects an execution unit of a microcontroller to a sequencer in a memory co-processor.
In one particular embodiment, there are two command FIFOs in the memory co-processor, for holding (1) commands transferred directly to the execution unit (e.g. simple load, store and crc store commands), and (2) commands that go through the sequencer first (so that the sequencer reorders these commands according to their sequence number).
In such an embodiment, a memory co-processor distinguishes between the two types of commands, because the commands that go through the sequencer usually need to use the alu stage of the execution unit pipe, and the alu stage is not available every cycle. The simple load and store commands can be inserted then, in order to avoid loss of cycles due to stalls.
The memory co-processor of one embodiment implements the Virtual Scheduling Algorithm of the ITU I.371 to perform policing of ATM cells. The memory co-processor uses an extention to this algorithm for variable length frames. Furthermore, in some embodiments, for ATM cells the memory co-processor performs the Virtual Scheduling Algorithm GCRA(I, L). For variable size frames the memory co-processor performs extended GCRA(I, L, S) algorithm (S stands for frame size in pre-defined units, e.g., 64 bytes). The memory co-processor returns a single bit to indicate conforming/non-conforming.
Numerous modifications and adaptations of the embodiments, examples, and implementations described herein will be apparent to the skilled artisan in view of the disclosure.
For example, under certain circumstances, no-need tasks may be allowed to change their decision, e.g. if a needy task that is to be granted access has not yet issued an access request. Moreover, instead of granting access to the shared data to tasks as per sequence number, a synchronizing logic of the type described herein may grant access in any order among the tasks, depending on the embodiment. For example, such a synchronizing logic may operate in a first-in-first-out manner by granting access first to a task that sends in its synchronization request first. Alternatively, the synchronizing logic may grant access to the shared data based on a priority associated with each task, or simply in a round-robin fashion.
Numerous such modifications and adaptations of the embodiments described herein are encompassed by the attached claims. | Logic (also called “synchronizing logic”) in a co-processor (that provides an interface to memory) receives a signal (called a “declaration”) from each of a number of tasks, based on an initial determination of one or more paths (also called “code paths”) in an instruction stream (e.g. originating from a high-level software program or from low-level microcode) that a task is likely to follow. Once a task (also called “disabled” task) declares its lack of a future need to access a shared data, the synchronizing logic allows that shared data to be accessed by other tasks (also called “needy” tasks) that have indicated their need to access the same. Moreover, the synchronizing logic also allows the shared data to be accessed by the other needy tasks on completion of access of the shared data by a current task (assuming the current task was also a needy task). | 6 |
TECHNICAL FIELD
The invention relates to methods and devices for reducing erosion in the bores of gun barrels caused by hot propellent gases generated by the ammunition, and more particularly to a method and apparatus for providing a thin protective film by injecting a liquid into the bore of the gun barrel.
BACKGROUND OF THE INVENTION
While the exact mechanisms for bore erosion may still be debatable, it is well established that the higher the surface temperature of the bore during firing of the ammunition, the more severe is the erosion. Several factors are believed to contribute to bore erosion. These include removal of material from the surface of the bore due to mechanical action, either by the projectile passing through the barrel or by the high velocity of the hot gases driving the projectile. Various thermal and chemical effects aid these processes. Also, the hot propellent gases may overheat the barrel, thereby subjecting it to increased frictional wear. In extreme cases, the barrel material may soften to where there is permanent deformation or warping. Barrel life is greatly reduced under such conditions. It is therefore apparent that significantly reducing barrel heating and bore erosion would significantly improve the service life of guns, particularly those of large caliber and/or high muzzle velocity.
With ever increasing demands for higher muzzle velocities and rates of fire, barrel erosion and barrel overheating have become significant problems in modern guns of various types. Higher muzzle velocities are obtained by increasing the operating pressures of the propellant gases and by the use of propellants with higher flame temperatures. The penalties associated with such improvements are increased barrel wall temperature and the attendant effects of increased erosion and bulk barrel temperature, all of which shorten the barrel service life and limit the rate of fire. Four different approaches have been tried in the past to find a solution that will effectively reduce barrel heating and erosion while maintaining desired muzzle velocities and rates of fire.
In the first approach, the bore of the barrel has been plated with chrome or some other hard refractory metal. However, such plating has a limited lifetime because it develops microcracks that cause peeling of the plated coating. A second approach involves the use of additive wear liners such as dimethylsilicone, talc-wax, or titanium dioxide-wax. These additives coat the surface of the bore and thereby reduce heat transfer and chemical attack on the bore wall.
The third approach for erosion and wear reduction is believed to be the most effective conventional way to decrease heat transfer to the barrel wall. This approach involves the use of additives mixed with the propellent to lower the flame temperature significantly, while imparting only a modest penalty to propellant performance. These additives are mostly binders that are less energetic than the main propellent material and generate low molecular weight combustion products. Examples of such additives are shown in FIG. 5 of the drawings. Another such additive is oxynitrotriazole as described in U.S. Pat. No. 5,034,072.
The fourth approach, the practicality of which may not have been demonstrated, involves providing a liquid cooling medium from the projectile itself. In this approach, a liquid filled capsule at the rear of the projectile ejects liquid onto the surface of the barrel bore as the projectile is propelled down the barrel and as the capsule is squeezed by the pressure of the propellant. An example of this approach is described in U.S. Pat. No. 4,203,364, entitled "Cartridge for Reducing Bore Erosion and Extending Barrel Life".
SUMMARY OF THE INVENTION
The invention provides a method and apparatus for significantly reducing gun barrel erosion and bulk barrel temperature in solid propellant guns by the injection of a liquid coolant onto the entrance surfaces of the barrel bore. Although the coolant may be injected via a plurality of passages extending radially relative to the axis of the bore, it is preferably injected from opposite directions through two passages each extending tangentially relative to the bore axis. Tangential injection is preferred because it utilizes centrifugal force to spread the liquid coolant circumferentially around the curved wall of the bore. The liquid coolant is fed to the injection passages from an annular liquid chamber formed between the rod of an injection piston and a surrounding housing wall provided by the gun block adjacent to its ammunition (breech) chamber.
One side of the piston head contacts the liquid and the opposite side is exposed to a gas chamber that is fed with a portion of the propellant gases so that, upon firing of the ammunition, the piston is driven forward to inject the coolant into the bore at or immediately behind the base of the projectile as it starts down the bore of the gun barrel. The liquid is injected at a pressure higher than the pressure of the propelling gases because the area of the head in contact with the gas is substantially larger than the area of the head in contact with the liquid. Although the preferred embodiment utilizes two coolant chambers and pistons, it is feasible to use one piston or more than two pistons each with its corresponding liquid chamber and injection passage.
Because the injected liquid spreads down the barrel wall as a thin vaporizing film immediately behind the projectile, the injected liquid effectively cools the barrel and shields the barrel wall from the hot propelling gases generated by the burning solid propellant. This shielding effect, which is more pronounced at the entrance to the barrel bore where the film is thickest and where the most erosion would otherwise occur, enables the use of "hot" (highly energetic) propellants for increased muzzle velocity without the need to increase the pressure in the breech chamber. Without the shielding effect, such hot propellants cannot be used effectively without special means for cooling the barrel wall externally. In the absence of external cooling or the shielding effect provided by the present invention, severe erosion would be produced by the very hot combustion gases generated by the burning of these hot propellants. Thus, the invention also enables a gun to have an increased firing rate without the need for externally cooling the barrel. The invention is particularly useful when applied to tank guns and to howitzers.
The present invention therefore teaches a method and apparatus whereby a coolant liquid is injected at or near the entrance to the barrel bore during each firing of the ammunition, which is the location most susceptible to combustion gas erosion. The liquid injection pressure is derived directly from the breech pressure by means of one or more differential area pistons. This arrangement provides for a compact and simple construction of the breech block. Because the liquid is preferably injected rapidly and tangentially relative to the bore axis, it spreads around the curved bore wall as a thin film due to centrifugal forces, and this liquid and its vapor will stay in the boundary layer as they follow the projectile down the barrel. Thus, the liquid and/or the vapor shield the barrel wall from the main hot gas flow, and the barrel temperature is lowered with less reduction of the muzzle energy than if protecting additives were included along with propellant in the propellant charge. Suitable coolant liquids for injection are water, methanol, ethanol, antifreeze solutions, and combinations thereof, and these are readily available. The alcohols and their solutions are preferred because they have low freezing points.
The present invention has numerous advantages over the prior art technology discussed in the Background above. Whereas the invention provides barrel cooling, barrel chrome plating does not reduce heat transfer from the hot gases. Hence, the increase in the bulk barrel temperature of plated barrels limits the sustained firing rates usable with such barrels. Furthermore, it is difficult and expensive to obtain a uniform chrome plating in the bore of a barrel.
Wear reducing additives consume propellant charge space and limit the geometry of the charge. These additives also are less effective when used in high performance guns. Propellant additives that lower flame temperature may appear to be promising, but they impart significant performance penalties and may shorten the shelf life of the main propellant and compromise its mechanical integrity. Liquid capsules at the rear of the projectile would significantly increase the cost of the ammunition and are believed to be impractical for most projectile designs. Even if practical, liquid capsules would be capable of cooling only around the moving projectile and therefore would be primarily effective well down the barrel length, not at the beginning of the barrel where erosion is most prominent.
BRIEF DESCRIPTION OF THE DRAWINGS
The construction, operation and advantages of the present invention may be understood and appreciated more fully from the detailed description below taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a plan view in cross section of the invention before firing of the gun;
FIG. 2 is a transverse cross-sectional view taken along lines 2--2 of FIG. 1;
FIG. 3 is a plan view in cross section illustrating operation of the FIG. 1 embodiment after firing of the gun;
FIG. 4 is a transverse cross-sectional view taken along lines 4--4 of FIG. 3;
FIG. 5 is a graph illustrating the change in gun muzzle kinetic energy from the base line energy of a base line propellant versus the change in propellant gas temperature from the base line temperature achieved by burning a hot propellant in the presence of ethanol as the liquid coolant used in the invention, and in the presence of various solid additives of the type mixed with a hot propellant; and,
FIG. 6 is a diagrammatic illustration of the term "Constant Solid Volume Fraction" as used in the ballistic calculations plotted in FIG. 5.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
There is shown in FIG. 1 a preferred embodiment of the invention as employed in a generic tank gun, generally designated 10, having a barrel 12 screwed into a gun block 14. Shown in the bore 16 of the barrel 12 is a projectile 18 backed by a propellent charge 20 and an ignitor 22 contained in a combustible casing 24. The projectile 18 has a base 19, the periphery of which is adapted to slide along the curved wall of the bore 16. If the gun is an artillery piece that does not use a cartridge as represented by the casing 24, the propellant charge 20 may be encased in bags as used for separately loaded ammunition.
The casing 24 is shown inserted into a breech (propellant) chamber 56 of the gun block 14 where it is held in position for firing by a breech plug 26 that screws into the rear of block 14 until it abuts against an annular spacer member 28. A breech plate 30 is then closed to lock and seal the casing 24 within the breech chamber 56. A forward casing seat 33 is defined by a housing wall 32 of the gun block. The housing wall 32 also forms the cylindrical breech chamber for receiving the casing 24. An outer portion 34 of housing wall 32 forms an entrance to the bore 16 and a seat for the inner end of the barrel 12.
The gun block 14 includes two identical stepped bores each having an outer bore portion 36 for guiding a rod 37 of a piston 35, and an inner bore portion 38 that is stepped radially outward from the outer bore 36 for receiving a piston head 39 arranged for sliding movement therein. An annular liquid chamber 42 is thus defined between the piston rod 37 and the surface of the inner bore 38. Liquid leakage around piston rod 37 is prevented by an O-ring seal 48 and liquid leakage around piston head 39 is prevented by an O-ring seal 50. The outer ends of piston rods 37 are exposed to ambient pressure. Referring now to FIG. 2, liquid chamber 42 is filled through an inlet passage 43 containing a fitting 41 providing a one way check valve as illustrated by a ball valve element 44 held against a valve seat by a spring 46.
When each piston head 39 is in its fully retracted position, it is seated against spacer 28 so as to be in spaced relation to the breech plug 26 and to define therebetween a gas chamber 52. Each gas chamber 52 is in fluid communication with the breech chamber 56 via a gas passage 54. As shown in FIG. 2, the axes of the piston rods preferably lie in a common plane with a central axis of the bore 16.
Each liquid chamber 42 is in fluid communication with the breech chamber 56 via a liquid passage 58 containing a stem valve 60 biased to the closed position shown in FIG. 2 by a coil spring 62 held in a valve housing 64 that is mounted by its threaded engagement with the gun block 14. The outlet 59 of the liquid passage 58 is in the vicinity of the bore entrance as formed by housing wall portion 34. In its closed position, the stem valve 60 seals the passage 58 so as to keep liquid from flowing from liquid chamber 42 to breech chamber 56 when chamber 42 is at ambient pressure. During the filling of liquid chamber 42 via valve fitting 41 in inlet passage 43, chamber 42 becomes slightly pressurized. This pressure acts on head 61 of stem valve 60 to cause the valve 60 to retract slightly, thereby momentarily opening the valve to vent air to ambient via liquid passage 58 and gun bore 16. Once the air is vented and the liquid fill pressure is terminated, the pressure in liquid chamber 42 returns to ambient and valve 60 closes fully.
Operation of the invention will now be described with reference to FIGS. 3 and 4. The ignitor 22 is fired in conventional fashion and causes the propellant charge 20 to ignite and burn, which also burns away the combustible casing 24. As the gas pressure rises due to combustion of the propellant charge in the breech chamber 56, the projectile 18 is propelled rapidly forward under the action of the expanding gas. A portion of the gas generated is communicated to the gas chambers 52 where its pressure acts on the area A G of the piston head 39, thereby causing the pressure of the liquid in chamber 42 to also rise. The liquid pressure then rises above the gas pressure because the cross-sectional area A E at the end of piston rod 37 is exposed to ambient pressure, and therefore the liquid contact area A L of piston head 39 is substantially less than the gas contact area A G , i.e., A L =A G -A E . As the liquid pressure rises, it causes stem valve 60 to retract against the tension of spring 62, thereby opening the valve and allowing the liquid in chamber 42 to be injected into the bore 16 in the vicinity of its entrance as formed by the housing wall portion 34 adjacent to the outer portion of breech chamber 56. In the "vicinity" of the bore entrance may include an outer part of the breech chamber or an inner part of the barrel 12 so long as the film 70 forms immediately behind the projectile base 19 as it leaves its rest position adjacent to the breech chamber.
Although the liquid passages 58 may enter the bore from a radial direction, it is preferable that the passages 58 enter the bore tangentially as shown in FIG. 4. In addition, the respective areas A G and A L and the liquid passages 58 are sized so that the liquid is injected tangentially along the curved bore wall above the casing 24 at a sufficiently high velocity to provide the centrifugal forces needed to spread the liquid as a substantially uniform thin film 70 over the entire circumference of the inner end of the gun bore immediately behind where it is contacted by the perimeter of the projectile base 19. As the projectile 18 leaves its rest position, the liquid also flows into the inner end portion of the gun barrel 16 behind the projectile 18, where it continues to form the thin film 70 of liquid and/or vapor.
Thus, because of the centrifugal force provided by the tangential injection, the injected liquid spreads out as the thin film 70 on the barrel wall. The hot gas flow in the barrel pushing the projectile 18 also pushes the liquid layer 70 down the barrel on its bore wall, while vaporizing at least a portion of the liquid. Because the liquid and its vapor are in the boundary layer in contact with the bore wall, they follow the projectile down the barrel but at a lower speed than that of the projectile. The spreading liquid film 70 and the vapor produced thereby shield the barrel from the main hot gas flow, and also the temperature of the barrel is lowered due to the cooler liquid and the conversion of at least a portion of the liquid, if not all, to vapor. The physics of the liquid injection may be represented by the equations set forth below.
The balance of forces on the piston 35 may be represented as: ##EQU1## where P G and P L are the gas and liquid pressures, A G is the area of the piston head contacted by the gas and A E is the cross-sectional area of the piston rod.
The liquid mass injection rate is:
m.sub.L =ρ.sub.L A.sub.2i V.sub.L (2)
where ρ L is the liquid density, V L is the liquid injection velocity, and A 2i is the total cross-sectional area of the two liquid injection passages 58, i.e., A i +A i =A 2i .
V L is found from the Bernoulli equation: ##EQU2## where C D is the discharge coefficient. For a practical design of piston 35, a value of P L =1.33 P G is reasonable and this will result in injection velocities of 400 to 600 meters per second (m/s).
Suitable liquids for use in liquid chambers 42 include, without limitation, water, methanol, ethanol, and water solutions containing these alcohols or other antifreeze compositions. The alcohols and their solutions are preferred because they are readily available and easily vaporized, and have low freezing points and good cooling and protective characteristics. However, because these liquids do not increase the chemical energy available to the system, there is a penalty associated with the injection of these liquids into the bore of the gun barrel. The liquid is, in effect, a parasitic mass that is accelerated down the barrel by the gas flow, thereby consuming energy that otherwise would be available for transfer to the projectile 18 as kinetic energy.
On the other hand, because the hot combustion gas is cooled by the liquid, a hot burning propellant may be used that is more energetic than a base line (standard) propellant so that the projectile actually may gain considerably more muzzle kinetic energy without exceeding the desirable base line gas temperature at the wall of the bore. As a conservative example in support of this advantage, it may be assumed that the injected liquid instantly mixes with the propellant gas and immediately vaporizes, and that this vapor reaches physical, chemical and thermal equilibrium with the propellant gas. In other words, it is assumed that a portion of the system energy is used for completely vaporizing the liquid and for accelerating this vapor to the full velocity of the combustion gas. This is a conservative case because in reality the liquid and its vapor will reside in the boundary wall layer, lag the projectile motion, and leave unaffected the core of the gas in the bore of the barrel.
Shown in FIG. 5 by way of example are the results of ballistic calculations done with the Chem P method for injected ethanol and various solid additives. The Chem P method is presented in a paper by A. J. Kotlar entitled "The Effect of Variable Composition Equilibrium Thermochemistry In Constant Breech Pressure (CBP) Gun Simulations," Proceedings of the 15th International Symposium on Ballistics (1995), Vol. 3, p. 119-126. This method models an idealized gun system and adequately simulates optimized guns by imposing constant breech pressure, a Lagrange pressure gradient, perfect mixing, and chemical equilibrium. The gun in the FIG. 5 example is a standard 120 millimeter M256 tank gun. The base line propellent is known as JA2, the hot burning propellant is known as BAC85, and the cooling liquid is ethanol.
Because the premixing of various additives with the hot propellant BAC85 is an alternative to injecting ethanol or other liquids in accordance with the invention, the effects of mixing various solid additives with BAC85 are also shown in FIG. 5. The acronyms shown in FIG. 5 for the hot propellant and its solid additives have the following meanings: NQ is nitroguanidine, TAGN is triaminoguanidinium nitrate, HZBTA is hydrazinium bitetrazolamine, UREA is the generic name for carbamide, MENENA is N-methyl-betanitroxyethynitramine, CG is cyanoguanidine, TAZ is triaminoguanidinium azide, DADNH is 1,6-diazido-2,5-dinitrazahexane, DANPE is 1,5-diazido-2-nitrazapentane, DHED is dihydrazine ethylenedinitramine, CL20 is hexanitrohexaazaisowurtzitane, BAMO is 3,3-bis(azidomethyl)oxetane, and AMMO is 3-azidomethyl-3-methyl oxetane.
The results of the ballistic calculations are plotted in FIG. 5 as the percent change in muzzle kinetic energy from the base line energy versus the change in gas temperature from the base line temperature. These results show that it takes only 4 percent (4%) by weight of added liquid mass (ethanol) to cool the hotter combustion gas from burning BAC85 to the base line JA2 gas temperature, while still retaining over 80 percent (80%) of the muzzle kinetic energy gain for transfer to the projectile. Furthermore, the injected liquid performance is substantially better than that of any of the premixed additives.
Because the solids of the propellant and its additives are in granular form, the charge is porous and the actual loading density of the solids in the combustion (breech) chamber is less than their intrinsic density. The volume fraction is the ratio between the loading density of the baseline propellant JA2 (0.99 g/cc) and its intrinsic density (1.573 g/cc), i.e., 0.629. In the ballistic calculations, the mass of the solids is calculated such that the volume of the solids is a constant 0.629 of the combustion chamber volume. Because different solid additives have different densities, the actual charge mass will vary according to the additive used. In the case of a liquid additive in accordance with the invention, the charge mass is that of the BAC85 plus the liquid mass. In the corresponding ballistic calculations, the combustion chamber volume is increased by the volume of the liquid. Therefore, the calculations for both solid and liquid additives, as plotted in FIG. 5, were based on a "Constant Solid Volume Fraction" as illustrated diagrammatically in FIG. 6.
Bearing in mind that the calculations are overly conservative with respect to the liquid injection case but not the additive cases, the superiority of liquid injection according to the invention is even more striking. In reality, with liquid injection, the boundary layer on the inner surface of the barrel will be far cooler than with any of the additives because additive cooling is a bulk process throughout the breech chamber 56, while the liquid cooling is a boundary layer process as represented by the thin film 70. Similar ballistic calculations with water as the injected liquid indicate that for the same liquid percentage, there is a greater performance penalty with water than with ethanol. The reason for this is believed to be that ethanol generates hydrogen that lowers the average molecular weight of the propelling gases, whereas water generates water vapor that is heavier than hydrogen. In other words, the lower the average molecular weight of the propelling gas and vapor mixture, the better the performance achieved by liquid injection.
While the invention has been described above in conjunction with the preferred embodiments thereof, many changes, modifications, alterations and variations will be apparent to those skilled in the art when they learn of the invention. Thus, although the invention is described in conjunction with a particular projectile cartridge, it is also applicable to other types of cartridges and to ammunition of the non-fixed type where the propellant is loaded separately from the projectile. It is also feasible to use only one injection piston of the type shown, or to use more than two such pistons. It is also feasible to use an annular piston movable in an annular liquid chamber concentric to the breech chamber 56, such a piston and chamber arrangement being shown and described in my copending application, Ser. No. 08/946,863, which is pending and is entitled "Method and Apparatus for Dispensing Liquid with Gas", the entire contents of this copending application being incorporated herein by reference. Accordingly, the preferred embodiments of the invention set forth above are intended to be illustrative, not limiting, and various changes may be made without departing from the spirit and scope of the invention as defined by the claims set forth below. | A method and apparatus for injecting a liquid through a liquid passage cocting a liquid chamber to an outlet in the vicinity of the entrance of a gun bore. The liquid is forced through the passage by a piston movable in the liquid chamber in response to the pressure of a gas generated in a propellant chamber by combustion of a propellant for propelling a projectile down the bore. Two pistons and two liquid chambers may be arranged opposite to each other in a common plane with the propellant chamber and the outlets of the liquid passages may be located substantially opposite to each other in a wall of the bore. Each liquid passage may be arranged to inject the liquid in a tangential direction relative to the longitudinal axis of the bore so that centrifugal forces spread the liquid as a film around the circumference of the bore. Valves may be provided to close the respective liquid passages in the absence of pressure in the liquid chambers. | 5 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a Venetian blind cutting machine adapted to cut the headrail, bottom rail, and slats of a Venetian blind to the desired length and, more particularly, to such a Venetian blind cutting machine, which has means to lift/lower the Venetian blind to be cut automatically to the desired elevational cutting position.
[0003] 2. Description of the Related Art
[0004] A variety of Venetian blind cutting machines have been disclosed and have appeared on the market. Similar designs are seen in U.S. Pat. Nos. 5,799,557; 5,927,172; 6,089,302. These Venetian blind cutting machines commonly comprise a blind locating assembly having through holes for supporting the headrail, bottom rail, and slats of a Venetian blind to be cut, a cutter, and an air cylinder or reversible motor adapted to drive the cutter to cut the parts of the Venetian blind to the desired length. These Venetian blind cutting machines are commonly used in blind sale centers and operated by a salesman to cut the Venetian blind to the length requested by the consumer buying the Venetian blind. Because the blind locating assembly of a Venetian blind cutting machine fits one particular model of Venetian blinds only. When cutting a different model of Venetian blind, a different blind locating assembly shall be used. It is complicated to change the blind locating assembly of a Venetian blind.
[0005] In order to eliminate the aforesaid problem, Venetian blind cutting machines having two blind locating assemblies are developed. A Venetian blind cutting machine having two blind locating assemblies is suitable for cutting two different types of Venetian blinds.
[0006] Further, a Venetian blind cutting machine has a carriage adapted to carry a Venetian blind to be cut. When a Venetian blind placed on the carriage, it is then pushed into the blind locating assembly for cutting. When a Venetian blind cutting machine having two blind locating assemblies is used, the user may have to adjust the elevation of the blind carriage to the selected blind locating assembly. Because the elevation adjustment structure of the blind carriage is adjusted manually, the adjustment of the blind carriage takes much time and labor.
SUMMARY OF THE INVENTION
[0007] The present invention has been accomplished under the circumstances in view. It is therefore one object of the present invention to provide a Venetian blind cutting machine, which has means to automatically move the Venetian blind to the desired elevation for setting into the selected cutting position.
[0008] It is another object of the present invention to provide a Venetian blind cutting machine, which saves much vertical installation space.
[0009] To achieve these objects of the present invention, the Venetian blind cutting machine comprises a machine base, two blind locating modules mounted on the machine base at different elevations, the blind locating modules each having a set of through holes for supporting component parts of a Venetian blind to be cut, a blind carriage adapted to carry the Venetian blind to be cut, a carriage driving mechanism mounted on the machine base at one side of the blind locating modules for moving the blind carriage to the elevation of one of the blind locating modules for enabling the Venetian blind to be cut to be put in the selected blind locating module for cut, a cutter provided at the other side of the blind locating modules, and a cutter drive adapted to move the cutter across the imaginary axis passing through each of the through holes of the blind locating modules to cut the component parts of the loaded Venetian blind to the desired length and then to return the cutter after cutting.
[0010] According to a first embodiment of the present invention, the carriage driving mechanism uses a reversible motor to rotate a double-thread screw rod, causing two movable screw nuts to move two pair of links and to further lift/lower the blind carriage.
[0011] According to a second embodiment of the present invention, air cylinders are used to reciprocate two slides on two parallel sliding rails, causing the slides to move two pairs of links and to further lift/lower the blind carriage.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a top view of a Venetian blind cutting machine constructed according to a first preferred embodiment of the present invention.
[0013] [0013]FIG. 2 is a side view of the Venetian blind cutting machine according to the first embodiment of the present invention.
[0014] [0014]FIG. 3 is a sectional view in an enlarged scale taken along line 3 - 3 of FIG. 1.
[0015] [0015]FIG. 4 is an operational view of the present invention showing the blind carriage lifted to the elevation of the first blind locating module.
[0016] [0016]FIG. 5 is similar to FIG. 4 but showing the blind carriage lowered to the elevation of the second blind locating module.
[0017] [0017]FIG. 6 is a schematic drawing of a part of the Venetian blind cutting machine according to the second preferred embodiment of the present invention, showing the blind carriage moved between the upper limit position and the lower limit position.
[0018] [0018]FIG. 7 is a top plain view of FIG. 6.
DETAILED DESCRIPTION OF THE INVENTION
[0019] Referring to FIGS. 1 - 3 , a Venetian blind cutting machine 1 in accordance with the first preferred embodiment of the present invention is shown comprised of a machine base 10 , two blind locating modules, namely, the first blind locating module 20 and the second blind locating module 30 , a cutter unit 40 , a limiter 50 , and a die block adjustment mechanism 60 .
[0020] The machine base 10 comprises a base support frame 11 , and a vertical mount 12 located on the top side of the base support frame 11 . The vertical mount 12 has a first side 121 , a second side 122 opposite to the first side 121 , and two openings (not shown) cut through the first side 121 and the second side 122 at different elevations.
[0021] The blind locating modules 20 and 30 each have a first side 21 or 31 , a second side 22 or 32 opposite to the first side 21 or 31 , through holes 23 or 33 , and die blocks 24 or 34 . The through holes 23 and 33 of the blind locating modules 20 and 30 are made subject to the cross-sections of the component parts of two different types of Venetian blinds, so that the component parts of two different types of Venetian blinds can be respectively positioned in the through holes 23 and 33 of the blind locating modules 20 and 30 . The blind locating modules 20 and 30 are respectively mounted on the vertical mount 12 of the machine base 10 at different elevations, keeping the first sides 21 and 31 of the blind locating modules 20 and 30 respectively attached to the second side 122 of the vertical mount 12 and the through holes 23 and 33 of the blind locating modules 20 and 30 respectively aimed at the openings of the vertical mount 12 . The two opposite sides corresponding to the first sides 21 and 31 and second sides 22 and 32 of the blind locating modules 20 and 30 are defined hereinafter as the first lateral side and the second lateral side respectively.
[0022] The cutter unit 40 comprises two cutters 41 and 42 , and a cutter drive 43 . The cutters 41 and 42 are respectively coupled to a respective transverse sliding track at the second sides 22 and 32 of the blind locating modules 20 and 30 for a reciprocating motion on the respective transverse sliding track. The reciprocating paths provided by the transverse sliding tracks at the second sides 22 and 32 of the blind locating modules 20 and 30 pass across the imaginary axes passing through the through holes 23 and 33 of the blind locating modules 20 and 30 respectively, so that the cutters 41 and 42 can be moved across the imaginary axes passing through the through holes 23 and 33 . The cutter drive 43 comprises a reversible motor 431 mounted on the machine base 10 , and a transmission gear set 433 formed of transmission gears 433 a and 433 b and a rack 433 c and coupled between the output shaft 432 of the reversible motor 431 and the cutters 41 and 42 for reciprocating the cutters 41 and 42 along the transverse sliding tracks at the second sides 22 and 32 of the blind locating modules 20 and 30 . During each reciprocating cycle, the cutters 41 and 42 are moved across the imaginary axes passing through the through holes 23 and 33 and then returned to their former positions.
[0023] The limiter 50 comprises a rack 51 mounted on the machine base 10 , two pairs of sliding rails 52 respectively made of round rods and mounted in the rack 51 at different elevations corresponding to the through holes 23 and 33 of the blind locating modules 20 and 30 , two slides 53 respectively and slidably coupled to the pairs of sliding rails 52 , two stop plates 54 respectively mounted on the slides 53 and extended across the imaginary axes passing through the through holes 23 and 33 and adapted to stop the slats of the Venetian blinds being inserted through the through holes 23 and 33 of the blind locating modules 20 and 30 for cut, and two coil springs 55 respectively mounted on the sliding rails 52 and stopped against the slides 53 .
[0024] The die block adjustment mechanism 60 is located on the machine base 10 , and adapted to adjust the positions of the die blocks 24 and 34 of the blind locating modules 20 and 30 manually.
[0025] The structure of the aforesaid Venetian blind cutting machine is similar to the conventional designs. The operation of the Venetian blind cutting machine is outlined hereinafter. At first, the operator insert the component parts of one of the two different Venetian blinds from the first lateral side through the through holes 23 or 33 of the blind locating modules 20 and 30 to the second lateral side, enabling the corresponding ends of the component parts of the inserted Venetian blinds to be respective topped at the stop plates 54 . Thereafter, the operator starts the cutter drive 43 of the cutter unit 40 to feed the cutters 41 and 42 , causing the cutters 41 and 42 to cut the component parts of the inserted Venetian blinds to the desired length.
[0026] The Venetian blind cutting machine further comprises a blind carriage 70 , and a carriage driving mechanism 80 . The carriage driving mechanism 80 comprises a base framework 81 located on the machine base 10 , a reversible motor 82 , a double-thread screw rod 83 , two transmission devices 84 , and four links 85 . The base framework 81 comprises a platform 811 , and two side plates, namely, the first side plate 812 and the second side plates 813 vertically disposed at two lateral sides of the platform 811 . The reversible motor 82 is located on the first side plate 812 , keeping the output shaft (not shown) thereof suspended above the platform 811 . The double-thread screw rod 83 has one end coupled to the output shaft of the reversible motor 82 , a middle part supported in an axle bearing in an upright axle holder 814 at the platform 811 , and the other end supported in an axle bearing in the second side plate 813 . The two threads 831 and 832 of the double-thread screw rod 83 extend in reversed directions. The transmission devices 84 are screw nuts respectively threaded onto the threads 831 and 832 of the double-thread screw rod 83 . The links 85 are respectively and bilaterally pivoted with one end thereof to the transmission devices 84 . The blind carriage 70 has four pivot holders 71 fixedly provided at the bottom sidewall thereof in four corners, and respectively pivoted to the other end of each of the links 85 . The blind carriage 70 is maintained in horizontal in the first lateral side relative to the blind locating modules 20 and 30 .
[0027] When started the reversible motor 82 to rotate the double-thread screw rod 83 , the screw nuts 84 are moved relative to each other along the double-thread screw rod 83 , thereby causing the links 85 are moved to lift or lower the blind carriage 70 between the elevation of the first blind locating module 20 and the elevation of the second blind locating module 30 .
[0028] Further, sensors, for example, limit switches (not shown) are provided at locations within the path of the screw nuts 84 to control the upper and lower limit positions of the blind carriage 70 , enabling the blind carriage 70 to be stopped at the elevation of first blind locating module 20 or the elevation of the second blind locating module 30 .
[0029] Referring to FIGS. 4 and 5, by means of the blind carriage 70 and the carriage driving mechanism 80 , the operator can carry a Venetian blind to be cut on the blind carriage 70 to the elevation of the first blind locating module 20 as shown in FIG. 4, or the elevation of the second blind locating module 30 as shown in FIG. 5 subject to the type of the Venetian blind carried on the blind carriage 70 . If the Venetian blind must be set in the first blind locating module 20 for cutting, the operator can control the carriage driving mechanism 80 to lift the blind carriage 70 to the elevation of the first blind locating module 20 as shown in FIG. 4, and then put the component parts of the Venetian blind on the blind carriage 70 , and then push the component parts of the Venetian blind through the through holes 23 of the first blind locating module 20 , and then operate the cutter unit 40 to cut the component parts of the Venetian blind to the desired length. If the Venetian blind must be set in the second blind locating module 30 for cutting, the operator can control the carriage driving mechanism 80 to lower the blind carriage 70 to the elevation of the second blind locating module 30 as shown in FIG. 5, and then put the component parts of the Venetian blind on the blind carriage 70 , and then push the component parts of the Venetian blind through the through holes 33 of the second blind locating module 30 , and then operate the cutter unit 40 to cut the component parts of the Venetian blind to the desired length.
[0030] By means of controlling the carriage driving mechanism 80 , the blind carriage 70 is automatically adjusted to the desired elevation for enabling the workpiece to be set into position for cutting by the cutter unit 40 . Therefore, the blind cutting machine saves much labor and time.
[0031] When the carriage 70 lowered to the lower limit position (the elevation of the second blind locating module 30 ), the links 85 are approximately set in horizontal and received in between the blind carriage 70 and the platform 811 of the base framework 81 of the carriage driving mechanism 80 . At this time, the height between the base framework 81 and the blind carriage 70 is minimized, i.e., the installation of the carriage driving mechanism 80 does not occupy much vertical installation space.
[0032] [0032]FIGS. 6 and 7 show the second preferred embodiment of the present invention. Similar to the aforesaid first embodiment of the present invention, the blind cutting machine according to the second embodiment of the present invention is comprised of a machine base, two blind locating modules, a cutter unit, a limiter, and a die block adjustment mechanism. This embodiment further comprises a blind carriage 70 and a carriage driving mechanism 90 .
[0033] The carriage driving mechanism 90 comprises a base framework 91 located on the machine base, two sliding rails 92 , two air cylinders 93 , two slides 94 , and four links 95 . The base framework 91 comprises a platform 911 , and two side plates 912 vertically disposed at two lateral sides of the platform 911 . The sliding rails 92 are connected between the side plates 912 and arranged in parallel. The air cylinders 93 are respectively mounted in the side plates 912 , each having a piston rod 931 suspended above the platform 911 between the sliding rails 92 . The slides 94 are slidably mounted on the sliding rails 92 and coupled to the piston rods 931 of the air cylinders 93 . The links 95 are respectively and bilaterally pivoted with one end thereof to the slides 94 . The blind carriage 70 has four pivot holders 71 fixedly provided at the bottom sidewall thereof in four corners and respectively pivoted to the other end of each of the links 95 . The blind carriage 70 is maintained in horizontal in the first lateral side relative to the blind locating modules.
[0034] When compressed air provided to the air cylinders 93 to extend out the piston rods 931 , the slides 94 are moved along the sliding rails 92 toward each other to lower the blind carriage 70 to the lower limit position. On the contrary, when compressed air provided to the air cylinders 93 to pull back the piston rods 931 , the slides 94 are moved along the sliding rails 92 apart from each other to lift the blind carriage 70 to the upper limit position. | A Venetian blind cutting machine is constructed to include a machine base, two blind locating modules mounted on the machine base at different elevations, each of which having a set of through holes for supporting component parts of a Venetian blind to be cut, a blind carriage adapted to carry the Venetian blind to be cut, a carriage for moving the blind carriage to the elevation of one of the blind locating modules for enabling the Venetian blind to be cut to be put in the selected blind locating module for cut, a cutter provided at the other side of the blind locating modules, and a cutter drive adapted to move the cutter across the imaginary axis passing through each of the through holes of the blind locating modules to cut the component parts of the loaded Venetian blind and then to return the cutter after cutting. | 8 |
TECHNICAL FIELD
The present invention relates to 9-hydrazone and 9-azine erythromycin derivatives and a process of making the same. These compounds are useful intermediates in the process of preparing 6-O-alkyl erythromycin thereof.
BACKGROUND OF THE INVENTION
6-O-methylerythromycin A (clarithromycin), shown below, is a potent macrolide antibiotic disclosed in U.S. Pat. No. 4,331,803.
In general, the process for making clarithromycin can be thought of as a four-step procedure beginning with erythromycin A as the starting material:
Step 1: optionally convert the 9-oxo group to an oxime; Step 2: protect the 2′ and 4″ hydroxyl groups; Step 3: methylate the 6-hydroxyl group; and Step 4: deprotect at the 2′, 4″ and 9-positions.
A variety of means for preparing 6-O-methylerythromycin A have been described. 6-O-methylerythromycin A can be prepared by methylating a 2′-O-3′-N-dibenzyloxycarbonyl-des-N-methyl derivative of erythromycin A•(U.S. Pat. No. 4,331,803). 6-O-methylerythromycin A can also be made from 9-oxime erythromycin A derivatives (See, e.g., U.S. Pat. Nos. 5,274,085; 4,680,386; 4,668,776; 4,670,549 and 4,672,109, U.S. Pat. No. 4,990,602 and European Patent Application 0260938 A2).
In those reports relating to 9-oxime erythromycin A derivatives, the oxime is protected during methylation with a 2-alkenyl group (U.S. Pat. Nos. 4,670,549 and 4,668,776), a benzyl or substituted benzyl group (U.S. Pat. Nos. 4,680,386, and 4,670,549) or a moiety selected from the group consisting of lower alkyl, substituted alkyl, lower alkenyl, aryl substituted methyl, substituted oxalkyl, substituted thiomethyl (U.S. Pat. No. 4,672,109), and ketal group (U.S. Pat. No. 4,990,602).
There continues to be a need to provide a rapid, efficient method of producing 6-O-alkyl erythromycin compounds that uses mild, neutral synthetic conditions and to provide novel intermediates useful in the production of 6-O-alkyl erythromycin derivatives.
SUMMARY OF THE INVENTION
The invention relates to novel 9-hydrazone and 9-azine erythromycin derivatives, to a process of making the same, and their use as intermediates in the preparation of 6-O-alkyl erythromycin.
In one aspect, the present invention relates to a compound having the formula:
wherein R and Rz 1 are independently a hydrogen or a nitrogen-protecting group; R 2 and R 4 are independently a hydrogen or a hydroxy-protecting group; R 3 is a loweralkyl or aryl group; R 5 is a hydrogen, hydroxy or a protected hydroxy group; and R 6 and R 7 are independently at each occurrence a hydrogen, an alkyl or an aryl group.
In another aspect, the present invention relates to a process for preparing a compound of the formula I, wherein the process comprises
a) reacting an erythromycin of the formula I:
wherein R 5 is as defined above, with hydrazine to convert the 9-keto into a corresponding 9-hydrazone erythromycin;
b) protecting the 2′-hydroxy, and optionally protecting the 4″-hydroxy, and the amino nitrogen of the hydrazone with hydroxy and nitrogen protecting groups, respectively; and c) selectively alkylating the 6-hydroxy group.
In still another aspect, the present invention relates to a process for preparing a compound of the formula II, wherein the process comprises
a) reacting an erythromycin of the formula III:
wherein R 5 is as defined above, with hydrazine to convert the 9-keto into a corresponding 9-hydrazone erythromycin;
b) reacting the hydrazone from step (a) with a ketone, an aldehyde or an acetal thereof or an ortho formate to produce a corresponding erythromycin 9-azine; c) protecting the 2′-hydroxy and optionally protecting the 4″-hydroxy and the amino nitrogen of the 9-azine, with hydroxy-protecting and nitrogen-protecting groups, respectively; and d) selectively alkylating the 6-hydroxy group.
The compounds of the invention are useful as intermediates in the preparation of 6-O-alkyl erythromycins which are potent antibacterial compounds.
The process of converting the compound of formula (a) into 6-O-alkyl erythromycin comprises deprotecting the hydroxy and nitrogen protected groups or the compound.
Alternatively, the process of converting the compound of formula (II) into 6-O-alkyl erythromycin comprises reacting the compound with hydroxylamine to afford the corresponding oxime, followed by deprotection with sodium hydrogen sulfite; or reacting the compound with hydrazine to afford the corresponding hydrazone and followed by deprotection with nitrous acid.
DETAILED DESCRIPTION OF THE INVENTION
A number of defined terms are used herein to designate particular elements of the present invention.
The term “erythromycin derivatives” refers to erythromycin A or B having no substituent group or having conventional substituent groups, in organic synthesis, in place of the hydrogen atoms of the 2′-, and/or 4″-hydroxy groups.
The term “alkyl” refers to saturated, straight- or branched-chain hydrocarbon radicals containing between one and ten carbon atoms including, but not limited to, methyl, ethyl, propyl, isopropyl, n-butyl, tert-butyl and neopentyl.
The term “aryl” refers to a mono-, fused bicyclic or fused tricyclic carbocyclic ring system having one or more aromatic rings including, but not limited to, phenyl, naphthyl, tetrahydronaphthyl, phenanthrenyl, biphenylenyl, indanyl, indenyl and the like. The term “bicyclic aryl” as used herein includes naphthyl, tetrahydronaphthyl, indanyl, indenyl and the like. The term “tricyclic aryl” as used herein includes anthracenyl, phenanthrenyl, biphenylenyl, fluorenyl, and the like. Aryl groups (including bicyclic and tricyclic aryl groups) can be unsubstituted or substituted with one, two or three substituents independently selected from loweralkyl, haloalkyl, alkoxy, thioalkoxy, amino, alkylamino, dialkylamino, alkenyloxy, hydroxy, halo, mercapto, nitro, carboxaldehyde, carboxy, alkoxycarbonyl and carboxamide. Substituents also include methylenedioxy and ethylenedioxy. In addition, substituted aryl groups include tetrafluorophenyl and pentafluorophenyl.
The term “alkylaryl” refers to an aryl group having alkyl substituents attached to the aryl group.
The term “alkylating reagent” refers to a reagent capable of placing an alkyl group onto a nucleophilic site, including, but not limited to, alkyl halides such as methyl bromide, ethyl bromide, n-propyl bromide, methyl iodide, ethyl iodide, n-propyl bromide; dialkyl sulfates such as dimethyl sulfate, diethyl sulfate, di-n-propyl sulfate; and alkyl or aryl sulfonates such as methyl-p-toluenesulfonate, ethyl methanesulfonate, n-propyl methanesulfonate, methyl trifluoromethanesulfonate and the like.
The term “aryl(loweralkyl)” refers to a loweralkyl radical having appended thereto 1-3 aromatic hydrocarbon groups, as for example benzyl, diphenylbenzyl, trityl and phenylethyl.
The term “aryloxy” refers to an aromatic hydrocarbon radical which is joined to the rest of the molecule via an ether linkage (i.e., through an oxygen atom), as for example phenoxy.
The term “cycloalkyl” refers to a saturated monocyclic hydrocarbon radical having from three to eight carbon atoms in the ring and optionally substituted with between one and three additional radicals selected from among loweralkyl, halo(loweralkyl), loweralkoxy, halogen. Examples of cycloalkyl radicals include, but are not limited to, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, 1-fluoro-cyclopropyl, 2-fluorocyclopropyl and 2-aniinocyclopropyl.
The term “hydroxy-protecting group” is well-known in the art and refers to substituents on functional hydroxy groups of compounds undergoing chemical transformation which prevent undesired reactions and degradations during a synthesis (see, for example, T. H. Greene and P. G. M. Wuts, Protective Groups in Organic Synthesis, 2nd edition, John Wiley & Sons, New York (1991)). Examples of hydroxy-protecting groups include, but are not limited to, benzyloxycarbonyl, acetyl, or a substituted silyl group of formula SiR 8 R 9 R 10 , wherein R 8 , R 9 and R 10 are the same or different and each is a hydrogen atom, a loweralkyl group, a phenyl-substituted alkyl group in which the alkyl moiety has 1 to 3 carbon atoms, a phenyl group, a cycloalkyl group having 5 to 7 carbon atoms, or a loweralkenyl group having 2 to 5 carbon atoms and wherein at least one of R 8 , R 9 and R 10 is not a hydrogen atom; and the like
The term “loweralkenyl” refers to a straight- or branched-chain hydrocarbon radical containing between two and six carbon atoms and possessing at least one carbon-carbon double bond. Examples of loweralkenyl radicals include vinyl, allyl, 2- or 3-butenyl, 2-,3- or 4-pentenyl, 2-,3-,4- or 5-hexenyl and isomeric forms thereof.
The term “loweralkoxy” refers to an loweralkyl radical which is joined to the rest of the molecule via an ether linkage (i.e., through an oxygen atom). Examples of loweralkoxy radicals include, but are not limited to, methoxy and ethyloxy.
The term “loweralkyl” refers to an alkyl radical containing one to six carbon atoms including, but not limited to, methyl, ethyl, propyl, isopropyl, n-butyl, tert-butyl and neopentyl.
The term “substituted alkylaryl” refers to an alkylaryl group as defined above, substituted with substituents such as nitro, alkyl, amino, halo, alkoxy as defined above, and the like.
The term “protected hydroxy” refers to a hydroxy group protected with a hydroxy protecting group, as defined above.
The term “polar aprotic solvent” refers to polar organic solvents lacking an easily removed proton, including, but not limited to, N,N-dimethyl-formamide, dimethyl sulfoxide, N-methyl-2-pyrrolidone, hexamethyl-phosphoric triamide, tetrahydrofuran, 1,2-dimethoxyethane, acetonitrile or ethyl acetate, and the like.
The term “aprotic solvent” as used herein refers to a solvent that is relatively inert to proton activity, i.e., not acting as a proton-donor. Examples include, but are not limited to, hydrocarbons, such as hexane and toluene, for example, halogenated hydrocarbons, such as, for example, methylene chloride, ethylene chloride, chloroform, and the like, heteroaryl compounds, such as, for example, tetrahydrofuran and N-methylpyrrolidinone, and ethers such as diethyl ether, bis-methoxymethyl ether. Such compounds are well known to those skilled in the art, and it will be obvious to those skilled in the art that individual solvents or mixtures thereof may be preferred for specific compounds and reaction conditions, depending upon such factors as the solubility of reagents, reactivity of reagents and preferred temperature ranges, for example. Further discussions of aprotic solvents may be found in organic chemistry textbooks or in specialized monographs, for example: Organic Solvents Physical Properties and Methods of Purification, 4th ed., edited by John. A. Riddick et al., Vol. 11, in the Techniques of Chemistry Series, John Wiley & Sons, NY, 1986.
The term “strong alkali metal base” refers to an alkali metal base having a weak conjugate acid, including, but not limited to, sodium hydroxide, potassium hydroxide, sodium hydride, potassium hydride, potassium t-butoxide, and the like.
The term “substituted aryl(loweralkyl)” refers to an aryl (loweralkyl) residue as defined above having between one and three non-hydrogen ring substituents, each independently selected from among halogen, loweralkoxy, loweralkyl, hydroxy-substituted loweralkyl, and (loweralkyl)amino. Examples of substituted aryl (loweralkyl) radicals include 2-fluorophenylmethyl, 4-fluorophenylethyl and 2,4-difluorophenylpropyl.
The compounds of the invention are represented by:
wherein R and R 1 are independenty a hydrogen or a nitrogen-protecting group; R 2 and R 4 are independently a hydrogen or a hydroxy-protecting group; R 3 is a loweralkyl or an aryl group; R 5 is a hydrogen, hydroxy or a protected hydroxy group; and R 6 and R 7 are independently at each occurrence a hydrogen, an alkyl or an aryl group.
Representative of the preferred compounds of the invention, include, but are not limited to compounds of formula I, wherein
R 2 and R 4 are trimethylsilyl groups, R 5 is hydroxyl, R 3 is methyl and R and R 1 are independently hydrogen and triisopropylsilyl groups; and
R 2 and R 4 are trimethylsilyl groups, R 5 is hydroxyl, R 3 is methyl and R and R 1 are independently hydrogen and t-butyldimethylsilyl groups.
Representative of the preferred compounds of the invention, also include, but are not limited to compounds of formula II;
wherein R 2 and R 4 are trimethylsilyl groups, R 5 is hydroxyl, R 3 is methyl and R and R 1 are independently hydrogen and isopropylidene; and
R 2 and R 4 are trimethylsilyl groups, R 5 is hydroxyl, R 3 is methyl and R and R 1 are independently hydrogen and cyclohexylidene.
The compounds of formula I are prepared by first converting the 9-keto group of an erythromycin A or B into erythromycin 9-hydrazone. The methods of preparing hydrazones are described in Sigal et al., J. Am. Chem. Soc., 78, 388-395, (1956). As for example, the 9-hydrazone is prepared by heating erythromycin at reflux in an alcoholic solvent such as methanol, ethanol or isopropanol in the presence of hydrazine until no starting material remains. The reaction typically lasts from about 12 to 36 hours. The solvent is then removed and the crude solid so obtained is used without further purification.
The 2′- and optionally the 4″-hydroxy groups of the erythromycin 9-hydrazone are then protected with a hydroxy protecting groups, such as silyl, acyl and sulfonyl groups and the like, by the methods described in T. H. Greene and P. G. M. Wuts, Protective Groups in Organic Synthesis, 2nd edition, John Wiley & Sons, New York (1991). When the protecting group is a silyl group, both the 2′- and 4″-hydroxy groups are silylated. Preferably, the 2′- and 4″-hydroxy groups are protected with trimethylsilyl groups by treating a suspension of erythromycin 9-hydrazone in acetonitrile with hexamethyldisilazane at ambient temperature and stirred for 12-24 hours. The resulting solution is made basic by adding aqueous sodium hydroxide to adjust the pH typically ranging from 8-13, preferably, 9. The erythromycin 9-hydrazone derivative thus obtained is extracted into an aprotic solvent and the solvent evaporated to give the erythromycin 2′,4″-bis-O-trimethylsilyl 9-hydrazone.
The amino nitrogen of the 9-hydrazone erythromycin derivative may optionally be protected by the nitrogen protecting groups by the methods described in T. H. Greene and P. G. M. Wuts, Protective Groups in Organic Synthesis, 2nd edition, John Wiley & Sons, New York, Chapter 7, (1991); and P. J. Kocienski, Protective Groups, Thieme, Chapter 6, (1994); and the references cited therein.
As for example, the amino nitrogen of the 9-hydrazone is protected by treating erythromycin 9-hydrazone with 1-2 equivalents of silylating agent such as triisopropylsilyl triflate in the presence of an organic base such as triethylamine in an aprotic solvent. Preferably, the reaction is carried out in the presence of triethylamine in dichloroethane. The reaction results in the formation of 9-(N-triisopropylsilyl) hydrazone erythromycin derivative which is protected at the 2′- and optionally at the 4″-positions. The hydrazone nitrogen may alternatively be protected by treating the 9-hydrazone with an appropriate ketal.
In another process of the invention, the erythromycin 9-hydrazone derivative is converted into an azine by the methods described in, for example, U.S. Pat. No. 3,780,020 and German Patent 1,966,310. As for example, the azine derivative is prepared by treating the hydrazone with an appropriate ketone, aldehyde or an acetal thereof or an orthoformate with or without a co-solvent and either with or without an added dehydrating agent such as molecular sieves. The reaction is carried out at a temperature between the room temperature and the boiling point of the ketone, aldehyde, or the co-solvent. The reaction is carried out for about one hour to about 24 hours. The azine nitrogen may be further protected by treating the 9-azine erythromycin derivative with an appropriate ketal in the presence of catalytic quantity of acid such as formic or acetic acid. The reaction mixture is stirred at ambient temperature overnight for 6 to 18 hours. The mixture is then basified to pH 8-13 and the product extracted into an appropriate solvent.
The alkylation of erythromycin 9-hydrazone derivative and erythromycin 9-azine-ketal derivative is achieved by reacting the starting compound with a suitable alkylating agent in the presence of a base. Typically, the reaction is carried out with an alkylating reagent in presence of a strong alkali metal base, in a suitable stirred or agitated polar aprotic solvent, or a mixture of such polar aprotic solvents maintained at a reaction temperature and for a period of time sufficient to effect alkylation, preferably from −15 C to room temperature for a period of one to 8 hours. The alkylating agents comprise methyl bromide, ethyl bromide, n-propyl bromide, methyl iodide, ethyl iodide, n-propyl bromide, dimethyl sulfate, diethyl sulfate, di-n-propyl sulfate, methyl-p-toluenesulfonate, ethyl methanesulfonate, methyl trifluoromethanesulfonate and n-propyl methanesulfonate. The amount of alkylating agent used is from zI to 3 molar equivalents relative to the 3′-N-oxide compound. The alkali metal base is selected from the group consisting of an alkali metal hydride, alkali metal hydroxide or alkali metal alkoxide. Examples of the alkali metal base include sodium and potassium hydride, sodium and potassium hydroxide and potassium t-butoxide. The amount of the base used is usually 1 to 2 equivalents relative to the starting compound.
The deprotection of the erythromycin 6-O-alkylated 9-hydrazone or 9-azine derivatives is carried out by the methods known in the art to obtain the erythromycin 6-O-alkylated 9-hydrazone or 9-azine. By way of an example, where the 2′- and 4″-positions are silylated, the silyl group can be removed by reacting the silylated derivative with formic acid in isopropanol. The silyl group can also be removed by using n-tetrabutylammonium fluoride in tetrahydrofuran, acetic acid, tetrahydrofuran and water, citric acid and methanol, Dowexz® resin and methanol, potassium carbonate and methanol, n-tetrabutylammonium chloride and potassium fluoride or hydrofluoric acid and acetonitrile. In the cases where the 9-hydrazone hydrogen is protected with a silyl group, removal of the silyl group is accomplished using the same procedure as set forth above.
In the alternative process, where the 9-hydrazone is converted into 9-azine, the 9-azine is removed by treating the 9-azine derivative with hydroxylamine or with hydrazine at an appropriate temperature and for a period of time sufficient to effect complete transformation. The reaction is carried out at a temperature from room temperature to 100° C. for a period of 12 to 24 hours. When treated with hydroxylamine, the resulting oxime is deprotected by methods well known in the art, preferably, by refluxing with sodium hydrogen sulfite in alcohol.
When treated with hydrazone, the resulting unsubstituted 9-hydrazone group is removed by methods known to those skilled in the art, preferably, by treating the hydrazone with nitrous acid in an aqueous/organic solution. The 6-O-alkyl erythromycin thus obtained is extracted from the aqueous solution after basification to pH 8-13.
Abbreviations
Certain abbreviations are used repeatedly in the specification which follows. These include: DMSO for dimethyl sulfoxide; HPLC for high performance liquid chromatography; IPCH ketal for isopropyl cyclohexyl ketal; TEA for triethylamine; TzEME for t-butyl methyl ether; TBAF for n-tetrabutylammonium fluoride; MeCN for acetonitrile, THF for tetrahydrofuran; HMDS for hexamethyldisilazane; and TMS for trimethylsilyl.
The invention may be better understood by reference to the following examples which are presented for illustration and not to limit the scope of the inventive concept
EXAMPLE 1
Example 1(a)
Erythromycin A 9-hydrazone
Erythromycin A (50 g) was dissolved in anhydrous methanol (150 mL) by gentle warming. To this solution was added a solution of 12.5 g anhydrous hydrazine in 50 mL of methanol. The mixture was heated at reflux for 24 hours with the exclusion of moisture from the air. The methanol and excess hydrazine were removed by evaporation under reduced pressure leaving an amorphous white solid which was crystallized from aqueous isopropanol to give the product (31 g).
Example 1(b)
Erythromycin A 2″,4″-bis-O-trimethylsilyl-9-hydrazone Erythromycin A 9-hydrazone (50 g) was suspended in acetonitrile. Formic acid (10 ml) and hexamethyldisilazane (55 g) were added sequentially below 20° C. The mixture was stirred at ambient temperature overnight. The resulting solution was cooled with an ice bath and then rendered basic (pH>9) with aqueous NaOH. The mixture was extracted with heptane and the heptane layer separated and dried (Na 2 SO 4 ). Evaporation in vacuo gave a white solid (40 g), characterized by the NMR and mass spectra.
1 Hnmr (500 MHz, CDCl 3 ), d: 2.66 (1H, H2), 1.15 (3H, C2C H 3 ), 4.26 (1H, C3C H ), 1.86 (1H, H4), 1.06 (C4C H 3 ), 3.50 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 1.63, 1.41 (2H, C′7C H 2 ), 3.31 (1H, C8C H ), 1.06 (3H, C8C H 3 ), 2.63 (1H, C10C H ), 1.11 (3H, C10C H 3 ), 3.39 (1H, C11C H ), 1.13 (3H, C12C H 3), 5.00 (1H, C13C H , 1.90, 1.44 (2H, C14C H 2 ), 0.83 (3H, C15C H 3 ), 4.37 (1H, C1′C H ), 3.16 (1H, C2′C H ), 2.48 (1H, C3′C H ), 2.21 (6H, C3′N(C H 3 ) 2 ), 1.62, 1.15 (2H, C4′C H 2 ), 3.59 (1H, C5′C H ), 1.13 (3H, C6′C H 3 ), 4.89 (1H, C1″C H ), 2.36, 1.46 (2H, C2″C H 2 ), 3.27 (3H, C3″OC H 3 ), 1.12 (3H, C3″C H 3 ), 3.13 (1H, C4″C H ), 4.25 (1H, C5″C H ), 1.19 (3H, C6″C H 3 ), 0.12 (9H, 4″OTMS), 0.08 (9H, 2′OTMS), 3.23 (1H, 60H), 3.18 (1H, 120H). 13 Cnmr (125MHz, CDCl 3 ), d: 176.6 (C═O), 44.8 (C2), 15.1 (C2Me), 79.2 (C3), 42.0 (C4), 10.0 (C4Me), 81.8 (C5), 75.6 (C6), 27.1 (C6Me), 39.0 (C7), 26.1 (C8), 19.0 (C8Me), 167.2 (C9, C═N), 33.2 (C10), 13.6 (C10Me), 71.1 (C11), 74.2 (C12), 16.1 (C12Me), 77.1 (C13), 21.2 (C14), 10.8 (C15), 102.9 (C1′), 73.2 (C2′), 65.2 (C3′), 40.9 (C3′NMe), 30.0 (C4′), 68.1 (C5′), 21.4 (C6′), 97.2 (C 3 ″), 35.7 (C2″), 73.1 (C3″), 49.6 (C3″OMe), 22.0 (C3″Me), 80.7 (C4″), 65.1 (C5″), 19.1 (C6″), 0.8 (C2′OTMS), 0.8 (C4″OTMS), MS (m/z): FAB 892 [M+H] +
Example 1(c)
Erythromycin 2′,4″-bis-O-trimethylsilyl-9-(N-triisopropylsilyl) hydrazone
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-hydrazone (1.5 g) was dissolved in CH 2 Cl 2 and TEA (0.5 ml) was added followed by triisopropylsilyl triflate (0.67 ml). The resulting mixture was stirred at ambient temperature for 2 h. Evaporation in vacuo gave an oil which was partitioned between TBME and water. The organic layer was separated and washed with water, then dried (Na 2 SO 4 ) and evaporated in vacuo to give a white solid 1.6 g; 91%. 1 Hnmr (500 MHz, CDCl 3 ), d: 2.63 (1H, H2), 1.16 (3H, C2C H 3 ), 4.21 (1H, C3C H ), 1.83 (1H, H4), 1.05 (C4C H 3 ), 3.46 (1H, C5C H ), 1.35 (3H, C6C H 3 ), 1.58, 1.38 (2H, C7C H 2 ), 3.32 (1H, C8C H ), 1.10 (3H, C8C H 3 ), 2.64 (1H, C10C H ), 1.10 (3H, C10C H 3 ), 3.45 (1H, C11C H ), 1.16 (3H, C12C H 3 ), 4.98 (1H, C13C H ), 1.91, 1.42 (2H, C14C 2 ), 0.86 (3H, C15C H 3 ), 4.45 (1H, C1′C H ), 3.20 (1H, C2′CH), 2.54 (1H, C3′CH), 2.25 (6H, C3′N(C H 3 )2), 1.65, 1.16 (2H, C4′C H 2 ), 3.67 (1H, C5′C H ), 1.16 (3H, C6′C H 3 ), 4.88 (1H, C1″C H ), 2.36, 1.46 (2H, C2″C H 2 ), 3.28 (3H, C3″OCH 3 ), 1.12 (3H, C3″CH 3 ), 3.13 (1H, C4″C H ), 4.21 (1H, C5″C H , 1.16 (3H, C6″C H 3 ), 0.13 (9H, 4″OTMS), 0.10 (9H, 2′OTMS), 3.23 (1H, 120H), 4.94 (1H, 11OH), 5.56 (1H, =N-NH-), 1.16, 1.04 (1H&3H, CH&CH 3 of iso-Pr).
13 Cnmr (125MHz, CDCl 3 ), d: 176.5 (C═O), 44.8 (C2), 14.5 (C2Me), 78.3 (C3), 42.9 (C4), 10.1 (C4Me), 82.8 (C5), 74.9 (C6), 25.6 (C6Me), 40.1 (C7), 24.6 (C8), 19.0 (C8Me), 158.7 (C9, C ═N), 33.4 (C10), 13.6 (C10Me), 72.2 (C11), 74.3 (C12), 16.4 (C12Me), 77.5 (C13), 21.7 (C14), 11.0 (C15), 102.5 (C1′), 73.1 (C2′), 65.3 (C3′), 40.9 (C3′NMe), 29.9 (C4′), 68.0 (C5′), 21.4 (C6′), 96.4 (C1″), 35.5 (C2″), 73.2 (C3″), 49.4 (C3″OMe), 22.2 (C3″Me), 80.7 (C4″), 65.0 (C5″), 19.1 (C6″), 0.9 (C2′OTMS), 0.8 (C4″OTMS), 18.2, 18.1, 17.7, 11.4 (iso-Pr).
MS (m/z): FAB1048 [M+H]+, FAB+KI 1086 [M+K] +
Example 1 (d)
Erythromycin A 2′4″-bis-O-timethylsilyl-6-O-methyl-9-(N-triisopropvlsilyl) hydrazone
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-(N-triisopropylsilyl) hydrazone (1.2 g, 1.146 mmol) was dissolved in a 1:1 mixture of DMSO and THF (10 ml) and the solution cooled to 5° C. Methyl iodide (0.43 ml; 6.9 mmol; 6eq) was added followed by KOH (0.26 g; 4.58 mmol; 4 eq). The resulting mixture was stirred at 5° C for lh the quenched by adding 40% aq. methylamine (1 ml) and the mixture stirred for 10 min. Saturated NaCl (20 ml) was added and the mixture was extracted with TBME. The organic layer was separated and washed with saturated NaCl solution, then dried (Na 2 SO 4 ) and evaporated in vacuo to give a white solid 1.18 g; 97%.
1 Hnmr (500 MHz, CDCl 3 ), d: 2.90 (1H, H2), 1.20 (3H, C2C H 3 ), 3.76 (1H, C3C H ), 1.90 (1H, H4), 1.08 (C4C H 3 ), 3.71 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 3.14 (3H, C6OC H 3 ), 1.60, 1.53 (2H, C7C H 2 ), 3.06 (1H, C8C H ), 0.97 (3H, C8C H 3 ), 2.52 (1H, C10C H ), 1.08 (3H, C10C H 3 ), 3.67 (1H, C11C H ), 1.18 (3H, C12C H 3 ), 5.14 (1H, C13C H ), 1.94, 1.46 (2H, C14C H 2 ), 0.83 (3H, C15C H 13 ), 4.46 (1H, C1′C H ), 3.14 (1H, C2′C H ), 2.52 (1H, C3′C H ), 2.22 (6H, C3′N(C H 3)2 ), 1.65, 1.13 (2H, C4′C H 2 ), 3.67 (1H, C5′CH), 1.18 (3H, C6′C H 3 ), 4.91 (1H, C1″C H ), 2.35, 1.49 (2H, C2″C H 2 ), 3.31 (3H, C3″OC H 3 ), 1.18 (3H, C3″C H 3 ), 3.16 (1H, C4″C H ), 4.23 (1H, C5″C H ), 1.22 (3H, C6″C H 3 ), 0.2 (9H, 4″OTMS), 0.10 (9H, 2′OTMS), 3.37 (1H, 120H), 5.25 (1H, 11OH), 5.28 (1H,=N-NH-), 1.19, 1.08 (1H&3H, CH&CH 3 of iso-Pr).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.4 (C═O), 45.2 (C2), 16.2 (C2 Me), 78.2 (C3), 38.8 (C4), 9.9 (C4 Me), 78.6 (C5), 78.7 (C6), 51.7 (C60Me), 20.7 (C6 Me), 37.7 (C7), 24.0 (C8), 19.2 (C8 Me), 158.9 (C9, C ═N), 32.6 (C10), 14.9 (C10 Me), 71.1 (C11), 74.0 (C12), 16.0 (C12 Me), 76.7 (C13), 21.2 (C14), 10.4 (C15), 102.3 (C1′), 73.4 (C2′), 65.2 (C3′), 41.0 (C3′NMe), 29.5 (C4′), 67.0 (C5′), 22.0 (C6′), 96.2 (Cl″), 35.9 (C2″), 73.1 (C3″), 49.6 (C3″OMe), 22.2 (C3″Me), 80.8 (C4″), 65.3 (C5″), 19.5 (C6″), 1.0 (C2′OTMS), 0.9 (C4″OTMS), 18.2, 17.9, 11.4 (iso-Pr). MS (mz/z):, FAB 1062 [M+H] +
EXAMPLE 2
Example 2(a)
Erythromycin A 2′,4″-bis-O-timethylsilyl-9-(N-tert-butyldimethylsilyl) hydrazone.
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-hydrazone (1.5 g) from Example 1(b) was dissolved in CH 2 CL 2 and TEA (0.5 ml) was added followed by tert-butyldimethylsilyl triflate (0.7 ml). The resulting mixture was stirred at ambient temperature for 2h. Evaporation in vacuo gave an oil which was partitioned between TBME and water. The organic layer was separated and washed with water, then dried (Na 2 SO 4 ) and evaporated in vacuo to give a white solid 1.61 g; 95%. 1 Hnmr (500 MHz, CDCl 3 ), d: 2.65 (1H, H2), 1.18 (3H, C2C H 3 ), 4.15 (1H, C3C H ), 1.82 (1H, H4), 1.06 (C4C H 3 ), 3.48 (1H, C5C H ), 1.34 (3H, C6C H 3 ), 1.57, 1.42 (2H, C7C H 2 ), 3.29 (1H, C8C H ), 1.12 (3H, C8C H 3 ), 2.68 (1H, C10 C H ), 1.12 (3H, C10C H 3 ), 3.48 (1H, C11C H ), 1.18 (3H, C12C H 3 ), 4.99 (1H, C13C H ), 1.94, 1.49 (2H, C14C H 2 ), 0.89 (3H, C15C H 3 ), 4.49 (1H, C1′C H ), 3.23 (1H, C2′C H ), 2.53 (1H, C3′C H ), 2.24 (6H, C3′N(C H 3 )2), 1.66, 1.21 (2H, C4′C H 2 ), 3.71 (1H, C5′C H , 1.18 (3H, C6′C H 3 ), 4.94 (1H, C1″C H ), 2.38, 1.49 (2H, C2″C H 2 ), 3.30 (3H, C3″OC H 3 ), 1.15 (3H, C3″C H 3 ), 3.16 (1H, C4″C H ), 4.22 (1H, C5″C H ), 1.18 (3H, C6″C H 3 ), 0.15 (9H, 4″OTMS), 0.11 (9H, 2′OTMS), 3.23 (1H, 120H), 4.94 (1H, l11OH), 5.54 (1H, =N-NH-), 0.16, 0.06 (6H, N-N-Si-(CH 3 ) 2 ), 0.91 (9H, N-Si-(C H 3 ) 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 176.6 (C═O), 44.6 (C2), 14.3 (C2 Me), 78.0 (C3), 42.9 (C4), 10.2 (C4 Me), 83.1 (C5), 74.8 (C6), 24.8 (C6 Me), 40.8 (C7), 24.8 (C8), 18.8 (C8 Me), 158.1 (C9, C═N), 33.5 (C10), 13.5 (C10 Me), 72.2 (Cl 11), 74.3 (C12), 16.4 (C12 Me), 77.7 (C13), 21.8 (C14), 11.2 (C15), 102.4 (C1′), 73.0 (C2′), 65.3 (C3′), 41.0 (C3′NMe), 29.7 (C4′), 67.9 (C5′), 21.6 (C6′), 96.0 (C1″), 35.4 (C2″), 73.2 (C3″), 49.4 (C3″OMe), 22.3 (C3″Me), 80.6 (C4″), 65.0 (C5″), 19.1 (C6″), 0.9 (C2′OTMS), 0.9 (C4″OTMS), 5.6, 5.9 (N-N-Si-(CH 3 ) 2 ), 18.1 (-N-Si-C), 26.4 (-N-Si-C(CH 3 ) 3 ). MS (m/z): FAB1006 [M+H] +
Example 2(b)
Erythromycin A 2′,4″-bis-O-trimethylsilyl-6-O-methyl-9-(N-tert-butyldimethylsilyl) hydrazone
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-(N-tert-butyldimethylsilyl) hydrazone (1.2 g, 1.193 mmol) was dissolved in a 1:1 mixture of DMSO and THF (10 ml) and the solution cooled to 5° C. Methyl iodide (0.45 ml; 7.157 mmol; 6eq) was added followed by KOH (0.267 g; 4.77 mmol; 4eq). The resulting mixture was stirred at 5° C. for 1h then quenched by adding 40% aq. methylamine (1 ml) and the mixture stirred for 10 min. Saturated NaCl (20 ml) was added and the mixture was extracted with TBME. The organic layer was separated and washed with saturated NaCl solution, then dried (Na 2 SO 4 ) and evaporated in vacuo to give a white solid 1.215 g; 99.9%.
1 Hnmr (500 MHz, CDCl 3 ), d: 2.89 (1H, H2), 1.19 (3H, C2C H 3 ), 3.75 (1H, C3C H ), 1.88 (1H, H4), 1.06 (C4C H 3 ), 3.68 (1H, C5C H ), 1.39 (3H, C6C H 3 ), 3.10 (3H, C60C H 3 ), 1.58, 1.52 (2H, C7C H 2 ), 2.99 (1H, C8C H ), 0.97 (3H, C8C H 3 ), 2.49 (1H, C10C H ), 1.10 (3H, C10C H 3 ), 3.66 (1H, C11C H ), 1.16 (3H, C12C H 3 ), 5.12 (1H, C13C H ), 1.94, 1.48 (2H, C14C H 2 ), 0.83 (3H, C15C H 3 ), 4.45 (1H, Cl′C1′C H ), 3.14 (1H, C2′C H ), 2.51 (1H, C3′C H ), 2.22 (6H, C3′N(C H 3 ) 2 ), 1.65, 1.16 (2H, C4′C H 2 ), 3.66 (1H, C5′C H ), 1.16 (3H, C6′C H 3 ), 4.91 (1H, C1 ″C H ), 2.35, 1.51 (2H, C2″C H 2 ), 3.31 (3H, C3″OC H 3 ), 1.16 (3H, C3″C H 3 ), 3.16 (1H, C4″C H ), 4.23 (1H, C5″C H ), 1.22 (3H, C6″C H 3 ), 0.09 (9H, 4″OTMS), 0.15 (9H, 2′OTMS), 3.38 (1H, 12OH), 5.46 (1H, 11OH), 5.20 (1H, =N-NH-), 0.16, 0.07 (6H, N-N-Si-(C H 3 ) 2 ), 0.92 (9H, N-Si-(C H 3 ) 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.5 (C═O), 45.2 (C2), 16.2 (C2 Me), 78.2 (C3), 38.8 (C4), 9.9 (C4 Me), 78.7 (C5), 78.7 (C6), 20.8 (C6 Me), 51.6 (C6OMe), 39.9 (C7), 24.0 (C8), 19.1 (C8 Me), 158.5 (C9, C ═N), 32.4 (C10), 15.0 (C10 Me), 71.2 (C11), 73.9 (C12), 16.0 (C12 Me), 76.8 (C13), 21.1 (C14), 10.4 (C15), 102.4 (C1″), 73.4 (C2′), 65.2 (C3′), 41.1 (C3′NMe), 29.5 (C4′), 67.1 (C5′), 22.0 (C6′), 96.2 (C1″), 35.9 (C2″), 73.1 (C3″), 49.6 (C3″OMe), 22.0 (C3″Me), 80.8 (C4″), 65.3 (C5″), 19.5 (C6″), 0.9 (C2′OTMS), 0.9 (C4″OTMS), 5.3, 5.7 (N-N-Si-(CH 3 ) 2 ), 18.0 (-N-Si-C), 26.2 (-N-Si-C(CH 3 ) 3 ). MS (m/z): FAB1020 [M+H]+, FAB+KI 1058 [M+K] +
Example 2(c)
Erythromycin A 6-O-methyl-9-hydrazone
Erythromycin A 2′,4″-bis-O-trimethylsilyl-6-O-methyl-9-(N-tert-butyldimethylsilyl) hydrazone (500 mg; 0.49 mmol) was dissolved in THF and 1 M TBAF (2.5 ml; 2.5 mmol, 5.1 eq) was added. The mixture was stirred at ambient temperature for 1h, then evaporated in vacuo. The resulting oil was partitioned between i-PrOAc and water. The organic layer was separated and dried with Na 2 SO 4 and evaporated in vacuo to give a white solid 300 mg; 80%. 1 Hnmr (500 MHz, CDCl 3 ), d: 2.95 (1H, H 2 ), 1.20 (3H, C2C H 3 ), 3.71 (1H, C3C H ), 1.96 (1H, H4), 1.11 (C4C H 3 ), 3.78 (1H, C5C H ), 1.44 (3H, C6C H 3 ), 3.19 (3H, C6OC H 3 ), 1.65, 1.54 (2H, C7C H 2 ), 3.16 (1H, C8C H ), 0.99 (3H, C8C H 3 ), 4.91 (2H, N-NH 2 ), 2.54 (1H, C10C H ), 1.11 (3H, C10C H 3 ), 3.51 (1H, C11C H ), 1.10 (3H, C12C H 3 ), 5.10 (1H, C13C H ), 1.92, 1.47 (2H, C14C H 2 ), 0.82 (3H, C15C H 3 ), 4.50 (1H, C1′C H ), 3.18 (1H, (C2′C H ), 3.44 (1H, C2′OH), 2.41 (1H, C3′C H ), 2.27 (6H, C3′N(C H 3 ) 2 ), 1.64, 1.20 (2H, C4′C H 2 ), 3.50 (1H, C5′C H ), 1.22 (3H, C6′C H 3 ), 4.95 (1H, C1″C H ), 2.36, 1.60 (2H, C2″C H 2 ), 3.32 (3H, C3″OCH 3 ), 1.25 (3H, C3″C H 3 ), 3.02 (1H, C4″C H ), 2.19 (1H, C4′OH), 4.03 (1H, C5″C H ), 1.29 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 174.9 (C═O), 44.8 (C2), 16.3 (C2 Me), 78.8 (C3), 38.1 (C4), 9.4 (C4 Me), 79.2 (C5), 79.1 (C6), 20.5 (C6 Me), 51.7 (C6OMe), 37.6 (C7), 26.1 (C8), 19.1 (C8 Me), 167.7 (C9, C═N), 32.6 (C10), 14.5 (C10Me), 71.1 (C11), 74.0 (C12), 15.9 (C12 Me), 77.0 (C13), 21.0 (C14), 10.6 (C15), 102.3 (C1′), 71.1 (C2′), 65.5 (C3′), 40.2 (C3′NMe), 28.6 (C4′), 68.5 (C5′), 21.4 (C6′), 96.3 (C1″), 35.0 (C2″), 72.7 (C3″), 49.4 (C3″OMe), 21.5 (C3″Me), 77.9 (C4″), 65.9 (C5″), 18.6 (C6″). MS (m/z): FAB 762 [M+H] +
Example 2(d)
6-O-Methyl Erythromycin A
Erythromycin A 6-O-methyl-9-hydrazone (2.0 g; 2.62 mmol) was suspended in MeCN (25 ml) and cooled to 0-5° C. In a separate flask, NaNO2 (0.54 g; 7.86 mmol) was dissolved in H 2 O (5 ml) and dil. HCl added to achieve pH 4. The freshly prepared nitrous acid was added dropwise to the cooled suspension and the resulting mixture allowed to warm to room temperature. Additional dil. HCl was added to readjust the pH to ca. 4. The mixture was stirred at ambient temperature overnight. The resulting mixture was basified with 5% NaOH to pH>9 and extracted with MeCN. The organic layer was separated and washed with saturated NaCl solution, dried (MgSO4) and evaporated in vacuo to give a pale yellow solid (2 g) which was recrystallized from iso-PrOH to give a white solid.
1 Hnmr (500 MHz, CDCl 3 ), d: 2.89 (1H, H2), 1.20 (3H, C2C H 3 ), 3.77 (1H, C3C H ), 1.92 (1H, H4), 1.10 (C4C H 3 ), 3.67 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 3.04 (3H, C6OC H 3 ), 1.85, 1.72 (2H, C7C H 2 ), 2.59 (1H, C8C H ), 1.13 (3H, C8C H 3 ), 3.00 (1H, C10C H ), 1.13 (3H, C10C H 3 ), 3.77 (11H, C H ), 1.12 (3H, C12C H 3 ), 5.05 (1H, C13C H ), 1.92, 1.47 (2H, C14C H 2 ), 0.84 (3H, C15C H 3 ), 4.44 (1H, C1′C H ), 3.19 (1H, C2′C H ), 2.42 (1H, C3′C H ), 2.29 (6H, C3′N(C H 3 ) 2 ), 1.66, 1.22 (2H, C4′C H 2 ), 3.49 (1H, C5′C H ), 1.23 (3H, C6′C H 3 ), 4.93 (1H, C1″C H ), 2.37, 1.59 (2H, C2″C H 2 ), 3.33 (3H, C3′OC H 3 ), 1.25 (3H, C3″C H 3 ), 3.03 (1H, C4″C H ), 4.01 (1H, C5″C H ), 1.31 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.8 (C═O), 45.1 (C2), 15.9 (C2 Me), 78.4 (C3), 39.2 (C4), 9.1 (C4 Me), 80.8 (C5), 78.4 (C6), 19.7 (C6 Me), 39.3 (C7), 45.2 (C8), 18.0 (C8 Me), 220.9 (C9, C═O), 37.2 (C10 ), 12.3 (C10Me), 69.1 (C11), 74.3 (C12), 15.9 (C12 Me), 76.6 (C13), 21.0 (C14), 10.6 (C15), 102.7 (C1), 71.0 (C2′), 65.6 (C3′), 40.3 (C3′NMe), 28.9 (C4′), 68.7 (C5′), 21.5 (C6′), 96.1 (C1″), 34.9 (C2″), 72.7 (C3″), 49.5 (C3″OMe), 21.4 (C3″Me), 77.9 (C4″), 65.8 (C5″), 18.7 (C6″). MS (m/z): FAB 748 [M+H] +
EXAMPLE 3
Example 3(a)
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-isopropylidene azine
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-hydrazone from Example 1(a) (2.0 g; 2.24 mmol) was dissolved in acetone (20 ml) and 3Åmolecular sieves (2 g) were added. The mixture was heated at reflux overnight, then diluted with MeCN. The sieves were removed by filtration though a pad of celite. The resulting solution was evaporated in vacuo to give a white solid (2 g).
1 Hnmr (500 MHz, CDCl 3 ), d: 2.86 (1H, H2), 1.15 (3H, C2C H 3 ), 4.18 (1H, C3C H ), 1.94 (1H, H4), 1.10 (C4C H 3 ), 3.59 (1H, C5C H ), 1.44 (3H, C6C H 3 ), 1.67, 1.49 (2H, C7C H 2 ), 3.53 (1H, C8C H ), 1.04 (3H, C8C H 3 ), 2.76 (1H, C10C H ), 1.22 (3H, C10C H 3 ), 3.71 (1H, C11C H ), 1.18 (3H, C12C H 3 ), 5.10 (1H, C13C H ), 1.92, 1.48 (2H, C14C H 2 ), 0.85 (3H, C15C H 3 ), 2.02, 1.86 (C17C H 3 ), 4.39 (1H, C1′C H ), 3.18 (1H, C2′C H ), 0.11 (9H, 2″OTMS), 2.53 (1H, C3′C H ), 2.23 (6H, C3′N(C H 3 ) 2 ), 1.66, 1.18 (2H, C4′C H 2 ), 3.62 (1H, C5′C H ), 1.17 (3H, C6′C H 3 ), 4.87 (1H, C1″C H ), 2.35, 1.49 (2H, C2″C H 2 ), 3.30 (3H, C3″OC H 3 ), 1.15 (3H, C3″C H 3 ), 3.16 (1H, C4″C H ), 0.14 (9H, 4″OTMS), 4.24 (1H, C5″C H ), 1.22 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.5 (C═O), 44.7 (C2), 16.0 (C2 Me), 79.7 (C3), 39.7 (C4), 9.7 (C4 Me), 81.4 (C5), 75.5 (C6), 27.1 (C6 Me), 39.1 (C7), 29.3 (C8), 18.8 (C8 Me), 178.5 (C9, C ═N), 33.1 (C10), 14.2 (C10 Me), 70.8 (C11), 74.4 (C12), 16.1 (C12 Me), 76.8 (C13), 21.1 (C14), 10.7 (C15), 163.5 (C16), 25.3, 18.3 (C17 C H 3 ), 102.6 (C1′), 73.4 (C2′), 1.0 (C2′OSi( C H 3 ) 3 ), 65.2 (C3′), 41.0 (C3′NMe), 29.8 (C4′), 67.6 (C5′), 21.8 (C6′), 96.7 (C1″), 36.0 (C2″), 73.2 (C3″), 49.7 (C3″OMe), 22.2 (C3″Me), 80.9 (C4″), 0.9 (C4″OSi( C H 3 ) 3 ), 65.0 (C5″), 19.4 (C6″). MS (m/z): 932 [M+H] +
Example 3(b)
Erythromycin A 2′, 4″-bis-O-trimethylsilyl-6-O-methyl-9-isopropylidene azine
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-isopropylidene azine (1.Og; 1.07 mmol) from the above Example was dissolved in a 1:1 mixture of THF/DMS 0 (10 ml) and cooled to 5° C. Methyl iodide (0.40 ml; 6.44 mmol) and KOH (0.237 g; 4.23 mmol) were added and the mixture was stirred at 5° C for 4 hr. The reaction was quenched by the addition of aq methylamine (1 ml). Saturated NaCl was added and the resulting mixture extracted with TBME. The organic layer was washed with saturated NaCl solution then dried (MgSO 4 ) and evaporated in vacuo to give a white solid 0.95 g (94%).
1 Hnmr (500 MHz, CDCl 3 ), d: 2.86 (1H, H 2 ), 1.18 (3H, C2C H 3 ), 3.77 (1H, C3C H ), 1.84 (1H, H4), 1.05 (C4C H 3 ), 3.61 (1H, C5C H ), 1.39 (3H, C6C H 3 ), 3.54 (1H, 6OMe), 1.59, 1.38 (2H, C7C H 2 ), 3.88 (1H, C8C H ), 1.01 (3H, C8C H 3 ), 2.68 (1H, C10 C H ), 1.20 (3H, C10C H 3 ), 3.78 (1H, C11C H ), 1.19 (3H, C12C H 3 ), 5.10 (1H, C13C H ), 1.95, 1.49 (2H, C14C H 2 ), 0.85 (3H, C15C H 3 ), 2.05, 1.95 (C17C H 3 ), 4.42 (1H, C1′C H ), 3.13 (1H, C2′C H ), 0.10 (9H, 2″OTMS), 2.51 (1H, C3′C H ), 2.21 (6H, C3′N(C H 3 ) 2 ), 1.64, 1.16 (2H, C4′C H 2 ), 3.64 (1H, C5′CH), 1.15 (3H, C6′C H 3 ), 4.90 (1H, C1″C H ), 2.34, 1.50 (2H, C2″C H 2 ), 3.31 (3H, C3″OC H 3 ), 1.15 (3H, C3″C H 3 ), 3.14 (1H, C4″C H ), 0.15 (9H, 4″OTMS), 4.22 (1H, C5″C H , 1.21 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.8 (C═O), 45.3 (C2), 16.0 (C2 Me), 78.0 (C3), 39.5 (C4), 9.7 (C4 Me), 78.8 (C5), 79.1 (C6), 20.1 (C6 Me), 54.0 (6OMe), 38.2 (C7), 28.7 (C8), 18.9 (C8 Me), 179.5 (C9, C═N), 33.1 (C10), 14.8 (C10 Me), 70.2 (C11), 73.9 (C12), 16.1 (C12 Me), 76.7 (C13), 21.2 (C14), 10.5 (C15), 163.4 (C16), 25.5, 18.4 (C17CH 3 ), 102.5 (C1′), 73.3 (C2′), 1.0 (C2′OSi(C H 3 ) 3 ), 65.1 (C3′), 41.0 (C3′NMe), 29.5 (C4′), 67.1 (C5′), 22.2 (C6′), 96.1 (C1″), 35.8 (C2″), 73.1 (C3″), 49.7 (C3″OMe), 21.9 (C3″Me), 80.8 (C4″), 0.8 (C4″OSiC H hd 3 ) 3 ), 65.1 (C5″), 19.4 (C6″) MS (m/z): 946 [M+H] +
Example 3(c)
Erythromycin A 6-O-methyl-9-isopropylidene azine
Erythromycin A 2′,4″-bis-O-trimethylsilyl-6-O-methyl-9-isopropylidene azine (0.7 g; 0.74 mmol) was dissolved in THF and 1M TBAF/THF solution (3.78 ml; 3.78 mmol) was added. The mixture was stirred at room temperature for 2h. The mixture was evaporated to dryness and the residue partitioned between EtOAc and 5% Aq NaOH solution. The organic layer was separated, dried (MgSO 4 ) and evaporated in vacuo to give a white solid 0.5 g (84%).
1Hnmr (500 MHz, CDCl 3 ), d: 2.90 (1H, H2), 1.20 (3H, C2C H 3 ), 3.75 (1H, C3C H ), 1.95 (1H, H4), 1.08 (C4C H 3 ), 3.66 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 2.96 (1H, 6OMe), 1.62, 1.54 (2H, C7C H 2 ), 3.89 (1H, C8C H ), 1.01 (3H, C8C H 3 ), 2.67 (1H, C10 C H , 1.19 (3H, C10C H 3 ), 3.76 (1H, C11C H ), 5.62 (11OH) 1.16 (3H, C12C H 3 ), 3.38 (12H), 5.11 (1H, C13C H ), 1.95, 1.48 (2H, C14C H 2 ), 0.84 (3H, C15C H 3 ), 2.06, 1.95 (C17C H 3 ), 4.46 (1H, C1′C H ), 3.24 (1H, C2′C H ), 2.50 (1H, C3′C H ), 2.35 (6H, C3′N(C H 3 )2), 1.73, 1.24 (2H, C4′C H 2 ), 3.50 (1H, C5′C H ), 1.23 (3H, C6′C H 3 ), 4.93 (1H, Cl″C H ), 2.35, 1.58 (2H, C2″C H 2 ), 3.33 (3H, C3″OC H 3 ), 1.25 (3H, C3″C H 3 ), 3.02 (1H, C4″C H ), 4.01 (1H, C5″C H ), 1.29 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl3), d: 175.4 (C═O), 45.1 (C2), 16.1 (C2 Me), 78.4 (C3), 39.0 (C4), 9.2 (C4 Me), 80.3 (C5), 78.8 (C6), 20.0 (C6 Me), 50.9 (6OMe), 37.8 (C7), 28.8 (C8), 19.0 (C8 Me), 179.5 (C9, C ═N), 33.0 (C10), 14.9 (C10Me), 70.3 (C11), 74.0 (C12), 16.0 (C12 Me), 76.9 (C13), 21.1 (C14), 10.6 (C15), 163.6 (C16), 25.5, 18.5 (C17C H 3 ), 102.6 (C1′), 71.1 (C2′), 65.5 (C3′), 40.3 (C3′NMe), 29.2 (C4′), 68.5 (C5′), 21.4 (C6′), 96.0 (C1″), 34.9 (C2″), 72.7 (C3″), 49.5 (C3″OMe), 21.5 (C3″Me), 77.9 (C4″), 65.7 (C5″), 18.6 (C6″).
MS (m/z): 802 [M+H] +
Example 3 (d)
Erythromycin A 6-O-methyl-9-oxime
Erythromycin A 6-O-methyl-9-isopropylidene azine (100 mg; 0.125 mmol) was dissolved in i-PrOH (5 ml) and 50% Aq NH 2 OH (5 ml) and AcOH (2 drops) were added. The mixture was heated at reflux overnight. The resulting solution was evaporated in vacuo and the residue was partitioned between EtOAc and 5% NaOH. The organic layer was separated, washed with brine, dried (MgSO 4 ) and evaporated in vacuo. The white residue was slurried with ACN, the suspended solid was filtered off and the filtrate evaporated to dryness to yield a white solid 89 mg (94%).
MS (m/z): 763 [M+H] +
Example 3(e)
6-O-methyl Erythromycin A
Erythromycin A 6-O-methyl-9-oxime (35 mg; 0.046 mmol) from the above example was dissolved in i-PrOH (2 ml) and H 2 O (3 ml) and sodium bisulfite (33 mg; .0174 mmol; 3.8eq) was added. The mixture was heated at reflux for 6 h, then evaporated to dryness, partitioned between ethyl acetate and 5% NaOH. The organic layer was dried (MgSO 4 ) and evaporated to give a white solid 25 mg (74%). 1 Hnmr (500 MHz, CDCl 3 ), d: 2.89 (1H, H2), 1.20 (3H, C2C H 3 ), 3.77 (1H, C3C H ), 1.92 (1H, H4), 1.10 (C4C H 3 ), 3.67 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 3.04 (3H, C6OCH 3 ), 1.85, 1.72 (2H, C7C H 2 ), 2.59 (1H, C8C H ), 1.13 (3H, C8C H 3 ), 3.00 (1H, C10C H ), 1.13 (3H, C10C H 3 ), 3.77 (1H, C11C H ), 1.12 (3H, C12C H 3 ), 5.05 (1H, C13C H ), 1.92, 1.47 (2H, C14C H 2 ), 0.84 (3H, C15C H 3 ), 4.44 (1H, C1′C H ), 3.19 (1H, C2′C H ), 2.42 (1H, C3′C H ), 2.29 (6H, C3′N(C H 3 )2), 1.66, 1.22 (2H, C4′C H 2 ), 3.49 (1H, C5′C H ), 1.23 (3H, C6′C H 3 ), 4.93 (1H, C1″C H ), 2.37, 1.59 (2H, C2″C H 2 ), 3.33 (3H, C3″OC H 3 ), 1.25 (3H, C3″C H 3 ), 3.03 (1H, C4″C H ), 4.01 (1H, C5″C H ), 1.31 (3H, C6″C H 3 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.8 (C═O), 45.1 (C2), 15.9 (C2 Me), 78.4 (C3), 39.2 (C4), 9.1 (C4Me), 80.8 (C5), 78.4 (C6), 19.7 (C6Me), 39.3 (C7), 45.2 (C8), 18.0 (C8Me), 220.9 (C9, C═O), 37.2 (C10), 12.3 (C10 Me), 69.1 (C11), 74.3 (C12), 15.9 (C12Me), 76.6 (C13), 21.0 (C14), 10.6 (C15), 102.7 (C1′), 71.0 (C2′), 65.6 (C3′), 40.3 (C3′NMe), 28.9 (C4′), 68.7 (C5′), 21.5 (C6′), 96.1 (C1″), 34.9 (C2″), 72.7 (C3″), 49.5 (C3″OMe), 21.4 (C3″Me), 77.9 (C4″), 65.8 (C5″), 18.7 (C6″).
MS (m/z): FAB 748 [M+H] +
MS (m/z): 748 [M+H] +
Example 4 (a)
Erythromycin A 9-cyclohexylidene azine
Erythromycin A hydrazone (10 g; 13.37 mmol) from Example 1 (a) was suspended in MeCN (70 ml) and IPCH ketal (10 ml) and formic acid (2 ml) were added. The resulting mixture was stirred at ambient temperature overnight The solution was basifzfed to pH>9 with 5% NaOH, the organic layer was separated, dried (MgSO 4 ) and evaporated in vacuo to give a white solid (10.925 g; 99%).
1 Hnmr (500 MHz, CDCl 3 ), d: 2.92 (1H, H2), 1.18 (3H, C2C H 3 ), 4.03 (1H, C3C H ), 2.06 (1H, H4), 1.11 (C4C H 3 ), 3.62 (1H, C5C H ), 1.47 (3H, C6C H 3 ), 2.94 (1H, 6O H ), 1.69, 1.51 (2H, C7C H 2 ), 3.43 (1H, C8C H ), 1.02 (3H, C8C H 3 ), 2.73 (1H, C10C H ), 1.21 (3H, C10C H 3 ), 3.72 (1H, C11C H ), 5.32 (1H, 11H), 1.13 (3H, C12C H 3 ), 3.19 (1H, 12H), 5.14 (1H, C13C H ), 1.91, 1.47 (2H, C14C H 2 ), 0.83 (3H, C15C H 3 ), 4.45 (1H, Cl′C1′C H ), 3.25 (1H, C2′C H ), 2.52 (1H, C3′C H ), 2.35 (6H, C3′N(C H 3 ) 2 ), 1.73, 1.25 (2H, C4′C H 2 ), 3.51 (1H, C5′C H ), 1.22 (3H, C6′C H 3 ), 4.92 (1H, C1″C H ), 2.34, 1.58 (2H, C2″C H 2 ), 3.31 (3H, C3″OC H 3 ), 1.24 (3H, C3″C H 3 ), 3.03 (1H, C4″C H ), 2.24 (9H, 4″OH), 4.02 (1H, C5″C H ), 1.30 (3H, C6″C H 3 ), 2.45, 2.27, 2.33, 1.72, 1.64, 1.59 (cyclohexyl C H 2 ).
13 Cnmr (125 MHz, CDCl3), d: 174.7 (C═O), 44.6 (C2), 16.3 (C2 Me), 80.2 (C3), 38.5 (C4), 9.3 (C4Me), 83.3 (C5), 75.2 (C6), 27.0 (C6Me), 38.5 (C7), 29.2 (C8), 18.7 (C8Me), 178.5 (C9, C ═N), 33.0 (C10), 14.2 (C10 Me), 70.8 (C11), 74.3 (C12), 16.1 (C12Me), 76.7 (C13), 21.0 (C14), 10.6 (C15), 102.7 (C1′), 71.1 (C2′), 65.6 (C3′), 40.3 (C3′NMe), 29.2 (C4′), 68.5 (C5′), 21.5 (C6′), 96.3 (C1″), 35.2 (C2″), 72.7 (C3″), 49.4 (C3″OMe), 21.3 (C3″Me), 77.9 (C4″), 65.6 (C5″), 18.6 (C6″), 168.6 (C1″), 35.6, 28.3, 27.3, 26.2, 25.7 (cyclohexyl CH 2 ).
MS (m/z): 828 [M+H] +
Example 4(b)
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-cyclohexylidene azine
Erythromycin A 9-cyclohexylidene azine (2.0 g; 2.42 mmol) was dissolved in MeCN (40 ml) and HMDS (20 g) was added. The mixture became immediately cloudy, and was stirred at ambient temperature over the weekend. The resulting mixture was basified with 5% NaOH, the organic layer was separated, dried (MgSO 4 ) and evaporated in vacuo to give a white solid 2.065 g; 88%).
1 Hnmr (500 MHz, CDCl 3 ), d: 2.88 (1H, H2), 1.17 (3H, C2C H 3 ), 4.19 (1H, C3C H ), 1.97 (1H, H4), 1.11 (C4C H 3 ), 3.61 (1H, C5C H ), 1.45 (3H, C6C H 3 ), 2.79 (1H, 6OH), 1.70, 1.50 (2H, C7C H 2 ), 3.48 (1H, C8C H ), 1.03 (3H, C8C H 3 ), 2.76 (1H, C10 C H ), 1.23 (3H, C10C H 3 ), 3.73 (1H, C11C H ), 5.29 (1H, 1 11OH), 1.18 (3H, C12C H 3 ), 3.21 (1H, 12 H ), 5.12 (1H, C13C H ), 1.93, 1.50 (2H, C14C H 2 ), 0.86 (3H, C15C H 3 ), 4.39 (1H, C1′C H ), 3.17 (1H, C2′C H ), 0.11 (9H, 2″OTMS), 2.54 (1H, C3′C H ), 2.23 (6H, C3′N(C H 3 ) 2 ), 1.66, 1.19 (2H, C4′C H 2 ), 3.63 (1H, C5′C H ), 1.17 (3H, C6′C H 3 ), 4.88 (1H, C1″C H ), 2.36, 1.50 (2H, C2″C H 2 ), 3.31 (3H, C3″OC H 3 ), 1.15 (3H, C3″C H 3 ), 3.17 (1H, C4″C H ), 0.15 (9H, 4″OTMS), 4.24 (1H, C5″C H ), 1.23 (3H, C6″C H 3 ), 2.44, 2.28, 2.34, 1.77, 1.63 (cyclohexyl C H 2 ).
13 Cnmr (125 MHz, CDCl 3 ), d: 175.4 (C═O), 44.7 (C2), 16.1 (C2 Me), 79.8 (C3), 39.5 (C4), 9.7 (C4Me), 81.3 (C5), 75.5 (C6), 27.2 (C6Me), 39.2 (C7), 29.1 (C8), 18.7 (C8Me), 178.3 (C9, C═N), 33.1 (C10), 14.2 (C10Me), 70.9 (C 11), 74.4 (C12), 16.1 (C12Me), 76.7 (C13), 21.1 (C14), 10.7 (C15), 102.6 (C1′), 73.5 (C2′), 1.0 (C2′OSi(C H 3 ) 3 ), 65.2 (C3′), 41.0 (C3′NMe), 29.8 (C4′), 67.6 (C5′), 21.8 (C6′), 96.7 (C1″), 36.0 (C2″), 73.2 (C3″), 49.7 (C3″OMe), 22.2 (C3″Me), 81.0 (C4″), 0.9 (C4′OSi(C H 3 ) 3 ), 65.0 (C5″), 19.4 (C6″), 168.2 (C1″′), 35.6, 28.4, 27.3, 26.2, 25.8 (cyclohexyl C H 2 ).
MS (m/z): 972 [M+H] +
Example 4(c)
Erythromycin A 2′,4″-bis-O-trimethylsilyl-6-O-methyl-9-cyclohexylidene azine
Erythromycin A 2′,4″-bis-O-trimethylsilyl-9-cyclohexylidene azine (1.0 g; 1.02 mmol) was dissolved in a 1:1 mixture of THF/DMSO (10 ml) and cooled to 5° C. Methyl iodide (0.36 ml; 5.82 mmol) and KOH (0.217 g; 3.88 mmol) were added and the mixture was stirred at 5° C. for 90 min. The reaction was quenched by the addition of aq methylamine (1 ml). Saturated NaCl was added and the resulting mixture extracted with TBME. The organic layer was washed with saturated NaCl solution then dried (MgSO 4 ) and evaporated in vacuo to give a white solid (0.85 g; 84%).
MS (m/z): 986 [M+H] +
1Hnmr (500 MHz, CDCl3) 5.57 (11OH). 5.10 (C13CH), 4.90 (C1″CH), 4.42 (C1′CH) 4.22 (C5″CH), 4.09 (C3CH), 3.30 (C3″OMe), 2.96 (C6OMe), 2.90 (H2), 2.22 (C3′NMe2), 2.44, 2.28, 2.34, 1.77, 1.63 (cyclohexyl CH2), 1.49 (C14CH2), 1.40 (C6 Me), 1.21 (C6″CH3), 1.20 (C10CH3), 1.19 (C12Me), 1.18 C2 Me), 1.15 (C3″Me), 1.05 (C4CH3), 1.01 (C8CH3), 0.85 (Cl5CH3), 0.10 (2′OTMS), 0.15 (4″OTMS) 13Cnrnr (125 MHz, CDC13) 175.9 (C═O), 45.5 (C2), 79.0 (C3), 39.5 (C4), 9.5 (C4 Me), 80.9 (C5), 79.0 (C6), 19.4 (C6Me), 39.2 (C7), 45.5 (C8), 19.4 (C8Me), 36.0 (C10), 14.9 (C10Me), 70.2 (C11), 73.9 (C12), 16.1 (C12Me), 76.6 (C13), 21.0 (C14), 10.6 (C15), 102.6 (C1′), 73.3 (C2′), 65.1 (C3′), 40.7 (C3′NMe), 29.5 (C4′), 67.2 (C5′), 21.4 (C6′), 96.0 (C1″), 35.8 (C2″), 73.9 (C3″), 78.0 (C4″), 65.1 (C5″), 18.8 (C6″)
Example 4(d)
Erythromycin A 6-O-methyl-9-cyclohexylidene azine
Erythromycin A 2′,4″-bis-O-trimethylsilyl-6-O-methyl-9-cyclohexylidene azine (4 g; 4.06 mmol) was dissolved in THF (40 ml) and 1 M TBAF/THF solution (20.70 ml; 20.70 mmol) was added. The mixture was stirred at room temperature for 2h. The mixture was evaporated to dryness and the residue partitioned between EtOAc and 5% Aq NaOH solution. The organic layer was separated, dried (MgSO 4 ) and evaporated in vacuo to give a white solid 2.9 g (85%). MS (m/z): FAB 842 [M+H] +
Example 4(e)
6-O-methyl Ery A
Erythromycin-6-O-methyl-9-cyclohexylidene azine (200 mg; 238 mmol) was dissolved in i-PrOH (10 nmL) and 50%aq NH 2 OH (10 mL) and AcOH (4 drops) were added. The mixture was heated at reflux overnight. The resulting solution was evaporated to dryness and the residue was partitioned between EtOAc and 5% NaOH. The organic layer was separated and dried (MgSO 4 ) and evaporated in vacuo giving erythromycin A 6-O-methyl-9-oxime as an off-white solid 146 mg (81%) Spectral and chromatographic data were identical with Example 3d. The oxime (50 mg; 0.0657 mmol) was dissolved in IPA (2 mL) and H 2 O (3 mL) and sodium bisulfite (47 mg; 0.249 mnmol; 3.8 eq) was added. The mixture was heated at reflux overnight then evaporated in vacuo and partitioned between EtOAc and 5% NaOH. The organic layer was separated, dried (MgSO4) and evaporated in vacuo to give a white solid 55 mg.
1Hnmr (500 MHz, CDCl 3 ), d: 2.89 (1H, H2), 1.20 (3H, C2C H 3 ), 3.77 (1H, C3C H ), 1.92 (1H, H4), 1.10 (C4C H 3 ), 3.67 (1H, C5C H ), 1.41 (3H, C6C H 3 ), 3.04 (3H, C6OC H 3 ), 1.85, 1.72 (2H, C7C H 2 ), 2.59 (1H, C8C H ), 1.13 (3H, C8C H 3 ), 3.00 (1H, C10C H ), 1.13 (3H, C10C H 3 ), 3.77 (1H, C11C H ), 1.12 (3H, C12C H 3 ), 5.05 (1H, C13C H ), 1.92, 1.47 (2H, C14C H 2 ), 0.84 (3H, C15C H 3 ), 4.44 (1H, C1′C H ), 3.19 (1H, C2′C H ), 2.42 (1H, C3′C H ), 2.29 (6H, C3′N(C H 3 ) 2 ), 1.66, 1.22 (2H, C4′C H 2 ), 3.49 (1H, C5′C H , 1.23 (3H, C6′C H 3 ), 4.93 (1H, C1 ″C H ), 2.37, 1.59 (2H, C2″C H 2 ), 3.33 (3H, C3″OC H 3 ), 1.25 (3H, C3″C H 3 ), 3.03 (1H, C4-″C H ), 4.01 (1H, C5″CH), 1.31 (3H, C6″C H 3 ). 13 Cnmr (125 MHz, CDCl 3 ), d: 175.8 (C═O), 45.1 (C2), 15.9 (C2 Me), 78.4 (C3), 39.2 (C4), 9.1 (C4Me), 80.8 (C5), 78.4 (C6), 19.7 (C6Me), 39.3 (C7), 45.2 (C8), 18.0 (C8Me), 220.9 3 (C9, C═O), 37.2 (C10), 12.3 (C10Me), 69.1 (C15), 74.3 (C12), 15.9 (C12Me), 76.6 (C13), 21.0 (C14), 10.6 (C15), 102.7 (C1′), 71.0 (C2′), 65.6 (C3′), 40.3 (C3′NMe), 28.9 (C4′), 68.7 (C5′), 21.5 (C6′), 96.1 (C1″), 34.9 (C2″), 72.7 (C3″), 49.5 (C3″OMe), 21.4 (C3″Me), 77.9 (C4″), 65.8 (C5″), 18.7 (C6″).
MS (m/z): FAB 748 [M+H] + | Disclosed are 9-hydrazone erythromycin and 9-azine erythromycin derivatives and the processes for making the same. The compounds are useful intermediates for conversion into 6-O-alkyl erythromycin. Also disclosed are the processes for converting the compounds into 6-O-alkyl erythromycin. | 2 |
PRIORITY
The present application claims priority to U.S. Provisional Application No. 61/505,399 filed Jul. 7, 2011, the disclosure of which is incorporated herein by reference.
FIELD
The present disclosure relates to a system for gas exchange chambers, and more particularly to method and system for a controlled source gas exchange chamber with automated testing capability.
BACKGROUND AND SUMMARY
Gas exchange chambers are used to monitor static states of plants and the composition of the immediately surrounding air once plants are allowed to exchange gasses with supplied ambient air.
According to an embodiment of the present disclosure, an open gas exchange measuring system is disclosed including: a controller; a test chamber; a customizable gas source that provides gas to the test chamber, the gas source being controlled by the controller, the controller providing for customizing characteristics of the gas provided to the test chamber as desired; and a measuring device.
According to another embodiment of the present disclosure, a gas measuring system is disclosed including: a controller; a gas source; a measuring device; a plurality of fixed lower test chamber portions, each lower test chamber portion having a position suitable for receiving a test subject, and a moveable upper test chamber portion. The moveable upper portion being sealable to each of the plurality of lower test chambers; the controller controlling the composition of gas supplied to upper test chamber portion from the gas source, the controller controlling the position of the moveable upper test chamber.
According to another embodiment of the present disclosure, a gas measuring system is provided including: a test chamber; a gas source; a first test chamber portion; a second test chamber portion; a third test chamber portion; and a controller including a data storage member. The data storage member including a plurality of instructions thereon that, when invoked by the controller, cause the system to perform the steps of: placing the second test chamber portion in contact with the first test chamber portion; customizing gas flow from the gas source to the first test chamber portion to provide a first gas to the first test chamber portion via the second test chamber portion, the first gas having a first set of desired customized characteristics; moving the second test chamber out of contact with the first test chamber portion and into contact with the third test chamber portion; and customizing gas flow from the gas source to the to the third test chamber portion to provide a second gas to the third test chamber portion via the second test chamber portion, the second gas having a second set of desired customized characteristics.
BRIEF DESCRIPTION OF THE DRAWINGS
The above-mentioned and other features of the disclosure, and the manner of attaining them, will become more apparent and the disclosure itself will be better understood by reference to the following description taken in conjunction with the accompanying drawings, wherein:
FIG. 1 illustrates a schematic of a system for supplying controlled gasses to one or more of a plurality of plants under test and for measuring gas exchange response;
FIG. 2 illustrates a chamber usable in the system of FIG. 1 .
Corresponding reference characters indicate corresponding parts throughout the several views. The exemplifications set out herein illustrate exemplary embodiments of the invention, and such exemplifications are not to be construed as limiting the scope of the invention in any manner.
DETAILED DESCRIPTION
The embodiments disclosed herein are not intended to be exhaustive or to limit the disclosure to the precise forms disclosed in the following detailed description. Rather, the embodiments are chosen and described so that others skilled in the art may utilize their teachings.
Referring to FIG. 1 , an exemplary gas exchange monitoring system 10 is shown. System 10 includes supply buffers 12 , supply pumps 14 , manifold 16 , gas analyzer 18 , chamber 20 , and computer 22 . System 10 is shown as an open system gas exchange chamber, however, it is envisioned that the concepts and teachings herein are also applicable to closed system gas exchange chambers.
Supply buffers 12 are gas repositories. Supply buffers 12 are provided with differing gaseous elements having differing physical/chemical characteristics. Buffers 12 are customizable according to tests desired to be carried out. By way of example, four buffers 12 are supplied with varying amounts of CO 2 , O 2 , ambient air, trace gasses (such as ethylene), or any other desired gaseous elements. Each buffer 12 is adjusted by temperature, vapor pressure deficit (VPD), and any other desired characteristic. To this end, heaters, coolers, humidifiers, dehumidifiers, and other condition altering devices 24 are coupled to each buffer 12 .
Supply pumps 14 are coupled to each supply buffer 12 . Supply pumps 14 control both the amount of gas supplied from each buffer 12 , the flow rate of supplied gas, and in closed systems, the pressure at which the gas is supplied.
Supply pumps 14 supply gas from buffers 12 to manifold 16 . Inputs 26 of manifold 16 are coupled to respective outputs of supply pumps 14 . Manifold 16 combines the outputs from pumps 14 . Manifold 16 further includes valves therein. Accordingly, system 10 is not restricted to supplying only the gaseous states of buffers 12 , but rather combinations of the gaseous states of buffers 12 are achieved by varying the amounts of gas taken and mixed from each buffer 12 . Outlet 28 of manifold 16 is supplied to inlet 30 of chamber 20 and to reference inlet 32 of gas analyzer 18 .
Gas analyzer 18 is, in the present example, a CO 2 /H 2 O analyzer, such as one produced by Li-Cor Biosciences with the model number of LI-7000. It should be appreciated that analyzer 18 is chosen to provide for monitoring of the chemicals/variables/features under study.
In addition to receiving input from manifold outlet 28 , analyzer 18 receives input from outlet 34 of chamber 20 at sample inlet 33 . Accordingly, analyzer 18 is provided with the gasses being supplied to chamber 20 and the gasses that result from the input gas being subjected to the presence of test subjects 36 (illustrated as plants) within chamber 20 . Chamber outlet 34 is vented to ambient air in opens systems but could be vented to a collection chamber (not shown) or re-circulated in other embodiments.
Computer 22 is coupled to analyzer 18 to allow monitoring, saving, and manipulation of the data provided by analyzer 18 . As previously discussed, analyzer 18 includes at least two channels (from manifold outlet 28 and chamber outlet 34 ). Computer 22 includes programming to interface with analyzer 18 and allow graphical presentation of the data received therefrom. Computer 22 is further coupled to chamber 20 , supply pumps 14 , and manifold 16 . Computer 22 is able to control supply pumps 14 and manifold 16 to provide desired gas compositions to chamber 20 at desired times.
Chamber 20 is shown in more detail in FIG. 2 . Chamber 20 includes a fixed lower portion 38 and a moveable upper portion 40 . Lower portion 38 is actually one of a plurality of identical lower portions 38 . Moveable upper portion 40 is selectively associated with a plurality of lower portions 38 . Embodiments are envisioned where system 10 also includes a plurality of upper portions 40 . Test subjects 36 (or plants) under test are located within each lower portion 38 .
Lower portions 38 are shown as being cylindrical and presenting an interface portion 42 on an upper lip. While other shapes and orientations are envisioned, lower portions within a system 10 are all similarly shaped and oriented. For example, another such orientation results in lower portions 38 being disposed within the floor or retractable into a floor such that interface portion 42 is flush with the floor. As shown, adjacent lower portions 38 are separated from each other by a defined inter-pot distance 44 . The provided example provides that the inter-pot distance between lower portions 38 is constant for all lower portions 38 . FIG. 2 shows two lower portions 38 that are separated in a left-right direction of the page. It should be appreciated that lower portions 38 are envisioned as being laid out in a grid of two dimensions (rows and columns), not shown. Accordingly, inter-pot distance 44 corresponds to a column width. The grid also has a row width that may or may not be equal to inter-pot distance 44 (column width). Embodiments are envisioned where the row width is equal to inter-pot distance 44 . In the present example, inter-pot distance 44 is chosen such that the effect that tests being conducted at one lower portion 38 have minimal or no effect on tests being run at a second lower portion 38 . Embodiments are also envisioned where inter-pot distance 44 is chosen to approximate the distance between plants that would be experienced in a planted field. Inter-pot distance 44 also allows for chamber 20 to fully enclose test subject 36 without enclosing any of adjacent test subject 36 . Inter-pot distance 44 is also chosen to allow desired airflow once chamber 20 encloses test subject 36 . Additionally, embodiments are envisioned wherein the floor of lower portion 38 includes a scale. The scale is coupled to computer 22 and provides an electronic weight signal thereto. Additionally, while chamber 20 is discussed as only enclosing one test subject 36 at a time, embodiments are envisioned where multiple test subjects 36 are enclosed together. In such embodiments, test subjects 36 enclosed together are usually of the same type.
Upper portion 40 includes base 62 , movement linkages 46 , input/output interfaces 48 , motors 50 , spools 52 , cables 54 , drape 56 , support rings 58 , and interface portion 60 . Base 62 is shown as being a flat square member on which the balance of the pieces of upper portion 40 are mounted. However, it should be appreciated that the depiction of base 62 is conceptual. An actual base 62 is shaped and sized to support and provide mounting surfaces for the balance of the pieces of upper portion 40 . Base 62 is coupled to movement linkages 46 . Movement linkages 46 suspend upper portion 40 above lower portion 38 and test subjects 36 . Movement linkages 46 further allow upper portion 40 to be moved and successively centered over multiple lower portions 38 . Computer 20 is coupled to motors (not shown) that control the movement of movement linkages 46 .
Base 62 provides an air-tight coupling to drape 56 . Drape 56 is impervious to gas and illustratively made of a cylinder of flexible transparent plastic of a ply that can sustain repeated flexing. A plurality of support rings 58 is disposed on the interior of drape 56 at varying heights to maintain an internal opening diameter within drape 56 . Alternatively, support rings 58 can take the form of a continual helix that approximates a spring.
Lower end 64 of drape 56 is coupled to interface portion 60 . Interface portion 60 is sized to sealingly interface with interface portion 42 of lower portion 38 . The seal of interface portion 42 to fixed lower portion 38 is air-tight to provide a volume within drape 56 that is gaseously isolated from the surrounding air.
Cables 54 are coupled to lower end 64 of drape and extend vertically upwardly to base 62 . Cables 54 are further coupled to spools 52 that are coupled to and rotatable relative to base 62 . Spools 52 are coupled to motors 50 that selectively turn spools to wind and unwind cables 54 from spools 52 . Such winding and unwinding of cables 54 from spools 52 raise and lower, respectively, the interface portion 60 and drape 56 . Accordingly, drape 56 is provided a lowered position where interface portion 60 seals to interface portion 42 . Likewise, drape 56 is provided a raised position where interface portion 60 is disengaged from interface portion 42 and lower end 64 is raised to a height higher than the height of test subjects 36 . The raised position of drape 56 causes/allows flexing of drape 56 to a compressed orientation.
Alternatively, embodiments are envisioned where harder plastic is used for drape 56 . Such embodiments use the harder plastic in a telescoping manner such that collapsed (retracted) and expanded orientations are again provided. Air-tight seals are provided between telescoping portions to maintain the seal of chamber 20 .
Input/output interfaces 48 are linked to chamber inlet 30 and chamber outlet 34 , respectively. Input/output interfaces 48 are positioned on base 62 such that they are in communication with the interior volume of drape 56 . Thus, when drape 56 is in its lowered position that defines an isolated volume, the isolated volume is in gaseous communication with manifold 16 and with gas analyzer 18 . Inlet 30 is also envisioned to have specific ducting to provide that input gas is evenly distributed within chamber 20 . Similarly, outlet 34 is positioned and ducted to maximize the likelihood that gas being sampled is gas that has interacted with test subjects 36 as opposed to coming directly from inlet 30 .
In use, a location with an array containing a plurality of lower portions 38 is provided. Test subjects 36 are placed in one or more lower portions 38 .
Computer 22 is provided with a plurality of data structures to control system 10 to conduct one or more experiments on test subjects 36 . As noted, lower portions 38 are arranged with a set inter-pot distance 44 . Regardless of the exact layout, computer 22 is provided data that indicates the positioning of the lower portions 38 . The positioning data may be in the form of an existing data file or in the form of user input. Additionally, for any specific experiment run, computer 22 is provided data indicative of which lower portions 38 are in use (that contain a test subjects 36 ).
Computer 22 is likewise provided with data structures that contain instructions for movement linkages 46 (and the motors that control them) to cause moveable upper portion 40 to be positioned above each fixed lower portion 38 .
Computer 22 accesses the data structure for the experiment protocol to determine which fixed lower portion 38 are in use for the protocol being executed. Similarly, the experiment protocol provides data indicative of what physical/chemical characteristics are provided by each of supply buffers 12 . Computer 22 is provided with data structures that contain instructions for operation of supply pumps 14 and manifold 16 to cause desired gas compositions to be supplied to chamber 20 .
Thus, with proper setup of lower portions 38 with test subjects 36 and of supply buffers 14 , an experiment can be developed and carried out with a plurality of similar or different subjects (test subjects 36 ). Computer 22 is provided with a data structure that indicates the particular gas compositions to be supplied to each test subjects 36 . Thus, for “n” test subjects 36 , the experiment protocol provides a treatment to be carried out.
Once the experiment protocol data structure is invoked, computer 22 first positions moveable upper portion 40 over the first fixed lower portion 38 and test subjects 36 by emitting signals to instruct movement linkages 46 to move appropriately. Computer 22 then emits instructions to activate motors 50 and unspool cables 54 until interface portion 60 engages interface portion 42 . Computer 22 then emits signals that selectively cause activation of supply pumps 14 and manifold 16 to produce the desired gaseous composition at inlet 30 . As previously noted, the gaseous composition is likewise provided to gas analyzer 18 . Accordingly, to the extent that the signals emitted from computer 22 do not produce an exactly precise gaseous composition, gas analyzer 18 is able to test the composition actually emitting from manifold 16 .
Gas analyzer 18 is also testing the gas composition leaving chamber 20 via outlet 34 . By taking successive readings, gas analyzer 18 is able to detect and report to computer 22 changes in gas composition over time. Differences in gas composition between inlet 30 and outlet 34 are presumed to be an artifact of the interaction between the provided gas and test subjects 36 . Furthermore, in that the supplied gas is customizable, system 10 is able to measure the reactions/responses that plants have to changes in the provided atmosphere (gases). System 10 is further able to monitor transient reactions of test subjects 36 (and the resulting changes in output gasses) to the atmospheric changes. In one embodiment where system 10 monitors transient reactions, gas analyzer 18 focuses on readings between when the chamber is able to effect a full chamber air exchange and when the test subjects 36 are able to assume a new gas exchange equilibrium with the new gaseous composition. One such example is to focus on the times between 20 and 70 seconds after a new gas composition is provided to test subjects 36 . In the embodiment, 20 seconds is relevant in that it is the time that the chamber needs to effect an air change within the chamber (3 exchanges per minute=1 change in 20 seconds). Additionally, 70 seconds is relevant in that test subjects 36 are believed to reach a gas exchange equilibrium 50 seconds after application of the new gaseous composition. Once the experiment is completed and the data is gathered, computer 22 emits signals to cause moveable upper portion 40 to move on to a second fixed lower portion 38 and test subjects 36 .
To this end, drape 56 is retracted via motors 50 , spools 52 , and cables 54 . Upper portion 40 is then moved above second fixed lower portion 38 and test subjects 36 . Drape 56 is then lowered via motors 50 , spools 52 , and cables 54 such that interface portion 42 engages interface portion 60 of the second fixed lower portion 38 . Again, computer 22 emits instructions to cause activation of supply pumps 14 and manifold 16 to produce the desired gaseous composition at inlet 30 . It should be appreciated that the gas composition supplied to the second fixed lower portion 38 can be the same or different than the gas composition supplied to the first fixed lower portion 38 .
Additionally, the gas composition can be changed in the midst of a trial (i.e. the trial may be testing the plant response to going from a first gas composition to a second gas composition). Such gas composition changes include but are not limited to increases/decreases in atmospheric vapor pressure deficit (VPD), temperature, CO 2 concentration, and consecutive changes (raising or lowering) these variables. Furthermore, monitoring output changes relative to the input changes provide transient reaction data. The transient reaction data can provide information about the performance of the test subjects 36 in terms of change in canopy gas exchange capacity, instantaneous water use efficiency in reaction to environmental stimulus, and traits such as drought tolerance, nitrogen use efficiency, tolerance to flood stress, photosynthetic capacity, and any others desired and detectable via the described devices and methods. Additional properties, such as canopy transpiration, transpiration rate, net CO 2 assimilation, CO 2 assimilation rate, net CO 2 assimilation rate, CO 2 concentration, Irradiance, Leaf Stomatal Conductance, and leaf Surface Temperature can also be determined. Accordingly, system 10 provides a high throughput system for screening for traits such as, but not limited to, drought tolerance and nitrogen use efficiency.
While this invention has been described as having preferred designs, the present invention can be further modified within the spirit and scope of this disclosure. This application is therefore intended to cover any variations, uses, or adaptations of the invention using its general principles. Further, this application is intended to cover such departures from the present disclosure as come within known or customary practice in the art to which this disclosure pertains and which fall within the limits of the appended claims. | A gas measurement system is provided that includes a mechanism for customizing gas supplied to the system. The system further includes a plurality of test locations that can be serviced by a common vessel portion and common sampling and testing infrastructure. The system further includes a controller that is able to control the customization of the supply gas and the location of the common vessel portion. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
Not applicable.
BACKGROUND OF THE INVENTION
The present invention is related to cut protection gloves made of a textile material with a cut resistant fibre.
Such cut protection gloves can protect the user against cutting injuries of all kinds, for instance when working with sharp-edged objects, tools, knives or other blades. The protection effect against cuttings is achieved in that special cut resistant fibres are contained in the material from which the glove is made.
Different materials are used as the cut resistant fibres, which have enhanced cut resistance compared with other frequently processed fibres, those from cotton, polyamide or polyester for instance. Fibres of glass, aramides, high density polyethylene, high density polymers or metals are frequently used. A multiplicity of such cut resistant fibres is known from the European Patent Document EP 0 435 889 B2, the entire contents of which is incorporated herein by reference, among others.
In order to provide effective cutting protection, the cut resistant fibres and the textile materials made there from have a series of properties, which adversely affect a high wearing comfort of cut protection gloves made from these materials. Among these, there is a high stiffness in particular, which can limit the perfect fit, the dexterity and the tactility, and also a humidity take-up ability which is significantly reduced with respect to other textile materials, which can lead to increased sweating and to an unfavourable microclimate in the gloves. When using filament yarns in particular, the skin's sensorial ability is also deteriorated, because textile materials made from such yarns have a relatively smooth and closed surface structure, which sits closer to the skin than other textiles with a more open structure with small fibres sticking out. Thus, such cut protection gloves might stick more to skin which is wetted by sweat.
In the context of the generation of sweat taking place more severely with gloves from synthetic fibres, problems through bacterial contamination and the generation of disagreeable odour's might also occur.
Just with cut protection gloves for the professional field, which have frequently to be worn over longer periods of time, a high wearing comfort is very important. Insufficient comfort properties may even lead to safety risks in the practical use, because in this case, the users tend to do off the cut protection gloves for a while.
In order to increase the wearing comfort of cut protection gloves, it is known to combine the textile material having the cut resistant fibres with an additional textile material. The additional textile material is comprised of fibres with better comfort properties, of cotton for instance, and is processed to a liner or to an inside cladding. This liner is glued or sewed together with the cut protection material, so that the inner sides of such a glove are formed by the material with the better comfort properties. Various realisations of an inner cladding for gloves are known from the German utility document 20 2005 008 041 U1, the entire contents of which is incorporated herein by reference.
Based on this, it is the objective of the present invention to provide a cut protection glove made of a textile material having a cut resistant fibre, which can be manufactured in a simple way and which has improved comfort properties.
BRIEF SUMMARY OF THE INVENTION
The cut protection glove of the present invention made from a textile material with a cut resistant fibre is characterized in that the textile material incorporates a bamboo fibre. The textile material can be an arbitrary material made up of fibres, a knitted fabric, a woven fabric or a tissue for instance, also designated with the general expression cloth in the common language. The textile material incorporates a cut resistant fibre, i.e. a fibre with an enhanced cut resistance compared to ordinary fibre materials. In this, the textile material and the cut resistant fibre are processed into one single textile material. Different cut resistant fibres can also be combined in the textile material. The content of the cut resistant fibre in the textile material is as high that even the textile material has an increased cut resistance. In addition, the textile material has a bamboo fibre. Thus, the cut resistant fibre and the bamboo fibre are processed into one single textile material. The material can also have further fibres. It is also possible that the cut protection glove has a further textile material, in the form of a reinforcement or a cushion, for instance.
Bamboo fibres are cellulose fibres which are obtained from the bamboo plant. The bamboo fibres are known as bast fibres and also as regenerated bamboo fibres. A regenerated bamboo fibre is preferably used. These fibres are very soft and have particularly good grip properties, which are comparable to those of viscose or silk. The fibres have a gloss giving the appearance of high value, and they are particularly long-living and wear-resistant. In addition, the fibres are particularly lightweight. Furthermore, the bamboo fibres have a particularly high take-up ability for humidity through their particular micro-structure, and they can release the once taken-up humidity particularly quickly again. Through the combination of the bamboo fibres with the cut resistant fibres into one single textile material, even a cut protection glove made from this material has substantially improved comfort properties. Through the take-up ability for humidity, the glove does not feel wet to the touch even at relatively strong sweating. At the same time, a pleasant cooling effect is achieved by the quick release of the humidity ingested by the textile material, which counter-acts excessive sweating. Due to the natural anti-bacterial properties of the bamboo plants, the same are normally cultivated without using pesticides, and a chemical antibacterial finish can be omitted. The danger of allergic reactions or skin irritations is substantially reduced by this. These favourable antibacterial properties remain conserved even after washing several times.
A further advantage of the combination of a cut resistant fibre with a bamboo fibre into one single textile material is that the production of the gloves made from this material is greatly simplified, because gluing or sewing together of different layer's of material is not necessary.
In a particularly preferred embodiment, the textile material has a cut resistant yarn with the cut resistant fibre and a bamboo yarn with the bamboo fibre. Thus, the cut resistant fibres and the bamboo fibres are each processed into one separate yarn, from which the textile material is produced by machine-knitting, weaving or entangling. The use of different yarns permits a particularly simple and targeted combination of the two fibres by conventional processing methods, like knitting machines, for instance. In doing so, the composition of the textile material can be influenced by corresponding processing of the two yarns, so that the content of cut resistant fibres is increased in the particularly stressed portions of the cut protection glove with respect to less stressed portions, for instance.
In a further preferred embodiment of the present invention, the inner side of the cut protection glove is formed by the bamboo yarn. Thus, it is provided to process the two yarns with each other to the textile material such that the material facing the skin is essentially the bamboo yarn. The advantageous comfort properties of the bamboo yarn, the pleasant skin feeling in particular, take optimally advantage by doing so. Preferably, the outer side of the cut protection glove is substantially formed by the cut resistant yarn, or it has an increased content of this yarn.
According to a further preferred embodiment of the present invention, the bamboo yarn and the cut resistant yarn form a two-layer knitted fabric. In this it is provided that an inner layer of the knitted fabric is formed by the bamboo yarn and an outer layer by the cut resistant yarn. Both yarns are combined with each other in the manufacture of the knitted fabric and are intricated into each other. By a suitable knitting method, one single textile material with the advantageous two-layer structure is produced in doing so, the so-called “double-face-structure”.
In a further preferred embodiment of the present invention, the bamboo yarn forms a cladding. The cladding is located on the inner side of the cut protection glove.
In a further preferred embodiment of the present invention, the cut resistant fibre is processed in a core-sheath-yarn. By doing so, the properties of the cut resistant yarn formed by the core-sheath-yarn can be improved themselves.
According to a further preferred embodiment of the present invention, the core of the core-sheath-yarn is comprised of metal or a glass fibre. In this case, the core of the core-sheath-yarn contributes in particular to the enhanced cut resistance.
In a further preferred embodiment of the present invention, the sheath of the core-sheath-yarn is comprised of polyester, polyamide, high-density polyethylene, aramide or cellulose yarn. Thus, depending on the selection of the material, the sheath of the core-sheath-yarn can contribute to the enhanced cut resistance, when using aramide for instance, or the sheath can improve the comfort properties of the cut resistant yarn, by a wrapping with cellulose yarns for instance.
According to a further preferred embodiment of the present invention, the sheath of the core-sheath-yam is comprised of the bamboo fibre. In this case, the advantageous properties of the bamboo fibre can be integrated into the cut resistant yarn. Thus, it is possible to produce the textile fabric from one single yarn, which contains the cut resistant fibre as well as the bamboo fibre. However, it is also possible to process further bamboo fibres or a bamboo yarn made from the same to the textile material, in addition to a core-sheath-yam with the bamboo fibre which has an increased cut resistance. Thus, there are a manifold of possibilities to adapt the properties of the textile material to the respective requirements, the compromise between optimum wearing comfort and optimum cut protection properties in particular.
In a further preferred embodiment of the present invention, the textile material has a coating on the outer side. Preferably, the coating is comprised of nitrile, chloroprene or polyurethane. By means of the coating, additional protection properties can be imparted to the cut protection glove, tightness against liquids and resistance against chemicals for instance. The nitrile coating is liquid-tight and it may cover the cut protection glove completely or partially. Preferably, only the inner hand, the fingers and the thumb are provided with the coating, whereas the back of the hand remains uncoated. By doing so, the breathing activity of the cut protection glove is maintained at least partially.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
In the following, the present invention is explained in more detail by means of an example of its realisation depicted in three figures.
FIG. 1 shows a cut protection glove of the present invention;
FIG. 2 shows a cut-out of the textile material of the cut protection glove of FIG. 1 , in a cross-section.
FIG. 3 shows a core-sheath-yarn which is used as a cut resistant yarn in the textile material according to FIG. 2 , in a cross-section.
DETAILED DESCRIPTION OF THE INVENTION
While this invention may be embodied in many different forms, there are described in detail herein a specific preferred embodiment of the invention. This description is an exemplification of the principles of the invention and is not intended to limit the invention to the particular embodiment illustrated
FIG. 1 shows a cut protection glove of the present invention, which has been knitted completely on a special glove knitting machine. The meshwork produced by the knitting machine has a “single-Jersey”-bonding. The subdivision of the knitting machine is thirteen gauge, i.e. thirteen needles per inch. Such knitting machines can process or knit together, respectively, different yarns from different yarn rolls at the same time. The structure depicted in FIG. 2 can be achieved by a special yarn guiding in this.
The material of the knitted glove depicted in a cross-section in FIG. 2 is comprised of three layers. The middle layer 14 has a cut resistant yarn on the side facing the hand, and it is knitted together with a further material layer 16 comprised of the bamboo yarn. The two layers 14 and 16 form a double-layer knitted fabric produced by the knitting machine. By means of a dipping method, the outer side of the glove is provided with a nitrile coating 18 after the knitting process. The inner side 17 of the double-layer knitted fabric facing the skin is formed exclusively by the bamboo yarn processed to the inner layer 16 . The bamboo yarn has a metric number of Nm 50/1. During the knitting process, the bamboo yarn is entangled with the cut resistant yarn of the outer material layer 14 of the knitted fabric.
In FIG. 3 , the structure of the core-sheath-yarn 20 is sketched out, which serves as a cut resistant yarn for the outer material layer 14 of the knitted fabric. The core-sheath-yarn 20 has a core 22 , which is comprised of a glass-fibre multifilament with a degree of fineness of 110 dtex. This glass fibre multifilament core is enveloped by a sheathing 24 of polyester yarn, two polyester yarns of fineness degree 110 dtex being used for this.
The above disclosure is intended to be illustrative and not exhaustive. This description will suggest many variations and alternatives to one of ordinary skill in this art. All these alternatives and variations are intended to be included within the scope of the claims where the term “comprising” means “including, but not limited to”. Those familiar with the art may recognize other equivalents to the specific embodiments described herein which equivalents are also intended to be encompassed by the claims.
Further, the particular features presented in the dependent claims can be combined with each other in other manners within the scope of the invention such that the invention should be recognized as also specifically directed to other embodiments having any other possible combination of the features of the dependent claims. For instance, for purposes of claim publication, any dependent claim which follows should be taken as alternatively written in a multiple dependent form from all prior claims which possess all antecedents referenced in such dependent claim if such multiple dependent format is an accepted format within the jurisdiction (e.g., each claim depending directly from claim 1 should be alternatively taken as depending from all previous claims). In jurisdictions where multiple dependent claim formats are restricted, the following dependent claims should each be also taken as alternatively written in each singly dependent claim format which creates a dependency from a prior antecedent-possessing claim other than the specific claim listed in such dependent claim below.
This completes the description of the preferred and alternate embodiments of the invention. Those skilled in the art may recognize other equivalents to the specific embodiment described herein which equivalents are intended to be encompassed by the claims attached hereto. | A cut protection glove, made of a textile material having a cut resistant fibre, characterized in that the textile material has a bamboo fibre. | 3 |
TECHNICAL FIELD
[0001] This application has priority rights of Japanese patent application No. 2013-19628, filed Feb. 4, 2013, which is herein incorporated by references.
[0002] The present invention relates to a method for forming a multilayer coating film, especially, a method for forming a multilayer coating film of applying a first water-based base coating composition, a second water-based base coating composition and a clear coating composition by so-called wet on wet coating and simultaneously heating and curing the three layers.
BACKGROUND OF THE INVENTION
[0003] An automobile coating basically includes sequentially applying an electrodeposition coating film, a first base coating film (also called a water-based intermediate coating film), a second base coating film (also called a color base coating film) and a clear coating film on a steel plate as a coating material. In such a coating, there are two methods; one method includes multiple heating and curing per forming a composed coating film, and the other method includes a simultaneously curing of layered multiple coating films. In these methods, the method including a simultaneously curing of layered multiple coating films can omit a heating and curing step and provide an energy-saving coating, and is advantageous.
[0004] As a method for a simultaneously curing of layered multiple coating films, a three-coat and one-bake coating by successively forming a first base coating film, a second base coating film and a clear coating film by wet on wet coating and simultaneously heating and curing is performed. However, a conventional three-coat and one-bake coating requires a preliminary drying step (so-called a preheating step) by drying, for example, at 60 to 100° C. for 2 to 20 minutes after a first base coating composition is applied, especially in case that a water-base coating composition is used. The preheat step can prevent occurrence of mixing of two coating film layers (mixing of layers). The mixing of layers is generated when a second water-based coating film is formed on an uncured first water-based coating film immediately after the first water-based coating film is formed, and water and/or an organic solvent in an uncured second water-based coating film is (are) moved to the uncured first water-based coating film. The mixing of layers frequently deteriorates film appearance of resulting multilayer coating film.
[0005] On the other hand, further omission of a preheat step after forming an uncured first water-based base coating film has been required in view of further requirement for reduce burden on the environment such as reduction of CO 2 emission and energy saving. By contrast, resulting multilayer coating film requires no less excellent film appearance than ones obtained by conventional coating method.
[0006] JP 2001-009357 A (Patent Document 1) describes a coating formation method for successively forming an intermediate coating film using a water-based intermediate coating composition, a metallic base coating film using a water-based metallic base coating composition, and a clear coating film using a clear coating composition on a substrate, characterized in that the water-based intermediate coating composition and/or the water-based metallic base coating composition comprise(s) a polycarbodiimide compound and an aqueous resin having carboxyl group (claim 1 ). Patent Document 1 also discloses that the method can provide formation of multilayer coating film with excellent appearance by controlling affinity and bleeding in the interlayers between respectively neighboring layers in the case where the water-based intermediate coating composition and the base coating composition are successively formed on a substrate. However, the coating formation method includes a preheat step of 80° C. for 5 minutes (paragraph [0101]).
[0007] JP 2004-358462 A (Patent Document 2) describes a method for forming a multilayer coating film characterized by sequentially applying a water-based intermediate coating composition, a water-based base coating composition and a clear coating composition on an electrodeposition coating film by wet-on-wet coating and simultaneously heating and curing them, wherein the water-based intermediate coating composition comprises an acrylic resin emulsion having a glass transition temperature of −50 to 20° C., a solid acid value of 2 to 60 mgKOH/g and a solid hydroxyl value of 10 to 120 mgKOH/g, a urethane resin emulsion having a solid acid value of 5 to 50 mgKOH/g, and a curing agent (claim 1 ). Patent Document 2 also discloses that the method can provide a multilayer coating film having excellent smoothness of its surface with effectively preventing mixing of layers between an intermediate coating film and a base coating film. However, the method for forming a multilayer coating film also includes a preheat step of 80° C. for 5 minutes after applying the water-based intermediate coating composition (paragraph [0117]).
[0008] JP 2009-262002 A (Patent Document 3) describes a method for forming a multilayer coating film characterized by sequentially applying a water-based intermediate coating composition, a water-based base coating composition and a clear coating composition on an electrodeposition coating film by wet-on-wet coating and simultaneously heating and curing them, wherein the water-based intermediate coating composition comprises an acrylic resin emulsion having a solid hydroxyl value of 50 to 120 and a solid acid value of 20 to 60 mgKOH/g, a completely alkyl-etherified melamine resin having alkyl side chain group with 1-4 carbon atoms, and a carbodiimide compound (claim 1 ). Patent Document 3 also discloses that the method can prevent mixing of layers between an intermediate coating film and a base coating film in a three-coat-one-bake coating method. However, the method for forming a multilayer coating film also includes a preheat step of 80° C. for 5 minutes (paragraph [0162]).
[0009] JP 2012-116879 A (Patent Document 4) describes a water-based intermediate coating composition containing an acrylic resin emulsion and a curing agent, wherein addition of an aqueous dispersion of dimer acid derivative to the water-based intermediate coating composition provides formation of pseudo-crystalline state in the water-based intermediate coating composition and hydrophobicity to prevent transfer of solvents including water from a water-based base coating composition. However, in the method of Patent Document 4, complete deletion of a preheat step is difficult, and mixing of layers or sagging occurs.
PRIOR ART DOCUMENTS
Patent Documents
[0000]
Patent Document 1: JP 2001-009357 A
Patent Document 2: JP 2004-358462 A
Patent Document 3: JP 2009-262002 A
Patent Document 4: JP 2012-116879 A
SUMMARY OF THE INVENTION
Problems to be Resolved by the Invention
[0014] The present invention is intended to solve the conventional problems described above. For more details, a main object of the present invention is to provide constituents of a first water-based base coating composition and a second water-based base coating composition without defects such as mixing of layers in a wet-on-wet coating including applying the first water-based base coating composition to form an uncured first water-based base coating film and applying the second water-based base coating composition thereon without curing.
Means of Solving the Problems
[0015] The present invention provides a method for forming a multilayer coating film including the steps of;
[0016] (1) applying a first water-based base coating composition on a surface of a coating material to form an uncured first water-based base coating film,
[0017] (2) applying a second water-based base coating composition on the uncured first water-based base coating film to form an uncured second water-based base coating film,
[0018] (3) applying a clear coating composition on the uncured second water-based base coating film to form an uncured clear coating film, and
[0019] (4) simultaneously heating and curing the uncured first water-based base coating film, the uncured second water-based base coating film and the uncured clear coating film formed in the steps (1), (2) and (3) to form a multilayer coating film, wherein
[0020] the first water-based base coating composition comprises a hydrophilic associated type viscosity agent, and
[0021] the second water-based base coating composition comprises a film forming resin, and the film forming resin comprises an acrylic emulsion resin (A), a water soluble acrylic resin (B) and a water soluble polyester resin (C), wherein
[0022] a rate represented by the following formula:
[0000] ( A )/( A+B+C ) wherein (A) is a resin solid content by mass of the acrylic emulsion resin (A), and (A+B+C) is a total resin solid content by mass of the acrylic emulsion resin (A), the water soluble acrylic resin (B) and the water soluble polyester resin (C),
is from 40% to 60% expressed in percentage, in which the above problems can be solved.
[0024] The prevent invention may also include the embodiments described below:
[0025] the hydrophilic associated viscosity agent in the first water-based base coating composition is a polyamide type viscosity agent,
[0026] the acrylic emulsion resin (A) in the second water-based base coating composition comprises a single layered acrylic emulsion resin (a) and a core-shell type acrylic emulsion resin (b),
[0027] a viscosity at a temperature of 20° C. of the uncured first water-based base coating film after applying the second water-based base coating composition is from 45 to 100 Pa·s at a shear rate of 0.01/s, and
[0028] no heating or drying step is included between the step (1) and the step (2).
Advantageous Effect of the Invention
[0029] Inventors of the present invention have studied a coating method without defects such as sagging and mixing of layers even if the coating method includes no preheat step (pre-drying step) in the process of application of a first water-based base coating composition to form an uncured first water-based base coating film and applying a second water-based base coating composition on the uncured first water-based base coating film. A viscosity of a first water-based base coating film at 20° C. without preheat is from 50 to 100 Pa·s at a shear rate of 0.01/s. By contrast, a viscosity of a first water-based base coating film after a preheat step is more than 10,000 Pa·s at a shear rate of 0.01/s. The inventors tried to find correlation between sagging after application of a second water-based coating composition and a viscosity of a first water-based coating film on the assumption that a maximum viscosity of a first water-based coating film without preheat is about 150 Pa·s at a shear rate of 0.01/s. However, they did not find the correlation.
[0030] Therefore, the inventors measured a viscosity of a first water-based coating film after application of a second water-based coating composition in a special manner and investigated correlation between sagging and the viscosity. They have found correlation that high viscosity of a first water-based coating film after application of a second water-based coating composition provides decrease of sagging. For more detail, they have found that sagging frequently occurs when the viscosity at 20° C. and a shear rate of 0.01/s is less than 45 Pa·s, however generation of sagging significantly decrease when the viscosity is not less than 45 Pa·s. The present invention is achieved based on the above findings. The present invention is achieved by addition of a hydrophilic associated type viscosity agent to a first water-based coating composition and selecting constituents of a second water-based coating composition for preventing transfer of water in order to increasing viscosity of a first water-based coating film at the time of after application of a second water-based coating composition.
[0031] Application of constituents of the first water-based base coating composition and the second water-based base coating composition according to the present invention in a coating method by so-called wet-on-wet coating can prevent defects such as sagging or mixing of layers even if the coating step does not include a preheat step (in other words, a pre-drying step). The present invention can achieve omission of preheat step which is conventionally-required in making a multilayer coating film using water-based coating compositions. The present invention can provide energy omission required in a preheat step, furthermore, omission of coating time and coating step.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0032] First Water-Based Base Coating Composition
[0033] A first water-based base coating composition according to the present invention generally contains an acrylic emulsion resin and a curing agent. The first water-based base coating composition according to the present invention further contains a hydrophilic associated type viscosity agent. The first water-based base coating composition may contain a pigment and optional additives.
[0034] Acrylic Emulsion Resin
[0035] A glass transition temperature (Tg) of an acrylic resin which is composed of an acrylic emulsion resin may preferably be from −20° C. to 60° C., more preferably from −10° C. to 50° C., most preferably from 0° C. to 40° C. When a glass transition temperature (Tg) of the resin is less than −20° C., a mechanical strength of a coating film may deteriorate and a chipping resistance may lower. On the other hand, when a glass transition temperature (Tg) of the resin is more than 60° C., an impact resistance may deteriorate because of hardness and brittleness of a coating film and chipping resistance may lower. A glass transition temperature (Tg) of the acrylic emulsion resin can be calculated based on known glass transition temperatures (Tg) of monomer(s) and/or homopolymer(s) and amount rates of them.
[0036] A solid acid value of the acrylic resin which is composed of the acrylic emulsion resin may preferably be from 2 to 60 mgKOH/g, more preferably from 5 to 50 mgKOH/g. When a solid acid value of the resin is less than 2 mgKOH/g, storage stability, mechanical stability and freezing stability and the like of the acrylic emulsion resin or the first water-based base coating composition containing the acrylic emulsion resin may lower, and various strength of a coating film, chipping resistance and water resistance of a coating film may lower because of lack of sufficient curing property in a curing reaction for a curing agent such as a melamine resin. On the other hand, when a solid acid value of the resin is more than 60 mgKOH/g, polymerization stability of the resin or water resistance of a resulting coating film may lower. A solid acid value of the acrylic resin can be adjusted by selecting a kind of monomer(s) and/or an amount of monomer(s) to obtain a solid acid value in the range described above. As described below, it is important to use a monomer having carboxyl group as an ethylenically unsaturated monomer having acid group (ii). It may be preferable that an amount of the monomer having carboxyl group contained in the ethylenically unsaturated monomer having acid group (ii) is not less than 50% by mass, more preferably not less than 80% by mass.
[0037] A solid hydroxyl value of the acrylic resin which is composed of the acrylic emulsion resin may preferably be from 10 to 120 mgKOH/g, more preferably from 20 to 100 mgKOH/g. When a solid hydroxyl value of the resin is less than 10 mgKOH/g, mechanical strength of a coating film may lower, chipping resistance may lower and water resistance and solvent resistance may lower due to insufficient curing property in a curing reaction for a curing agent. On the other hand, when a solid hydroxyl value of the resin is more than 120 mgKOH/g, water resistance of a resulting coating film may lower, and various strength of a coating film, in particular, chipping resistance, solvent resistance and water resistance may lower, because compatibility with a curing agent becomes lower and strain of a coating film and unevenness of curing reaction may occur.
[0038] A solid acid value and a solid hydroxyl value of the acrylic resin can be calculated based on a solid acid value and a solid hydroxyl value of a monomer mixture used in a preparation of the resin.
[0039] The acrylic emulsion resin contained in the first water-based base coating composition used in the method for forming a multilayer coating film can be obtained by emulsion polymerization of a monomer mixture containing a (meth)acrylic acid alkyl ester (1), an ethylenically unsaturated monomer having acid group (ii) and an ethylenically unsaturated monomer having hydroxyl group (iii). Each compounds (i) to (iii) as a component in the monomer mixture exemplified below may be a singular compound or in an appropriate combination of two or more compounds.
[0040] The (meth)acrylic acid alkyl ester (i) is used as a component for making a main backbone of the acrylic emulsion resin. An example of the (meth)acrylic acid alkyl ester (i) includes methyl (meth)acrylate, ethyl (meth)acrylate, propyl (meth)acrylate, n-butyl (meth)acrylate, isobutyl (meth)acrylate, t-butyl (meth)acrylate, hexyl (meth)acrylate, 2-ethyl hexyl (meth)acrylate, octyl (meth)acrylate, nonyl (meth)acrylate, decyl (meth)acrylate, dodecyl (meth)acrylate, (meta)acrylic acid stearyl ester and the like. In this specification, for example, the term “methyl (meta)acrylate” represents methyl acrylate and methyl methacrylate.
[0041] The ethylenically unsaturated monomer having acid group (ii) is used as a component for improving various performance such as storage stability, mechanical stability and freezing stability of resulting acrylic emulsion resin and promoting curing reaction for a curing agent such as a melamine resin. The acid group may preferably be selected from carboxylic acid group, sulfonate group, phosphate group and the like. The most preferable acid group is carboxylic acid group in view of improving property of various stabilities described above and promoting property of curing reaction.
[0042] An ethylenically unsaturated monomer having carboxylic acid group includes, for example, acrylic acid, methacrylic acid, crotonic acid, isocrotonic acid, ethacrynic acid, propyl acrylic acid, isopropyl acrylic acid, itaconic acid, maleic anhydride, fumaric acid, and the like. An ethylenically unsaturated monomer having sulfonate group includes, for example, p-vinyl benzene sulfonic acid, p-acrylamide propane sulfonic acid, t-butyl acrylamide sulfonic acid, and the like. An ethylenically unsaturated monomer having phosphate group includes, for example, LIGHT-ESTER PM (produced by KYOEISHA CHEMICAL Co., LTD.), such as monophosphate of 2-hydroxyethyl acrylate, monophosphate of 2-hydroxypropyl methacrylate, and the like.
[0043] The ethylenically unsaturated monomer having hydroxyl group (iii) can provide the resulting acrylic resin emulsion with a hydrophilicity due to the hydroxyl group therein. The resulting acrylic resin emulsion can improve its application workability and anti-freezing stability of the resulting coating composition containing the emulsion, and provide the resulting resin emulsion with a curing reactivity to the curing agent such as melamine resin, isocyanate or the like.
[0044] The ethylenically unsaturated monomer having hydroxyl group (iii) includes, for example, 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate, N-methylolacrylamide, allyl alcohol, epsilon-caprolactone-modified acrylic monomer and the like.
[0045] The epsilon-caprolactone-modified acrylic monomer includes, for example, Placcel FA-1, Placcel FA-2, Placcel FA-3, Placcel FA-4, Placcel FA-5, Placcel FM-1, Placcel FM-2, Placcel FM-3, Placcel FM-4 and Placcel FM-5, which are produced by DAICEL CHEMICAL INDUSTRIES, LTD, etc.
[0046] The monomer mixture which is used for preparation of the acrylic emulsion resin may optionally contain at least one monomer selected from the group consisting of styrene monomers, (meth)acrylonitriles and (meth)acrylamides, in addition to the above monomers (i) to (iii). The styrene monomers include styrene and alpha-methyl styrene and the like.
[0047] Herein, the monomer mixture may further contain a crosslinkable monomer such as an ethylenically unsaturated monomer having carbonyl group, a monomer having hydrolyzable and polymerizable silyl group, various polyfunctional vinyl monomers and the like. In case that such a crosslinkable monomer is contained, the resulting acrylic emulsion resin becomes self-crosslinkable.
[0048] The ethylenically unsaturated monomer having carbonyl group includes, for example, a monomer having keto group such as acrolein, diacetone (meta)acrylamide, acetoacetoxyethyl (meta)acrylate, formyl styrol, alkyl vinyl ketone having 4-7 carbon atom (for example, methyl vinyl ketone, ethyl vinyl ketone, butyl vinyl ketone) and the like. In these monomers, diacetone (meta)acrylamide may preferably be used.
[0049] The monomer having hydrolyzable and polymerizable silyl group includes, for example, a monomer having alkoxysilyl group such as gamma-(meta)acryloxy propyl methyl dimethoxysilane, gamma-(meta)acryloxy propyl methyl diethoxysilane, gamma-(meta)acryloxy propyl triethoxysilane and the like.
[0050] The polyfunctional vinyl monomer is a compound having two or more radical-polymerizable ethylenically unsaturated groups. The polyfunctional vinyl monomer includes, for example, a divinyl compound such as divinylbenzene, ethyleneglycol di(meta)acrylate, hexanediol di(meta)acrylate, polyethyleneglycol di(meta)acrylate, allyl(meta)acrylate, 1,4-butanediol di(meta)acrylate, 1,6-hexane di(meta)acrylate, neopentylglycol di(meta)acrylate, pentaerythritol di(meta)acrylate and the like; and pentaerythritol tri(meta)acrylate, trimethylol propan tri(meta)acrylate, dipentaerythritol hexa(meta)acrylate and the like.
[0051] The acrylic emulsion resin used in the method for forming a multilayer coating film according to the present invention can be prepared by emulsion polymerization of a monomer mixture containing the above components (i) to (iii). The emulsion polymerization (an emulsion copolymerization) can be carried out, in the presence of a radical polymerization initiator and an emulsifier, by heating the above-described monomer mixture in an aqueous medium with stirring. A reaction temperature may preferably be within a range of, for example, from 30 to 100° C., and reaction time may preferably be within a range of, for example, from 1 to 10 hours. The reaction temperature can be controlled by adding dropwise a portion or whole of the monomer mixture or the pre-emulsified monomer mixture into a reaction vessel containing water and an emulsifier.
[0052] As the radical polymerization initiator, a known initiator for an emulsion polymerization to prepare a conventional acrylic resin may be used. The initiator includes, for example, a water-soluble free radical polymerization initiator, for example, a persulfate compound such as potassium persulfate, sodium persulfate, ammonium persulfate; an azo type compound such as 4,4′-azobis (4-cyanovaleric acid); and the like, which is used in an aqueous solution. A preferable initiator may include, for example, in an aqueous solution, a so-called redox initiator in a combination of an oxidizing agent, such as potassium persulfate, sodium persulfate, ammonium persulfate, hydrogen peroxide and the like; and a reducing agent, such as sodium hydrogensulfite, sodium thiosulfate, Rongalit, ascrobic acid and the like.
[0053] The emulsifier includes an anionic or nonionic emulsifier selected from amphipathic compounds, each of which has a hydrocarbon group having 6 or more of carbon atoms and a hydrophilic moiety, such as a carboxylate, a sulfonate or a sulfuric acid partial ester, in one molecule. The anionic emulsifier includes an alkaline metal salt or an ammonium salt of a half ester of sulfuric acid with an alkyl phenol or a fatty alcohol; an alkaline metal salt or an ammonium salt of an alkyl sulfonate or an allyl sulfonate; an alkaline metal salt or an ammonium salt of a half ester of sulfuric acid with a polyoxyethylene alkylphenyl ether, a polyoxyethylene alkyl ether or a polyoxyethylene allyl ether, etc. The nonionic emulsifier includes a polyoxyethylene alkylphenyl ether, a polyoxyethylene alkyl ether, a polyoxyethylene allyl ether, etc. The emulsifier may include another emulsifiers other than these conventional anionic and nonionic emulsifiers, such as various anionic and nonionic reactive emulsifiers, each of which has, in its molecule, a radically polymerizable unsaturated double bond-containing group, such as an acrylic group, a methacrylic group, a propenyl group, an allyl group, an allyl ether group, a maleic group, etc. An appropriate single emulsifier may be used alone, or two or more emulsifiers may be used in an appropriate combination.
[0054] Herein, during the emulsion polymerization, preferably, an auxiliary agent (a chain-transfer agent) in order to control the molecular weight may appropriately be used depending on the polymerization conditions, such as a mercaptan compound, a lower alcohol, alpha-methyl styrene dimer or the like. The auxiliary agent (a chain-transfer agent) can accelerate the emulsion polymerization, accelerate the formation of the resulting coating film with a smooth and uniform surface, and improve an adherence to the substrate, therefore, may preferably be used.
[0055] Herein, the emulsion polymerization includes any conventional polymerization, such as a polymerization including a continuous uniform addition of a monomer at a single stage; a core-shell polymerization including a multi-stage monomer feeding; a power feed polymerization wherein formulation of the monomers to be fed is continuously altered during the polymerization, etc. In case that a conventional continuous uniform addition of a monomer at a single stage is used, a single layered acrylic emulsion resin can be obtained. In case that a core-shell polymerization including a multi-stage monomer feeding is used, a core-shell type acrylic emulsion resin can be obtained.
[0056] The above-described emulsion polymerization can provide the acrylic emulsion resin which can be used in the present invention. A weight average molecular weight of an acrylic resin which composes the acrylic emulsion resin is generally, but is not particularly limited to, a range of from about 50000 to about 1000000, and a preferable range of from about 100000 to about 800000. The weight average molecular weight as used herein is a value measured by GPC (gel permeation chromatography) method, as a calculated reduced value with a polystyrene standard.
[0057] In the present invention, a base compound can be added to the resulting acrylic emulsion resin to improve dispersion stability of the acrylic emulsion resin by neutralization of all or partial carboxylic acid groups therein. The base compound includes, for example, ammonia compounds, various amine compounds, alkali metals and the like.
[0058] Curing Agent
[0059] The first water-based base composition may preferably contain a curing agent. The curing agent is not particularly limited, as long as the curing agent can provide curing reaction for the acrylic emulsion resin and can be added to the first water-based base coating composition. The curing agent includes, for example, a melamine resin, a blocked isocyanate resin, an oxazoline compound or a carbodiimide compound and the like. These curing agents may be used alone, or two or more curing agents may be used in an appropriate combination.
[0060] The melamine resin is not particularly limited, and a conventional melamine resin used as a curing agent can be used. The melamine resin may preferably be, for example, an alkyl-etherified melamine which is an alkyl-etherified compound, more preferably be a melamine resin which is substituted by methoxy group and/or butoxy group. A concrete example of the melamine resin includes,
[0000] a melamine resin having mere methoxy group(s) such as Cymel 325, Cymel 327, Cymel 370, Mycoat 723;
a melamine resin having both of methoxy group(s) and butoxy group(s) such as Cymel 202, Cymel 204, Cymel 211, Cymel 232, Cymel 235, Cymel 236, Cymel 238, Cymel 251, Cymel 254, Cymel 266, Cymel 267, Cymel 285 (each of them is a product name, produced by Nihon Cytec Industries Inc.);
a melamine resin having mere butoxy group(s) such as Mycoat 506 (product name, produced by Mitsui Cytec Industries Inc.), U-Van 20N60, U-Van 20SE (each of them is a product name, produced by Mitsui Chemicals, Inc.)
These melamine resins may be used alone, or two or more melamine resins may be used in a combination.
[0061] In these melamine resins, Cymel 211, Cymel 251, Cymel 285, Cymel 325, Cymel 327, Mycoat 723 may more preferably be used.
[0062] The blocked isocyanate resin is a prepared by blocking a polyisocyanate compound with a blocking agent. The polyisocyanate compound is not limited as long as the compound has two or more isocyanate groups in one molecular, and may be, for example,
[0000] aliphatic diisocyanates such as hexamethylene diisocyanate (HMDI), trimethylhexamethylene diisocyanate (TMDI) and the like;
aliphatic-cyclic diisocyanates such as isophorone diisocyanate (IPDI) and the like;
aromatic-aliphatic diisocyanates such as xylylene diisocyanate (XDI) and the like;
aromatic diisocyanates such as tolylene diisocyanate (TDI), 4,4-diphenylmethane diisocyanate (MDI) and the like;
hydrogenated diisocyanates such as dimer acid diisocyanate (DDI), hydrogenated TDI (HTDI), hydrogenated XDI (H6XDI), hydrogenated MDI (H12MDI) and the like; and
biurets and nulates thereof, etc. The polyisocyanate compound may be used solely or in combination thereof.
[0063] The blocking agent employed for blocking the polyisocyanate compound is not limited and may include, example,
[0000] an oxime type compound such as methyl ethyl ketoxime, acetoxime, cyclohexanone oxime and the like;
a phenol type compound such as m-cresol, xylenol and the like;
an alcohol type compound such as butanol, 2-ethylhexanol, cyclohexanol, ethyleneglycol monoethyl ether and the like;
a lactam type compound such as epsilon-caprolactam and the like;
a diketone type compound such as diethyl malonate, acetoacetic ester and the like;
a mercaptan compound such as thiophenol and the like;
a urea compound such as thiourea and the like;
an imidazole compound, a carbamic acid and the like.
In these compounds, the oxime type compound, phenol type compound, alcohol type compound, lactam type compound, diketone type compound may preferably be used.
[0064] The oxazoline compound may preferably a compound having two or more 2-oxazoline group, and includes, for example, the following oxazoline compounds and an oxazoline group-containing polymer. The oxazoline compound may be used alone, or two or more compounds may be used in an appropriate combination. The oxazoline compound may be prepared by the following methods of: dehydration reduction of amide alcohol in the presence of a catalyst with heating; synthesis of alkanolamine and nitrile; synthesis of alkanolamine and carboxylic acid; or the like.
[0065] The oxazoline compound may include, for example, 2,2′-bis-(2-oxazoline), 2,2′-methylene-bis-(2-oxazoline), 2,2′-ethylene-bis-(2-oxazoline), 2,2′-trimethylene-bis-(2-oxazoline), 2,2′-tetramethylene-bis-(2-oxazoline), 2,2′-hexamethylene-bis-(2-oxazoline), 2,2′-octamethylene-bis-(2-oxazoline), 2,2′-ethylene-bis-(4,4′-dimethyl-2-oxazoline), 2,2′-p-phenylene-bis-(2-oxazoline), 2,2′-m-phenylene-bis-(2-oxazoline), 2,2′-m-phenylene-bis-(4,4′-dimethyl-2-oxazoline), bis-(2-oxazolinylcyclohexane)sulfide, bis-(2-oxazolinylnorbornane)sulfide and the like. The oxazoline compound may be used alone, or two or more compounds may be used in an appropriate combination.
[0066] The oxazoline group-containing polymer may be prepared by polymerization of addition-polymerizable oxazoline and optional at least one other polymerizable monomer. The addition polymerizable oxazoline may include, for example, 2-vinyl-2-oxazoline, 2-vinyl-4-methyl-2-oxazoline, 2-vinyl-5-methyl-2-oxazoline, 2-isopropenyl-2-oxazoline, 2-isopropenyl-4-methyl-2-oxazoline, 2-isopropenyl-5-ethyl-2-oxazoline and the like. The oxazoline may be used alone, or two or more may be used in an appropriate combination. Above all, 2-isopropenyl-2-oxazoline may more preferably be used in view of industrially easily availability.
[0067] An amount of the addition-polymerizable oxazoline is not limited, and may be 1 mass % or more, based on an amount of the oxazoline group-containing polymer. When an amount of the addition-polymerizable oxazoline is less than mass %, insufficient curing may be obtained and durability and water resistance of a resulting coating film may be deteriorated.
[0068] The other polymerizable monomer is not limited as long as the monomer can react with the addition-polymerizable oxazoline and does not react with a oxazoline group. The other polymerizable monomer includes, for example, (meta)acrylic acid esters such as (meta)acrylic acid methyl, (meta)acrylic acid butyl, (meta)acrylic acid-2-ethyl hexyl and the like;
[0000] unsaturated nitriles such as (meta)acrylonitrile and the like;
unsaturated amides such as (meta)acrylic amide, N-methylol (meta)acrylic amide and the like;
vinyl esters such as vinyl acetate, propionate vinyl and the like;
vinyl ethers such as methyl vinyl ether, ethyl vinyl ether and the like;
alpha-olefins such as ethylene, propylene and the like; halogenated alpha-beta-unsaturated monomers such as vinyl chloride, vinylidene chloride, fluorinated vinyl and the like;
alpha-beta-unsaturated aromatic monomers such as styrene, alpha-methyl styrene and the like; etc. The monomer may be used alone, or two or more may be used in an appropriate combination.
[0069] The oxazoline group-containing polymer may be prepared by polymerization of addition-polymerizable oxazoline and optional at least one other polymerizable monomer, in a conventionally known polymerization method such as a suspension polymerization, a solution polymerization, an emulsification polymerization and the like. A supply form of an oxazoline group-containing compound may include a solution of organic solvent, a solution of aqueous solvent, non-aqua dispersion, emulsion and the like, and is not limited in the above form.
[0070] The carbodiimide includes any carbodiimide compound prepared by any conventional method, such as a carbodiimide generally prepared by a condensation reaction wherein an organic diisocyanate is subjected to a decarboxylation at the isocyanate terminals to produce a polycarbodiimide compound.
[0000] In a preferable embodiment, the preparation of the polycarbodiimide compound includes steps of:
[0071] reacting a polycarbodiimide compound having at least two isocyanate groups in one molecule with a polyol wherein a hydroxyl group presets at the terminal to give a reaction product, wherein molar ratio of the total isocyanate groups of the polycarbodiimide compound to the total hydroxyl groups of the polyol is more than 1; and
[0072] reacting the reaction product with a hydrophilicizing agent having an active hydrogen and a hydrophilic moiety to produce a hydrophilicized carbodiimide compound. Such hydrophilicized carbodiimide compound is preferably used in the present invention.
[0073] The polycarbodiimide compound having at least two isocyanate groups in one molecule includes, but is not particularly limited to, preferably, a carbodiimide compound having an isocyanate group at one terminal and another isocyanate group on the other terminal, which has an excellent reactivity. The carbodiimide compound having at least two isocyanate groups on the both terminals can be prepared by a method known to those skilled in the art, for example, which includes a condensation wherein an organic diisocyanate is subjected to a decarboxylation.
[0074] Hydrophilic Associated Type Viscosity Agent
[0075] A hydrophilic associated type viscosity agent is a viscosity agent having a hydrogen bond between the viscosity agents or between the viscosity agent and a film forming resin, and exerts binding strength (interaction) therefrom. The hydrophilic associated type viscosity agent may include, for example, polyamide type viscosity agent, and a commercially available viscosity agents such as BYK-430 and BYK-431 (product names, all products are manufactured by BYK-Chemie company), Disparlon AQ-580, Disparlon AQ-600, Disparion AQ-607 (product names, all products are manufactured by Kusumoto Chemincals, Ltd.), Thixol W-300, Thixol W-400LP (product names, all products are manufactured by Kyoeisha Chemical Co., Ltd.), and the like.
[0076] The first water-based base coating composition may contain another viscosity agent(s) other than the hydrophilic associated type viscosity agent.
[0000] Another viscosity agent(s) may include a hydrophobic associate type viscosity agent which exerts viscosity derived from interaction of hydrophobic groups (hydrophobic parts) in the molecular, an alkali thickened type viscosity agent, and the like.
The hydrophobic associate type viscosity agent may include, for example, polyvinyl alcohol and polyethylene oxide, and a commercially available product (shown in a product name) such as Adeka nol UH-420, Adeka nol UH-462, Adeka nol UH-472, UH-540, Adeka nol UH-814N (all products are manufactured by Adeka corporation), Primal RH-1020 (manufactured by Rohm and Haas company), Kuraray Poval (manufactured by Kuraray co., ltd.) and the like.
The alkali thickened type viscosity agent may include, for example, a cellulose type such as viscose, methyl cellulose, ethyl cellupose, hydroxyethyl cellulose, and a commercially available product (shown in a product name) such as Tylose MH and Tylose H (all products are manufactured by Hoechst ltd.);
sodium polyacrylate, polyvinyl alcohol, carboxymethyl cellulose, a commercially available product (shown in a product name) such as Primal ASE-60, Primal TT-615, Primal RM-5 (all products are manufactured by Rohm and Haas company), UCAR Polyphobe (manufactured by Union Carbide Corporation) and the like.
[0077] A content of the hydrophilic associated type viscosity agent and another viscosity agent(s) in the first water-based base coating composition may preferably be 0.01 to 20 mass % based on a resin solid of the first water-based base coating composition (a resin solid content of all the resin components in the first water-based base coating composition), more preferably 0.1 to 10 mass %. When the content is less than 0.01 mass %, viscosity control effects may be deteriorated and sagging at coating may occur. When the content is more than 20 mass %, film appearance and coating film performance of the resulting coating film may be deteriorated.
[0078] A solid content ratio of the hydrophilic associated type viscosity agent and another viscosity agent(s) in the first water-based base coating composition may preferably be 100/0 to 50/50 in a ratio of the hydrophilic associated type viscosity agent/another viscosity agent(s), more preferably 100/0 to 80/20. When a ratio of another viscosity agent(s) is more than 50/50, sagging at coating and deterioration of finished appearance of the resulting multilayer coating film may occur.
[0079] The first water-based base coating composition used in the present invention may contain an additional resin component, a pigment-dispersing paste, and another additives in addition to the acrylic emulsion resin, the curing agent and the hydrophilic associated type viscosity agent.
[0080] The additional resin component is not limited and may include, for example, a polyester resin, an acrylic resin, a carbonate resin, an epoxy resin and the like.
[0081] The pigment-dispersing paste may be prepared by pre-dispersing a pigment and a pigment-dispersing agent in a small amount of an aqueous medium. The pigment-dispersing agent is a resin having a structure with a pigment-affinity part and a hydrophilic part. The pigment-affinity part and a hydrophilic part include, for example, a functional group such as nonionic, cationic or anionic groups. The pigment-dispersing agent may have two or more kinds of the functional group.
[0082] The nonionic functional group may include, for example, a hydroxyl group, an amido group, a polyoxyalkylene group and the like. The cationic functional group may include, for example, an amino group, an imino group, a hydrazino group and the like. In addition, the anionic functional group may include a carboxyl group, a sulfone acid group, a phosphate group and the like. The above pigment-dispersing agent may be prepared by a conventional method known in the art.
[0083] The pigment-dispersing agent may preferably be an agent which can disperse a pigment efficiently in a small amount. An example of the pigment-dispersing agent may be a commercially available agent (the following products are shown in a trade name), and may include, for example, an anion-nonion type dispersing agent such as Disperbyk 190, Disperbyk 181, Disperbyk 182, Disperbyk 184 (all products are manufactured by BYK-Chemie company), EFKAPOLYMER 4550 (manufactured by EFKA company); a nonionic dispersing agent such as Solsperse 27000 (manufactured by Avecia Inc.); an anionic dispersing agent such as Solsperse 41000, Solsperse 53095 (all products are manufactured by Avecia Inc.) and the like.
[0084] A number average molecular weight of the pigment-dispersing agent may preferably be in a range of 1,000 to 100,000, more preferably 2,000 to 50,000, most preferably 4,000 to 50,000. When a number average molecular weight is less than 1,000, dispersion stability may be insufficient. When a number average molecular weight is more than 100,000, handling property may be deteriorated due to excessive viscosity.
[0085] The above pigment-dispersing paste may be prepared by mixing and dispersing a pigment and the pigment-dispersing agent in a known method in the art. A content ratio of the pigment-dispersing agent in a preparation of a pigment-dispersing paste may preferably be within a range of 1 to 20 mass % based on a solid content of the pigment-dispersing paste. When a content ratio of the pigment-dispersing agent is less than 1 mass %, dispersion stability of a pigment may deteriorate. When a content ratio of the pigment-dispersing agent is more than 20 mass %, coating film performance of the resulting coating film may be deteriorated. A content ratio may more preferably be within a range of 5 to 15 mass %.
[0086] A pigment is not limited as long as the pigment is a pigment used in a conventional aqueous coating composition. The pigment may preferably be a coloring pigment in view of improvement of weather resistance and procurance of hiding property. A preferable example of the pigment may be titanium dioxide in view of excellent hiding property of color and inexpensiveness.
[0087] An example of the pigment other than titanium dioxide includes, for example, an organic coloring pigment such as an azo chelate-based coloring pigment, an insoluble azo type coloring pigment, a condensed azo type coloring pigment, a phthalocyanine-based coloring pigment, an indigo coloring pigment, a perinone type coloring pigment, a perylene type coloring pigment, a dioxane type coloring pigment, a quinacridone type coloring pigment, an isoindolinone type coloring pigment, a diketo-pyrrolo-pyrrole type coloring pigment, a benz-imidazolone type coloring pigment, a metal complex coloring pigment and the like; and an inorganic colored pigment such as chrome yellow, yellow iron oxide, red ocher, carbon black and the like. The pigment may include an extender pigment such as calcium carbonate, barium sulfate, clay, talc and the like, in addition to the above pigment.
[0088] A content mass ratio of the pigment based on a total mass of a resin solid content and the pigment in the first water-based base coating composition (PWC, pigment weight content) may preferably be within a range of 10 to 60 mass % When the content mass ratio is less than 10 mass %, hiding property may be lowered. When the content mass ratio is more than 60 mass %, film appearance of the coating film may be deteriorated because of viscosity increasing at a curing stage and lowing of flowability.
[0089] An example of the additives may be a conventional additive other than the above components, such as an ultraviolet rays absorbent, an antioxidant, an antifoaming agent, a surface regulator, a pinhole inhibitor and the like. A content of the additives may be within a conventional content in the art.
[0090] The first water-based base coating composition is prepared by mixing the acrylic emulsion resin, the curing agent and the hydrophilic associated type viscosity agent, and an optional another components.
[0000] Contents of the acrylic emulsion resin, the curing agent and the hydrophilic associated type viscosity agent shown in a mass ratio of a resin solid content may preferably be to 60 mass % of the acrylic emulsion resin, more preferably 10 to 50 mass %,
5 to 80 mass % of the curing agent, more preferably 10 to 70 mass %, and
0.01 to 20 mass % of the hydrophilic associated type viscosity agent, more preferably 0.1 to 10 mass %.
When a content of the acrylic emulsion resin is more than 60 mass %, film appearance of resulting coating film may be deteriorated. When a content of the acrylic emulsion resin is less than 1 mass %, workability at coating may be lowered.
When a content of the curing agent is more than 80 mass %, chipping property of resulting coating film may be deteriorated. When a content of the curing agent is less than 5 mass %, water resistance of resulting coating film may be lowered. When a content of the hydrophilic associated type viscosity agent is more than 20 mass %, film appearance or water resistance of resulting coating may be lowered. When a content of the hydrophilic associated type viscosity agent is less than 0.01 mass %, sagging or mixing layer may occur in a coating stage of the second water-based base coating composition.
[0091] The additional resin component, the pigment-dispersing paste and another additives which are optionally used may be used in proper contents. A content of the additional resin component may preferably be less than 50 mass % based on a resin solid content contained in the first water-based base coating composition. When a content of the additional resin component is more than 50 mass %, making high solid in the coating composition becomes difficult and is not preferable.
[0092] An order for adding the components is not limited. A form of the first water-based base coating composition is not particularly limited, as long as the coating composition is an aqueous coating composition, and includes, for example, a water-soluble form, a water-dispersion form, an emulsion form and the like.
[0093] Second Water-Based Base Coating Composition
[0094] A second water-based base coating composition used in a method for forming a multilayer coating film according to the present invention may be a second water-based base coating composition conventionally used in a coating of automobile body. The second water-based coating composition may contain, for example, a film forming resin, a curing agent, a pigment such as a luster pigment, a coloring pigment, an extender pigment and the like, and additives whish are solved or dispersed in an aqueous medium. The film forming resin includes an acrylic emulsion resin (A), a water soluble acrylic resin (B) and a water soluble polyester resin (C).
[0095] Acrylic Emulsion Resin (A)
[0096] As the acrylic emulsion resin (A), the acrylic emulsion described in the section of the first water-based base coating composition may be used. The acrylic emulsion resin (A) may preferably contain a single layered acrylic emulsion resin (a) and a core-shell type acrylic emulsion resin (b). In the second water-based base coating composition, the single layered acrylic emulsion resin (a) has lower water retention capacity compared with the core-shell type acrylic emulsion resin (b). In case that a content of the single layered acrylic emulsion resin (a) is too high, sagging or mixing layer in the first water-based base coating film may occur which is caused by increase of move of water toward the first water-based base coating film. In case that a content of the core-shell type acrylic emulsion resin (b) is too high, smoothness of a coating film may be lowered due to excess increase of coating film viscosity of the second water-based base coating composition. A content ratio of the single layered acrylic emulsion resin (a) and the core-shell type acrylic emulsion resin (b) is important in view of a balance between water retention capacity and smoothness of coating film. A content mass ratio of the single layered acrylic emulsion resin (a) in a resin solid content based on the acrylic emulsion resin (A) in a resin solid content, which is shown in (a)/(A), may preferably be within a range of 30 to 60% (expressed in percentage).
[0097] Water Soluble Acrylic Resin (B)
[0098] A water soluble acrylic resin (B) may be prepared by co-polymerization of a hydroxyl group-containing monomer and another monomer.
[0099] The hydroxyl group-containing monomer may include, for example, a hydroxyl group-containing (meta)acrylate such as 2-hydroxyethyl (meta)acrylate, hydroxypropyl (meta)acrylate, 2,3-dihydroxybutyl (meta)acrylate, 4-hydroxybutyl (meta)acrylate; a reactant of the hydroxyl group-containing (meta)acrylate and epsilon-caprolactone; an esterified compound of polyalcohol such as polyethyleneglycol mono(meta)acrylate with acrylic acid or methacrylic acid; and the like. A reactant obtained by ring-opening polymerization of epsilon-caprolactone and an esterified compound which is obtained by esterification of polyalcohol with acrylic acid or methacrylic acid may be used. The hydroxyl group-containing monomer (a) may be a singular compound or in an appropriate combination of two or more compounds. In this specification, the term “(meta)acrylate” means acrylate or methacrylate.
[0100] Another monomer may include, for example, a carboxyl group-containing monomer such as acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, fumaric acid and the like;
[0000] a dicarboxylic acid monoester monomer such as ethyl maleate, butyl maleate, itaconic acid ethyl ester, itaconic acid butyl ester and the like;
a (meth)acrylate alkylester monomer such as methyl (meta)acrylate, ethyl (meta)acrylate, propyl (meta)acrylate, n, i or t-butyl (meta)acrylate, 2-ethylhexyl (meta)acrylate, lauryl (meta)acrylate and the like;
an alicyclic group-containing monomer such as (meta)acrylic acid cyclopentyl, (meta)acrylic acid cyclohexyl, isobornyl (meta)acrylate, tricyclodecanyl (meta)acrylate, adamantyl (meta)acrylate and the like;
a (meth)acrylic acid aminoalkyl ester monomer such as (meta)acrylic acid aminoethyl, (meta)acrylic acid dimethyl aminoethyl, (meta)acrylic acid butyl aminoethyl and the like;
a (meth)acrylic acid aminoalkyl amide monomer such as aminoethyl (meth)acrylamaide, dimethylaminomethyl (meth)acrylamaide, methylaminopropyl (meth)acrylamaide; another amido group-containing monomer such as acrylic amide, methacrylamide, N-methylol acrylic amide, methoxybutyl acrylic amide, diacetone acrylic amide and the like;
a vinyl cyanide monomer such as (meth)acrylonitrile, alpha-chloro acrylonitrile and the like;
a saturated aliphatic carboxylic acid vinyl ester monomer such as vinyl acetate, vinyl propionate and the like;
a styrene monomer such as styrene, alpha-methyl styrene, vinyl toluene; and the like.
These monomers may be a singular compound or in an appropriate combination of two or more compounds.
[0101] In these another monomers, acrylic acid, methacrylic acid, methyl (meta)acrylate, ethyl (meta) acrylate, 2-ethylhexyl (meta) acrylate, lauryl(meta) acrylate, (meta)acrylic acid cyclohexyl and the like may preferably be used.
[0102] As a polymerization process of the hydroxy group-containing monomer and another monomer, a conventional process which is used in the art may be used. A polymerization process may include, for example, a bulk polymerization process, a solution polymerization process, a bulk-suspension two-step polymerization process including a suspension polymerization after a bulk polymerization and the like. In these polymerization processes, a solution polymerization process may preferably be used. The solution polymerization process may be, for example, a process of heating of the monomer mixture at a temperature of 80° C. to 200° C. with stirring in the presence of a radical polymerization initiator.
[0103] The water soluble acrylic resin (B) may preferably have a number average molecular weight within a range of 1,000 to 15,000, more preferably 1,000 to 8,000, most preferably 1,000 to 5,000. When a number average molecular weight is less than 1,000, coating film property of a resulting multilayer coating film may be deteriorated. On the other hand, when a number average molecular weight is more than 15,000, excess amount of solvent may be required in a preparation of a coating composition because of high viscosity of a resin component.
[0104] The water soluble acrylic resin (B) may preferably have a hydroxyl value of a solid content within a range of 50 to 250 mgKOH/g, more preferably 60 to 200 mgKOH/g, most preferably 80 to 180 mgKOH/g. When a hydroxyl value of a solid content is less than 50 mgKOH/g, coating film property of a resulting multilayer coating film may be deteriorated because of poor reactivity toward the curing agent. In addition, adhesion of coating film may be deteriorated. On the other hand, when a hydroxyl value of a solid content is more than 250 mgKOH/g, water resistance of a resulting multilayer coating film may be deteriorated.
[0105] The water soluble acrylic resin (B) may preferably have an acid value of a solid content within a range of 2 to 50 mgKOH/g, more preferably 5 to 20 mgKOH/g. When an acid value of a solid content is less than 2 mgKOH/g, coating film property of a resulting multilayer coating film may be deteriorated. On the other hand, when an acid value of a solid content is more than 50 mgKOH/g, water resistance of a resulting multilayer coating film may be deteriorated.
[0106] The water soluble acrylic resin (B) may be a commercially-available products. A concrete example of a commercially-available water soluble acrylic resin (B) may be, for example, Acrydic series (trade name) produced by DIC Corporation, such as Acrydic A-837, Acrydic A-871, Acrydic A-1370 and the like; Hariacron series (trade name) produced by Harima Chemicals Co., Ltd., such as Hariacron D-1703, Hariacron N-2043-60MEX and the like; Dianal series (trade name) produced by Mitsubishi Rayon Co., Ltd.; Hitaloid series (trade name) produced by Hitachi Chemical Co., Ltd.; Olester series (trade name) produced by Mitsubishi. Chemical Corporation; and the like.
[0107] Water Soluble Polyester Resin (C)
[0108] The second water-based base coating composition according to the present invention contains a water soluble polyester resin (C). The water soluble polyester resin (C) contained in the second water-based base coating composition can provide advantages such as improvement of coating workability and improvement of coating film appearance of a resulting coating film. As the water soluble polyester resin (C) contained in the second water-based base coating composition, a compound having two hydroxyl groups in one molecular, which is generally called a polyester polyol, may be preferably used. The water soluble polyester resin may be prepared by polycondensation reaction (esterification reaction) of polyalcohol with polybasic acid or anhydride thereof.
[0109] The polyalcohol may include, for example, ethylene glycol, diethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, neopentylglycol, 1,2-butanediol, 1,3-butanediol, 2,3-butanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, hydrogenated bisphenol A, hydroxyalkylated bisphenol A, 1,4-cyclohexanedimethanol, 2,2-dimethyl-3-hydroxypropyl-2,2-dimethyl-3-hydroxypropionate, 2,2,4-trimethyl-1,3-pentanediol, N,N-bis-(2-hydroxyethyl) dimethyl hydantoin, polytetramethylene ether glycol, polycaprolactone polyol, glycerin, sorbitol, trimethylol ethane, trimethylol propane, trimethylol butane, hexanetriol, pentaerythritol, dipentaerythritol, tris-(hydroxyethyl) isocyanate and the like. These polyalcohols may be a singular compound or in an appropriate combination of two or more compounds.
[0110] The polybasic acid or anhydride thereof may include, for example, phthalic acid, phthalic anhydrite, tetrahydrophthalic acid, tetrahydrophthalic anhydrite, hexahydrophthalic acid, hexahydrophthalic anhydrite, methyl tetrahydrophthalic acid, methyl tetrahydrophthalic anhydrite, himic anhydride, trimellitic acid, trimellitic anhydride, pyromellitic acid, pyromellitic anhydride, isophthalic acid, terephthalic acid, maleic acid, maleic anhydride, fumaric acid, itaconic acid, adipic acid, azelaic acid, sebacic acid, succinic acid, succinic anhydride, lactic acid, dodecenyl succinic acid, dodecenyl succinic anhydride, cyclohexane-1,4-dicarboxylic acid, endo anhydride and the like. These polybasic acids or anhydrides thereof may be a singular compound or in an appropriate combination of two or more compounds.
[0111] A water soluble polyester resin obtained by modification in use of a compound such as lactone, oils or fatty acid, melamine resins, urethane resins and the like may be used as the water soluble polyester resin (C). An example of a water soluble polyester resin obtained by modification in use of oils or fatty acid may include a modified polyester resin obtained by modification in use of oils such as castor oil, dehydration castor oil, coconut oil, corn oil, cottonseed oil, linseed oil, penile oil, poppy oil, safflower oil, bean oil, tung oil, or fatty acids obtained by extraction thereof. In a preparation of the modified polyester resin in use of oils or fatty acids, a total amount of the oils or fatty acids for incorporation may preferably be up to about 30 mass parts based on 100 mass parts of polyester resin.
[0112] The water soluble polyester resin (C) may preferably have a number average molecular weight of 500 to 6,000 in polystyrene conversion measured by gel permeation chromatography (CPC), more preferably 1,000 to 4,000. When a number average molecular weight is less than 500, adhesion of coating film of a resulting coating film may be deteriorated. When a number average molecular weight more than 6,000, coating concordance toward a coating substrate in coating step may be deteriorated.
[0113] The water soluble polyester resin (C) may preferably have a solid hydroxyl value of 80 to 350 mgKOH/g, more preferably 80 to 300 mgKOH/g, most preferably 150 to 250 mgKOH/g. When a solid hydroxyl value is less than 80 mgKOH/g, coating film property of a resulting multilayer coating film may be lower because of decrease of reactivity with a curing agent. In addition, adhesion of coating film of a resulting coating film may be deteriorated. When a solid hydroxyl value is more than 350 mgKOH/g, water resistance of a resulting multilayer coating film may lower.
[0114] In the second water-based base coating composition according to the present invention, it is required that a rate represented by the following formula:
[0000] ( A )/( A+B+C ) wherein (A) is a resin solid content by mass of the acrylic emulsion resin (A), and (A+B+C) is a total resin solid content by mass of the acrylic emulsion resin (A), the water soluble acrylic resin (B) and the water soluble polyester resin (C),
is from 40% to 60% expressed in percentage.
[0116] An acrylic emulsion resin generally has higher molecular weight, and tends to provide abrupt coagulation in case of high amounts of resin solids. Therefore, an acrylic emulsion has higher property of water exclusion, compared with a water soluble resin. Then, design of increasing an amount of a water soluble resin in the second water-based base coating composition (that is, reducing an amount of the acrylic emulsion resin (A)) can increase water-retaining capacity of a second water-based base coating composition, at the same time, can prevent mobilization of water into a first water-based base coating film (a lower layer) in a coating step. On the other hand, reducing an amount of the acrylic emulsion resin (A) may deteriorate design properties because of lower viscosity of uncured coating film (for example, orientation of aluminum pigments in a second water-based base coating film). Thus, it is important to design an amount ratio of the acrylic emulsion resin (A) and a water soluble resin, i.e., the water soluble acrylic resin (B) and the water soluble polyester resin (C), in order to keep the above functions in excellent states.
[0117] The present invention defines that a rate represented by the following formula:
[0000] ( A )/( A+B+C )
[0000] wherein (A) is a resin solid content by mass of the acrylic emulsion resin (A), and (A+B+C) is a total resin solid content by mass of the acrylic emulsion resin (A), the water soluble acrylic resin (B) and the water soluble polyester resin (C),
is from 40% to 60% expressed in percentage.
The rate expressed in percentage may preferably be from 50% to 60%, more preferably from 55% to 60%. When the ratio is less than 40%, a viscosity of the second water-based base coating film is lower and design property of coating film (orientation of aluminum pigments) deteriorates. When the ratio is more than 60%, water-retaining capacity of a second water-based base coating composition becomes lower, and coating defect such as sagging or mixing of layers occurs due to transfer of water toward the first water-based base coating film at the time of coating of the second water-based base coating composition.
[0118] Pigments
[0119] The second water-based base coating composition may preferably contain a pigment. As the pigment, a conventional pigment which is generally used in a coating field can be used. The pigment may include, for example, the pigment described in the first water-based base coating composition, in addition, uncolored or colored metal luster material of metal such as aluminum, copper, zinc, iron, nickel, tin, aluminum oxide and the like, an alloy thereof, and mixtures thereof; and a luster pigment such as an interference mica pigment, a white mica pigment, a graphite pigment and the like. The pigment may be used alone, or two or more pigments may be used in an appropriate combination.
[0120] A content mass ratio of the pigment based on a total mass of a resin solid content and the pigment in the second water-based base coating composition (PWC, pigment weight content) may generally be within a range of 0.1 to 50 mass %, preferably within a range of 0.5 to 40 mass %, more preferably within a range of 1 to 30 mass % When a pigment weight content is less than 0.1 mass %, an technical effects caused by a pigment may not be obtained. When a pigment weight content is more than 50 mass %, film appearance of resulting coating film may be deteriorated.
[0121] The second water-based base coating composition according to the present invention may optionally contain additives in addition to the above components. An example of the additives may be, for example, an organic solvent, a curing catalyst (an organic metal catalyst), a sagging-preventing/sedimentation-preventing agent, a surface conditioner, a color separation-preventing agent, a dispersing agent, an antifoaming/forming-preventing agent, a viscosity-adjusting agent (an thickener), a leveling agent, a matting agent, an ultraviolet rays absorbent, an antioxidant, a plasticizer, a film-forming assistant and the like.
[0122] The organic solvent may include, for example, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, Solvesso 100, Solvesso 150, Solvesso 200 (all products are produced by Exxon Chemistry Corporation), toluene, xylene, methoxybutyl acetate, cellosolve acetate, butyl cellosolve acetate, methyl acetate, ethyl acetate, butyl acetate, petroleum ether, petroleum naphtha and the like.
[0123] An amount of the organic solvent is not limited. However, it may be preferred that an amount of the organic solvent is an amount with an environmental protection and an environmental influence taken into consideration.
[0124] As the sagging-preventing/sedimentation-preventing agent, for example, Disparlon 6700 (a product name, fatty acid bisamide-based thixotropic agent, produced by Kusumoto Chemicals, Ltd.) and the like may preferably be used. As the color separation-preventing agent, for example, Disparlon 2100 (a product name, silicone-added aliphatic polycarboxylic acid, produced by Kusumoto Chemicals, Ltd.) and the like may preferably be used. As the antifoaming/forming-preventing agent, for example, Disparlon 1950 (a product name, a specific vinyl polymer, produced by Kusumoto Chemicals, Ltd.) and the like may preferably be used.
[0125] The surface conditioner may preferably include, for example, polyether-modified siloxane, polyester-modified polymethylalkyl siloxane, polyether-modified polydimethyl siloxane, acrylic group-containing polyether-modified polydimethyl siloxane and the like. Using such surface conditioner can provide a surface tension of the coating composition within a suitable range.
[0126] The second water-based base coating composition can be prepared in a same manner as the preparation method of the first water-based base coating composition. A type of the second water-based base coating composition is not particularly limited, as long as the coating composition is an aqueous coating composition, and includes, for example, a water-soluble form, a water-dispersion form, an emulsion form and the like.
[0127] Clear Coating Composition
[0128] A clear coating composition used in a method for forming a multilayer coating film according to the present invention may be a usual clear coating composition for coating of an automobile body. The clear coating composition may be, for example, a clear coating composition containing a film-forming resin and an optional curing agent and additives in a form of dispersed or dissolved in medium. The film-forming resin may include, for example, an acrylic resin, a polyester resin, an epoxy resin, an urethane resin and the like. These resins may be used in a combination of a curing agent such as an amino resin, an isocyanate resin and mixtures thereof. From the viewpoint of the transparency, acid etch resistance or the like, the combination of the acrylic resin and/or polyester resin with an amino resin, or the acrylic resin and/or polyester resin having carboxylic acid-epoxy curing system and the like may be preferred.
[0129] The clear coating composition may be of any coating type, such as any of an organic solvent-based coating composition, an aqueous (water-soluble, water-dispersible, or emulsion) coating composition, a non-water-dispersible coating composition and a powdered coating composition. The clear coating composition may further contain additives such as a curing catalyst, a surface conditioner, a viscosity modifier, an ultraviolet-rays absorbent, a light stabilizer and the like.
[0130] Method for Forming a Multilayer Coating Film
[0131] A method for forming a multilayer coating film according to the present invention is a method including the steps of;
[0132] (1) applying a first water-based base coating composition on a surface of a coating material to form an uncured first water-based base coating film,
[0133] (2) applying a second water-based base coating composition on the uncured first water-based base coating film to form an uncured second water-based base coating film,
[0134] (3) applying a clear coating composition on the uncured second water-based base coating film to form an uncured clear coating film, and
[0135] (4) simultaneously heating and curing the uncured first water-based base coating film, the uncured second water-based base coating film and the uncured clear coating film formed in the steps (1), (2) and (3) to form a multilayer coating film.
[0136] A coating material used in the method for forming a multilayer coating film according to the present invention is not particularly limited and may include, for example, iron, copper, aluminum, tin, zinc, an alloy thereof and the like, as well as a plated product and a vapor deposited product in use of the metal described above. The coating material may have a cured electrodeposition coating film on its surface. The cured electrodeposition coating film is obtained by applying an electrodeposition coating composition on a coating material and curing by heating.
[0137] The electrodeposition coating composition is not particularly limited, and a conventional cationic electrodeposition coating composition or a conventional anionic electrodeposition coating composition may be used as the electrodeposition coating composition. Methods and conditions of applying an electrodeposition coating composition and curing by heating may be a conventional method and condition in electrodeposition coating of an automobile body.
[0138] First, the first water-based base coating composition is applied on a surface of the coating material to form an uncured first water-based base coating film. For example, the first water-based base coating composition can be applied by spraying with an air electrostatic spray coater, which is so-called “react gun”; a rotary spray electrostatic coater, which is so-called “micro micro (μμ) bell”, “micro (μ) bell” or “metallic (meta) bell”; or the like.
[0139] A coating amount of the first water-based base coating composition is adjusted such that the resulting first base coating film has a cured coating film thickness of 5 to 40 μm, preferably 10 to 30 μm. When the film thickness is less than 5 μm, film appearance and chipping resistance of the resulting coating film may be lowered. On the other hand, when the film thickness is more than 40 μm, problems such as the sagging of the coating composition during the application thereof and an occurrence of pinholes when heating and curing the coating composition may occur.
[0140] In the method for forming a multilayer coating film according to the present invention, the second water-based base coating composition is applied on the obtained uncured first water-based base coating film to form an uncured second water-based base coating film, without heating and curing the first water-based base coating film in the coating of the first water-based base coating composition. In the method for forming a multilayer coating film according to the present invention, it is advantageous that wet-on-wet coating without preheat in coating the second water-based base coating composition on the uncured first water-based base coating film can be performed.
[0141] In a conventional wet-on-wet coating, a preheat step of an uncured first water-based base coating film before coating a second water-based base coating composition is generally performed. The reason why such preheat step is performed is to prevent the following defects:
[0000] pin hole caused by bumping of residual water contained in an uncured first water-based base coating film in curing and heating a multilayer coating film may frequently occur, and
mixing layer caused by mixing of an uncured first water-based base coating film and an uncured second water-based base coating film may occur in coating a second water-based base coating composition to lower film appearance of a multilayer coating film. Such preheat step includes, for example, a drying at a temperature of about 80° C. for one to 10 minutes.
[0142] In the present invention, specifying components contained in the first water-based base coating composition and the second water-based base coating composition can provide an advantageous effect of wet-on-wet coating without preheat in coating the second water-based base coating composition on the uncured first water-based base coating film. The term “without preheat” in this specification means, for example, applying the first water-based base coating composition at a room temperature (for example, 10 to 30° C.), then applying the second water-based base coating composition in 0 to 30 minutes after coating of the first water-based base coating composition. Such advantageous effect in the present invention seems to be caused by prevention of water-transfer contained in the second water-based base coating composition toward the uncured first water-based base coating film in coating the second water-based base coating composition on the uncured first water-based base coating film, and prevention of sagging and mixing layer caused by adjustment of viscosity of the uncured water-based base coating film resulting from the hydrophilic associated type viscosity agent.
[0143] The second water-based base coating composition is applied on the uncured first water-based base coating film to form an uncured second water-based base coating film. For example, the second water-based base coating composition can be applied by spraying with an air electrostatic spray coater, which is so-called “react gun”; a rotary spray electrostatic coater, which is so-called “micro micro (μμ) bell”, “micro (μ) bell”, or “metallic (meta) bell”; or the like.
[0144] A coating amount of the second water-based base coating composition is adjusted such that the resulting second base coating film has a cured coating film thickness of 5 to 30 μm. When the film thickness is less than 5 μm, inadequate hiding property or color unevenness appearance may occur. On the other hand, when the film thickness is more than 30 μm, problems such as the sagging of the coating composition during the application thereof and the occurrence of pinholes when heating and curing the coating composition may occur.
[0145] A viscosity at a temperature of 20° C. of the uncured first water-based base coating film after applying the second water-based base coating composition may preferably be from 45 to 100 Pa·s at a shear rate of 0.01/s, more preferably from 60 to 90 Pa·s, in view of smoothness of resulting multilayer coating film. The viscosity of the uncured first water-based base coating film can be measured by the followings:
[0000] (1) applying the first water-based base coating composition on a surface of cured electrodeposition coating film on a substrate, then having setting at 25° C. for 6 minutes, next, applying the second water-based base coating composition,
(2) after having setting at 25° C. for 3 minutes, putting an aluminum foil on a resulting second water-based base coating film, then, peeling the aluminum foil to remove the attached mere second water-based base coating film,
(3) gathering the remaining first water-based base coating film with a spatula, then measuring a viscosity of the uncured first water-based base coating film with a viscometer (MCR-301) produced by Anton Paar corporation at a shear rate of 0.01/s.
[0146] Next, applying the clear coating composition on the uncured second water-based base coating film to form an uncured clear coating film. The clear coating composition can be applied in a coating method corresponding to its type of the clear coating composition. Usually, the coating amount of the clear coating composition is adjusted such that the resulting clear coating film has a dry coating film thickness of 10 to 70 μm. When the film thickness is less than 10 μm, lowering of appearance, such as a gloss of the multilayer coating film may occur. On the other hand, when the film thickness is more than 70 μm, lowering of decorative (sharpness) of the coating film, sagging or unevenness of the coating composition during the application thereof may occur. It may be preferable that applying preheat, for example, at a temperature of 40 to 100° C. for 2 to 10 minutes after forming the uncured second water-based base coating film, in order to obtain more excellent film appearance.
[0147] Next, the uncured first water-based base coating film, the uncured second water-based base coating film and the uncured clear coating film are simultaneously heated and cured. The heating may be usually at a temperature of 110 to 180° C., preferably 120 to 160° C. The heating can provide a cured coating film having high degree of crosslinking. When a heating temperature is less than 110° C., inadequate curing may be obtained. When a heating temperature is more than 180° C., a hard and brittle coating film may be obtained. A heating time can be adjusted depending on a heat temperature, and may be, for example, 10 to 60 minutes at a hearing temperature of 120 to 160° C.
[0148] The multilayer coating film obtained by the method for forming a multilayer coating film according to the present invention has excellent smoothness and excellent film appearance, even when the second water-based base coating composition is applied wet-on-wet on the uncured first water-based base coating film without preheat after the first water-based base coating composition is applied.
[0149] The method for forming a multilayer coating film according to the present invention has such advantages. The present invention therefore does not need a preheat step after the first water-based base coating composition is applied, which provides energy saving and reduction of CO 2 emissions in coating steps. In addition, the present invention has advantages of facility cost and coating line spaces.
EXAMPLES
[0150] The present invention is more concretely illustrated below according to Examples, but the present invention is not limited only to these Examples. In Examples, unless otherwise noted, “parts” and “%” are by mass basis.
Preparation Example 1
Preparation of Acrylic Emulsion Resin
[0151] Water (445 parts) and 5 parts of Newcol 293 (an emulsifier manufactured by Nippon Nyukazai Co., Ltd.) were charged to a reaction vessel conventionally used for preparing acrylic resin emulsion with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a nitrogen inlet tube, and the temperature was raised to 75° C. with stirring. The mixture of monomer mixture of 145 parts of methyl methacrylate, 50 parts of styrene, 220 parts of ethyl acrylate, 70 parts of 2-hydroxyethyl methacrylate and 15 parts of methacrylic acid; and 240 parts of water and 30 parts of Newcol 293 (manufactured by Nippon Nyukazai Co., Ltd.); was emulsified with a homogenizer to form a monomer pre-emulsion. The monomer pre-emulsion was dropped to the reaction vessel for 3 hours with stirring. In parallel with the dropping of the monomer pre-emulsion, an aqueous solution prepared by dissolving 1 part of ammonium persulfate as a polymerization initiator in 50 parts of water was evenly dropped to the reaction vessel until the dropping of the monomer pre-emulsion was completed. After the completion of the dropping of the monomer pre-emulsion, the reaction was further continued for 1 hour at 80° C., and then cooled. After cooling, an aqueous solution prepared by dissolving 2 parts of dimethylamino ethanol in 20 parts of water was poured in the reaction vessel to obtain an acrylic emulsion resin having a solid component of 40.6% by mass.
[0152] The resulting acrylic emulsion resin had a solid acid value of 20 mgKOH/g, a solid hydroxyl value of 60 mgKOH/g and Tg of 30° C. The solid content was determined according to JIS K 5601-1-2, Determination of non-volatile matter content.
Preparation Example 2
Preparation of Pigment Dispersed Paste
[0153] Disperbyk 190 (4.5 parts, a nonion-anion-type dispersant, produced by BYK-Chemie company) as a dispersant, 0.5 part of BYK-011 (an antifoaming agent, produced by BYK-Chemie company) as an antifoaming agent, 22.9 parts of deionized water and 72.1 parts of titanium dioxide were pre-mixed, then mediums of glass beads were added into the resulting mixture contained in a paint conditioner and mixed and dispersed at room temperature until a grain size was not more than 5 μm, to obtain a pigment dispersed paste.
Preparation Example 3
Preparation of Polyester Resin Water Dispersion
[0154] In a reaction vessel conventionally used for preparing polyester resin with a stirrer, a thermometer, a reflux condenser and a nitrogen inlet tube, 19 parts of isophthalic acid, 36 parts of hexahydrophthalic anhydride, 7 parts of trimethylolpropane, 12 parts of neopentyl glycol, 26 parts of 1,6-hexanediol and 0.1 part of dibutyltin oxide as a catalyst were charged, and the temperature was raised from 150° C. to 230° C. for three hours and kept at a temperature of 230° C. for 5 hours.
[0155] After cooling at a temperature of 135° C., 7.7 parts of trimellitic anhydride was added and mixed for one hour to obtain a polyester resin having a solid acid value of 50 mgKOH/g, a solid hydroxyl value of 45 mgKOH/g and a number-average molecular weight of 2500. The reaction mixture was cooled to 90° C., and 7.3 parts of dimethyl ethanolamine and 225 parts of deionized water were added thereto, to obtain a polyester resin water dispersion having a solid component concentration of 30%.
Preparation Example 4
Preparation of First Water-Based Base Coating Composition (1)
[0156] After mixing 206.6 parts of the pigment dispersed paste obtained by Preparation example 2, 45.0 parts of the acrylic emulsion resin obtained by Preparation example 1, 62.4 parts of the polyester resin water dispersion obtained by Preparation example 3 and 78.7 parts of Cymel 211 (a melamine resin produced by Nihon Cytec Industries Co., Ltd., a nonvolatile content of 80%) as a curing agent were mixed, and 6.7 parts of BYK-430 (a hydrophilic associated type viscosity agent (a nonvolatile content of 30%), produced by BYK-Chemie company, the amounts corresponds to 2 mass % based on a resin solid content of a first water-based base coating composition) as a viscosity agent was added thereto and mixed, to obtain a first water-based base coating composition (1).
Preparation Example 5
Preparation of First Water-Based Base Coating Compositions (2)-(9)
[0157] Water-based base coating compositions (2)-(9) were prepared in the same manner as Preparation example 4, except that a type of a viscosity agent and an amount of a viscosity agent were changed from a hydrophilic associated type viscosity agent BYK-430 used as a viscosity agent, in accordance with Table 1. In the preparation of water-based base coating compositions (7)-(9), a hydrophobic associated type viscosity agent was used in place of a hydrophilic associated type viscosity agent.
[0000]
TABLE 1
Type of
viscosity
First water-based base coating composition
agent
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
BYK-430 * 1
2
AQ-607 * 2
2
1.6
1
1
1
UH-540 * 3
0.4
1
2
RHEOLATE266 * 4
1
2
BYK-425 * 5
1
2
A numerical value in Table means a mass % based on a resin solid content of a first water-based base coating composition.
* 1 A hydrophilic associated type viscosity agent, manufactured by BYK-Chemie company.
* 2 A hydrophilic associated type viscosity agent, manufactured by Kusumoto Chemincals, Ltd.
* 3 A hydrophobic associated type viscosity agent, manufactured by ADEKA Corporation.
* 4 A hydrophobic associated type viscosity agent, manufactured by Elementis plc.
* 5 A hydrophobic associated type viscosity agent, manufactured by BYK-Chemie company.
Preparation Example 6
Preparation of Single Layered Acrylic Emulsion Resin (a)
[0158] Into a reaction vessel, 126.5 parts of ion-exchanged water was charged and heated at a temperature of 80° C. under nitrogen atmosphere. Next, both of a mixture of a monomer mixture (100 parts) of 27.61 parts of methyl acrylate, 53.04 parts of ethyl acrylate, 4.00 parts of styrene, 9.28 parts of 2-hydroxyethyl methacrylate, 3.07 parts of methacrylic acid and 3.00 parts of allyl methacrylate, and a mixture of 0.7 part of AQUARON HS-10 (polyoxyethylene alkylpropenylphenyl ether sulfate, produced by Dai-ichi Kogyo Seiyaku co., ltd.) and 0.5 part of ADEKA REASOAP NE-20 (alpha-[1-[(allyloxy)methyl]-2-nonylphenoxy]ethyl)-omega-hydroxyoxyethylene, produced by ADEKA CORPORATION) and 80 parts of ion-exchanged water; and an initiator solution of 0.3 part of ammonium persulphate and 10 parts of ion-exchanged water; were simultaneously added dropwise into the reaction vessel over 2 hours respectively. After completion of the dropwise addition, aging was carried out at the same temperature for 2 hours. Next, the reaction mixture was cooled at 40° C. and filtered with a 400 mesh filter. Then 70 parts of ion-exchanged water and 0.32 part of dimethylaminoethanol were added to adjust a pH of 6.5, and a single layered acrylic emulsion resin (a) having an average particle diameter of 150 nm, non-volatilization of 25%, a solid acid value of 20 mgKOH/g and a hydroxyl value of 40 mgKOH/g was obtained.
Preparation Example 7
Preparation of Core-Shell Type Acrylic Emulsion Resin (b)
[0159] Into a separable flask (2 L) equipped with a stirrer, a reflux condenser, a dropping funnel, a nitrogen inlet tube and a thermo-sensor, 651 parts of ion-exchanged water was charged and heated at a temperature of 70° C. under nitrogen atmosphere. A pre-prepared pre-emulsion (1) as a first step monomer component of 300 parts of methyl methacrylate, 194 parts of styrene, 6 parts of methacrylic acid (a calculated Tg of core by the three monomers being 104° C.), 33 parts of 15% aqueous solution of polyoxyethylene nonylphenyl ether ammonium sulfate (High tenor N-08, produced by Dai-ichi Kogyo Seiyaku co., ltd.), 40 parts of 25% aqueous solution of polyoxyethylene nonylphenyl ether (Nonipol 200, produced by Sanyo Chemical Industries, ltd.) and 102 parts of ion-exchanged water was added dropwise from the dropping funnel over an hour and a half. At the same time, 30 parts of 5% ammonium persulphate was simultaneously added dropwise into the flask over an hour and a half. After completion of the dropwise addition, aging was carried out for 40 minutes, and a pre-prepared pre-emulsion (2) as a final step monomer component of 116 parts of 2-ethylhexyl acrylate, 206 parts of methyl methacrylate, 150 parts of styrene, 28 parts of acrylic acid (a calculated Tg of shell by the four monomers being 40° C.), 33 parts of 15% aqueous solution of High tenor N-08 (produced by Dai-ichi Kogyo Seiyaku co., ltd.), 40 parts of Nonipol 200 (produced by Sanyo Chemical Industries. ltd., 25% aqueous solution) and 102 parts of ion-exchanged water was added dropwise from the dropping funnel over an hour and a half. At the same time, 30 parts of 5% ammonium persulphate was simultaneously added dropwise into the reaction vessel over an hour and a half. After completion of the dropwise addition, aging was carried out for one hour. Next, the reaction mixture was cooled, and 4.6 parts of 25% aqueous ammonia was added thereto for neutralization, to obtain a core-shell type acrylic emulsion resin (b). The resultant core-shell type acrylic emulsion resin (b) had core Tg of 104° C., shell Tg of 40° C., non-volatilization of 49.2%, pH of 6.0, a viscosity of 550 mPa·s (measured by a B-type viscometer, with a use of a rotor No. 2, 30 rotation per minute, at 25° C., in which the same applies hereafter), a mean particle diameter of 140 nm, which was measured by a dynamic light scattering type particle size measurement device LB-500 (produced by Horiba ltd.) at 20° C.
Preparation Example 8
Preparation of Water-Soluble Acrylic Resin (B)
[0160] In a reaction vessel, 23.89 parts of tripropylene glycol methyl ether and 16.11 parts of propylene glycol methyl ether were charged and heated at a temperature of 105° C. with stirring under nitrogen atmosphere. Next, a monomer mixture of 13.1 parts of methyl methacrylate, 68.4 parts of ethyl acrylate, 11.6 parts of 2-hydroxyethyl methacrylate and 6.9 parts of methacrylic acid was prepared. Then 100 parts of resultant monomer mixture and an initiator solution of 10 parts of tripropylene glycol methyl ether and 1 part of t-butyl peroxy 2-ethyl hexanoate were simultaneously added dropwise into the reaction vessel over three hours. After completion of the dropwise addition, aging was carried out at the same temperature for 0.5 hour. Further, an initiator solution of 5 parts of tripropylene glycol methyl ether and 0.3 part of t-butyl peroxy 2-ethyl hexanoate was added dropwise into the reaction vessel over 0.5 hour. After completion of the dropwise addition, aging was carried out at the same temperature for 2 hours. After removal of 16.1 part of a solvent in a solvent removal device under reduced pressure (70 torr) at 110° C., 204 parts of ion-exchanged water and 7.1 parts of dimethyl amino ethanol were added to obtain a water-soluble acrylic resin (B). The resultant water-soluble acrylic resin (B) had non-volatilization of 30%, a solid acid value of 40 mgKOH/g, a hydroxyl value of 50 mgKOH/g, a viscosity of 140 Pa·s (measured by a E-type viscometer, 1 rpm/25° C.).
Preparation Example 9
Preparation of Water-Soluble Polyester Resin (C)
[0161] In a reaction vessel equipped with a stirrer, a condenser and a thermometer, 372 parts of dimethyl terephthalate, 380 parts of dimethyl isophthalate, 576 parts of 2-methyl-1,3-propane diol, 222 parts of 1,5-pentanediol and 0.41 part of tetrabutyl titanate were added and heated at a temperature between 160° C. to 230° C. and transesterificated over 4 hours. A pressure of the reaction system was gradually reduced over 20 minutes to reach a reduced pressure of 5 mmHg, further vacuumed to reach a vacuum pressure of not more than 0.3 mmHg, and carried out polycondensation reaction at 260° C. for 40 minutes. The resultant reaction mixture was cooled at 220° C. under a nitrogen atmosphere, and 23 parts of trimellitic anhydride was added thereto and reacted at 220° C. for 30 minutes to obtain a polyester resin. To 100 parts of the resultant polyester resin, 40 parts of butyl cellosolve and 2.7 parts of triethylamine were added, and stirred at 80° C. for one hour to dissolve it. Then, 193 parts of ion-exchanged water was slowly added to obtain a water-soluble polyester resin (C) having non-volatilization of 30%. In order to measure a mean particle diameter, a dedicated cell was charged with ion-exchanged water and one drop of the water-soluble polyester resin (C) was added and mixed to obtain a sample having a resin solid concentration of 0.1 mass %, and a mean particle diameter was measured by a dynamic light scattering type particle size measurement device LB-500 (produced by Horiba ltd.) at 20° C., which was 35 nm.
Preparation Example 10
Preparation of Second Water-Based Base Coating Composition (1)
[0162] As the acrylic emulsion resin (A), 50 parts of the single layered acrylic emulsion resin (a) obtained by Preparation example 6 (resin solid content of 25%) and 60 parts of the core-shell type acrylic emulsion resin (b) obtained by Preparation example 7 (resin solid content of 49.2%) were mixed and used. To the resulting mixture, 79 parts of the water-soluble acrylic resin (B) obtained by Preparation example 8 (resin solid content of 30%), 14 parts of the water-soluble polyester resin (C) obtained by Preparation example 9 (resin solid content of 30%), 38 parts of Cymel 204 as the melamine resin (a mixed alkylated-type melamine resin, produced by Mitsui Cytec company, resin solid content of 80%), 10 parts of Prime pole PX-1000 bifunctional polyetter polyol, produced by Sanyo Chemical Industries, ltd.), 21 parts of Alpaste 5H8801 as the luster pigment (an aluminum pigment, produced by Asahi Kasei corporation, solid content of 65%, PWC of 12%), 5 parts of an acrylic resin having phosphate group and 0.3 part of lauryl phosphoric acid were added, then 30 parts of 2-ethyl hexanol and 3.3 parts of Adeka nol UH-814N (a thickener, produced by Adeka corporation, solid content of 30%) were uniformly dispersed to obtain a second water-based base coating composition (1).
Preparation Example 11
Preparation of Second Water-Based Base Coating Compositions (2)-(8)
[0163] Second water-based base coating compositions (2)-(8) were prepared in the same manner as Preparation example 10 except that amounts of the acrylic emulsion resin (A), the water soluble acrylic resin (B), the water soluble polyester resin (C) and the other components were changed in accordance with Table 2.
[0000]
TABLE 2
second water-based base coating composition
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
acrylic
single
18
30
12
20
35
10
21
15
emulsion
layered
resin (A)
acrylic
emulsion
resin (a)
core-shell
42
30
28
20
25
50
49
15
type acrylic
emulsion
resin (b)
water soluble acrylic
34
34
50.4
40
34
34
24
35
resin (B)
water soluble polyester
6
6
9.6
20
6
6
6
35
resin (C)
(A)/(A + B + C)
60
60
40
40
60
60
70
30
(mass percentages %)
(a)/(A) (mass percentages
30
50
30
50
58
17
30
50
%)
Example 1
Formation of a Multilayer Coating Film
[0164] Powernics 110 (a cationic electrodeposition coating composition produced by Nippon Paint Co., Ltd.) was electrodeposition coated on a dull steel plate treated with zinc phosphate such that the thickness of the dry coating film was 20 μm, and then heat-cured at 160° C. for 30 minutes and cooled to obtain a substrate having cured electrodeposition coating film.
[0165] The first water-based base coating composition (1) obtained by Production example 4 was coated on the resulting substrate having cured electrodeposition coating film, by using an air spray coating, such that the film thickness was 20 μm, to form an uncured first water-based base coating film. Without lying in a preheat oven, the second water-based base coating composition (1) obtained by Production example 10 was coated on the resulting substrate, by using an air spray coating, such that the film thickness was 10 μm, followed by preheating at 80° C. for 3 minutes. Next, Macflow O-1800W-2 clear (an acid-epoxy curing type clear coating composition produced by Nippon Paint Co., Ltd.) was coated thereon as a clear coating composition by using an air spray coating such that the thickness of the dry coating film was 35 μm, and then was heated and cured at 140° C. for 30 minutes to obtain a test sample, on which a multilayer coating film was formed.
[0166] The above first water-based base coating composition (1), second water-based base coating composition (1) and clear coating composition were diluted described below and used for coating.
[0167] The first water-based base coating composition (1) diluent solvent: an ion-exchanged water 40 seconds/No. 4 Ford cup/20° C.
[0168] The second water-based base coating composition (2) diluent solvent: an ion-exchanged water 45 seconds/No. 4 Ford cup/20° C.
[0169] The clear coating composition diluent solvent: a mixture solvent, EEP (ethylethoxy propionate)/S-150 (aromatic hydrocarbon solvent, produced by Exson corporation)=1/1 (mass ratio) 30 seconds/No. 4 Ford cup/20° C.
[0170] The following evaluation tests were performed using the test sample obtained above. Evaluation results were shown in Table 3.
[0171] Design Property (Flip-Flop Property)
[0172] As for design property (flip-flop property) of the resultant multilayer coating film, L values of 15° (front) and 110° (shade) were measured with X-Rite MA-68II (produced by X-Rite corporation). These values show that the higher the values are, the better the design property are.
[0173] Smoothness (SW Values and LW Values)
[0174] As for film appearance of the resultant multilayer coating film, LW (wavelength region as a measurement: 1,300 to 12,000 μm) and SW (wavelength region as a measurement: 300 to 1,200 μm) were measured with Wave scan DOI (produced by BYK Gardner corporation) and evaluated. These values show that the smaller the values are, the better the smoothness are.
[0175] Sagging Property
[0176] Test plates were prepared in the same coating manner described above, except that a substrate having cured electrodeposition coating film and having a hole with a diameter of 5 mm was used as a coating substrate having cured electrodeposition coating film. Sagging lengths at the hole after heat curing were measured. These values show that the smaller the values are, the better the sagging properties are.
[0177] Measurement Method of Viscosity (Pa's) of the First Water-Based Base Coating Film after Applying the Second Water-Based Base Coating Composition
[0178] On a substrate having cured electrodeposition coating film, the first water-based base coating composition was applied. After setting at 25° C. for 6 minutes, the second water-based base coating composition was applied thereon. After setting at 25° C. for 3 minutes, an aluminum foil sheet was applied thereon and was peeled off with adherent uncured second water-based base coating film. The remaining first water-based base coating film was gathered with a spatula. A viscosity of the resultant sample (gathered material) was measured with a viscometer (MCR-301, produced by Anton Paar Corporation) at a shear rate of 0.01/s and at a temperature of 20° C.
Examples 2-7 and Comparative Examples 1-5
[0179] Test samples having multilayer coating film were prepared in the same manner as Example 1 except that the first water-based base coating composition and the second water-based base coating composition shown in Table 3 were used in place of the first water-based base coating composition (1) and the second water-based base coating composition (2). Measurement of viscosity (Pa·s) of an uncured water-based base coating film at step (2), and evaluation tests of design property, smoothness, sagging property were performed. The test results are shown in Table 3.
[0000]
TABLE 3
Examples
Comparative examples
1
2
3
4
5
6
7
8
1
2
3
4
5
Type of
First water-
(1)
(2)
(3)
(4)
(5)
(6)
(1)
(1)
(7)
(8)
(9)
(2)
(2)
coating
based base
composi-
coating com-
tion
position
Second water-
(1)
(1)
(1)
(2)
(3)
(4)
(5)
(6)
(1)
(1)
(1)
(7)
(8)
based base
coating
composition
Evalu-
viscosity of
78
88
80
74
69
63
52
99
38
32
41
43
74
ation
uncured first
water-based
base coating
film (Pa · s)
Sagging property
0
0
0
1
1
0
4
0
10
15
9
8
1
Design property
3.96
4.01
4.00
3.97
3.84
3.67
3.76
3.97
3.32
3.09
3.30
3.43
3.38
(flip-flop property)
Smooth-
SW
15.6
15.7
15.1
14.8
15.2
16.3
16.8
20.3
22.8
20.5
22.7
23.7
15.3
ness
value
LW
3.7
3.8
3.7
3.6
3.2
3.1
3.3
5.3
3.1
3.3
3.4
3.8
3.6
value
[0180] First water-based base coating compositions used in the above Examples contained the hydrophilic associated type viscosity agent. Therefore, the resulting multilayer coating film had excellent smoothness, excellent film appearance and no mixing of layers between a first water-based base coating film and a second water-based base coating film, even if second water-based base coating composition was applied without preheat in coating.
[0181] On the other hand, Comparative examples 1-3 contained a hydrophobic associated type viscosity agent and provided inferior sagging property, design property and film appearance (smoothness, in particular, inferior SW value). In use of a hydrophobic associated type viscosity agent, when a second water-based coating film was formed on an uncured first water-based coating film, water solvent in an uncured second water-based coating film seemed to be moved to the uncured first water-based coating film to provide lowing of viscosity of uncured first water-based base coating film. Therefore, inferior evaluation results were obtained. Each of comparative examples 4-5 was a comparative example in which an amount of acrylic emulsion resin (A) was larger than the range of the invention (Comparative example 4), and an amount of acrylic emulsion resin (A) was smaller than the range of the invention (Comparative example 5). Both of the comparative examples provided inferior sagging property, design property or film appearance.
[0182] The present invention has an advantage that the method in use of specific compositions of the first water-based base coating composition and the second water-based base coating composition according to the present invention provides a multilayer coating film having excellent smoothness and design property, and excellent film appearance, even when the second water-based base coating composition is applied wet-on-wet on the uncured first water-based base coating film without preheat after the first water-based base coating composition is applied. The present invention therefore does not need a preheat step after the first water-based base coating composition is applied, which provides energy saving and reduction of CO 2 emissions in coating steps. In addition, the present invention has advantages of facility cost and coating line spaces. | Provided is a method for forming a multilayer coating film, said method being suitably applicable to a wet-on-wet coating process comprising: applying a first water-borne base coating material to form an uncured first water-based base coating; and then applying a second water-based base coating material without preheating the uncured first water-borne base coating. A method for forming a multilayer coating film according to a wet-on-wet coating process which comprises applying a first water-based base coating material to the surface of a substrate to be coated and then applying, without preheating the thus formed coating, a second water-based base coating material, characterized in that: the first water-borne base coating material contains a hydrophilic association-type viscous material; and the composition of the second water-based base coating material is controlled. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a division of U.S. patent application Ser. No. 404,953, filed Oct. 10, 1973, which in turn is a Rule 60 Division of U.S. patent application Ser. No. 203,869, filed Dec. 1, 1971, now U.S. Pat. No. 3,787,409, issued Jan. 22, 1974.
BRIEF SUMMARY OF THE INVENTION
The invention relates to compounds characterized by the formula ##SPC1##
Wherein R is lower alkoxy, and addition salts thereof with pharmaceutically acceptable acids. The compounds of formula I are useful as potentiators of the antibacterial activity of sulfonamides, as well as antibiotics.
DETAILED DESCRIPTION OF THE INVENTION
The invention relates to compounds characterized by the formula ##SPC2##
Wherein R is lower alkoxy, which preferably has from 1 to 7 carbon atoms, for example, methoxy, ethoxy, propoxy, butoxy, pentoxy, and the like.
The most preferred embodiment of the invention is 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine.
The compounds of formula I are prepared in accordance with the process illustrated by the following reaction scheme: ##SPC3##
Wherein R is as previously described and R 1 and R 2 are lower alkyl of 1-7 carbon atoms; methyl is preferred.
The foregoing reaction is carried out by first reacting an aldehyde of formula II with a β-lower alkoxy propionitrile of formula III in the presence of an alkali metal lower alkoxide, such as sodium methoxide, potassium ethoxide, etc. and a lower alkanol of the formula R 2 OH, e.g., methanol, ethanol, propanol, etc. The reaction temperature is not critical, but it is generally in the range of about 60° to about 140°C. The reaction product obtained is a compound of formula IV which is readily converted into a compound of formula V by treatment with R 2 OH in the presence of an alkali metal lower alkylate under substantially anhydrous conditions. The reaction temperature is also not critical for this step, and temperatures of about 60° to about 140°C. are suitable here also. A compound of formula V is then reacted with guanidine, in the presence of a solvent, if required, to give an almost quantitative yield of a compound of formula I.
The aldehydes of formula II are known compounds or can readily be prepared by known techniques, for example, by the Rosenmund method (Organic Synthesis, I.C., p. 1332), or by the method of W. Bonthrone and J. W. Cornforth, J. Chem. Soc. (c) 1202 (1969).
The compounds of formula I form acid addition salts and such salts are also within the scope of this invention. Thus, the compounds of formula I form pharmaceutically acceptable addition salts with, for example, both pharmaceutically acceptable organic and inorganic acids, such as acetic acid, succinic acid, formic acid, methanesulfonic acid, p-toluene-sulfonic acid, hydrochloric acid, nitric acid, phosphoric acid, sulfuric acid, lactic acid, and the like.
The compounds of formula I are useful in combination with one or more sulfa drugs, such as, for example, N 1 -(3,4-dimethyl-5-isoxazolyl)-sulfanilamide, 5-methyl-3-sulfanilamido-isoxazole, N 1 -(2,6-dimethoxy-4-pyrimidinyl)-sulfanilamide, N 4 -ethoxyacetyl-N 1 -(5-methyl-3-isoxazolyl)-sulfanilamide, N 1 -(4,5-dimethyl-3-isoxazolyl)-sulfanilamide, N 1 -(5,6-dimethoxy-4-pyrimidinyl)-sulfanilamide, and the like, as antibacterial agents. The addition of a compound of formula I to one of the above-mentioned sulfonamides results in a marked potentiation of the anti-bacterial activity of the sulfonamide. Thus, the compounds of formula I are useful as potentiators of sulfonamides. The combination of a compound of formula I and a sulfonamide is prepared simply by admixture, which can ultimately be embodied into a suitable oral dosage form, as hereinafter described. Unexpectedly, the compounds of formula I also potentiate the anti-bacterial activity of antibiotics, such as, for example, oxytetracycline, penicillin and the like. Thus, the compounds of formula I are also useful as potentiators of antibiotics. The combination of a compound of formula I and an antibiotic is prepared simply by admixture, which can ultimately be embodied into a suitable oral dosage form, as hereinafter described.
The ratios in which a therapeutically active compound of formula I and a sulfonamide are utilized can be varied within wide limits. For example, the combination can contain from about 1 to about 50 parts, preferably from about 1 to about 20 parts, of sulfonamide or an equivalent amount of salt thereof to one part of a compound of formula I or equivalent amount of salt thereof.
The ratios in which a therapeutically active compound of formula I and an antibiotic are utilized can be varied within wide limits. For example, the combination can contain from about 1 to about 50 parts, preferably from about 1 to about 20 parts, of antibiotic or an equivalent amount of salt thereof to one part of a compound of formula I or equivalent amount of salt thereof.
The products of the invention can be incorporated into standard pharmaceutical dosage forms, for example, they are useful for oral or parenteral application with the usual pharmaceutical adjuvant material, for example, organic or inorganic inert carrier materials such as water, gelatin, lactose, starch, magnesium stearate, talc, vegetable oils, gums, polyalkyleneglycols, and the like. The pharmaceutical preparations can be employed in a solid form, for example, as tablets, troches, suppositories, capsules or in liquid form, for example, as solutions, suspensions or emulsions. The pharmaceutical adjuvant material can be added and can include preservatives, stabilizers, wetting or emulsifying agents, salts to change the osmotic pressure or to act as buffers. They can also contain other therapeutically active materials. The combination of a compound of formula I and a sulfonamide can be administered in unit dosage forms which contain 500 mg. of sulfonamide or an equivalent amount of a salt thereof and from about 10 mg. to about 100 mg. of a compound of formula I or an equivalent amount of a salt thereof. However, it is also within the scope of the invention to utilize a unit dosage form which will contain from about 250 mg. to about 750 mg. of sulfonamide or equivalent amount of a salt thereof and from about 5 mg. to about 150 mg. of a compound of formula I or equivalent amount of a salt thereof.
The combination of a compound of formula I and an antibiotic can be administered in dosage forms which contain 250 mg. of antibiotic or an equivalent amount of a salt thereof and from about 5 mg. to about 50 mg. of a compound of formula I or an equivalent amount of a salt thereof. However, it is also within the scope of the invention to utilize a unit dosage form which will contain from about 250 mg. to about 750 mg. of antibiotic or equivalent amount of a salt thereof and from about 5 mg. to about 150 mg. of a compound of formula I or an equivalent amount of salt thereof.
The frequency with which any such unit dosage will be administered to a warm-blooded animal will vary, depending upon the quantity of medicament present therein and the needs and requirements of the warm-blooded animal.
The sulfonamides hereinbefore described form salts with pharmaceutically acceptable bases, for example, they form salts with alkali metal bases, such as, for example, sodium hydroxide, potassium hydroxide or the like.
The following examples further illustrate the invention. All parts are by weight and all temperatures are in degrees Centigrade, unless otherwise mentioned.
EXAMPLE 1
Preparation of 3-methoxy-4,5-methylenedioxy-α-methoxymethylcinnamonitrile
3.8 g. of sodium were dissolved in 120 ml. of methanol under reflux. 56 g. of methoxypropionitrile and 60 g. of 3-methoxy-4,5-methylenedioxybenzaldehyde were then added and refluxed in the methanol mixture for 5 hours. Upon chilling, 3-methoxy-4,5-methylenedioxy-α-methoxymethyl-cinnamonitrile crystallized in needles of m.p. = 115°, in a yield of 68 g. = 83 percent. A sample of analysis was recrystallized from methanol, m.p. 115.5°-116.5°.
Analysis - C 13 H 13 NO 4 : Calc'd: C, 63.2; H, 5.26; N, 5.67. Found: C, 63.15; H, 5.22; N, 5.62.
EXAMPLE 2
Preparation of 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine
12.8 g. of sodium were dissolved in 185 ml. of methanol, under stirring and reflux. 68 g. of 3-methoxy-4,5-methylenedioxy-α-methoxymethylcinnamonitrile were added and the mixture was refluxed for 48 hours. The reactant dissolved gradually, and the solution darkened. Thereafter, the reaction was quenched with 500 ml. of water and neutralized with 20 ml. of acetic acid, followed by extraction with three portions of benzene, i.e., 600 + 50 + 50 ml. The benzene layer was dried over sodium sulfate and cleared by filtering it through a filter containing charcoal. The solvent was evaporated in vacuo and the residue removed by distillation at 184°-198°, 1.5 mmHg. The product was a viscous colorless oil of n D 22 = 1.5320. 41 g. was refluxed with 290 ml. of 1 molar methanolic guanidine solution for 1.5 hours. The methanol was then removed by distillation over an oil bath at 160° and the residue kept at that temperature until it solidified to a crystalline mass (10-15 min.). Thereafter, the product was slurried with water and filtered by suction. Yield of the crude product was 37 g. = 92 percent, m.p. unsharp 215°.
To purify the crude product it was slurried with 120 ml. of acetic acid and heated until it had dissolved. Upon cooling, the acetate crystallized as white needles which were pressed off on a suction filter and dissolved in 250 ml. of hot water. The solution was charcoaled and the 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine precipitated with an excess of ammonia, m.p. = 236°-237°, yield 28.5 g. = 70 percent.
Analysis - C 13 H 14 N 4 O 3 : Calc'd: C, 56.9; H, 5.11; N, 20.45. Found: C, 56.67; H, 5.27; N, 20.35.
EXAMPLE 3
Preparation of 3-ethoxy-3,4-methylenedioxy-α-methoxymethylcinnamonitrile
To a solution containing 2.16 g. of sodium in 100 ml. methanol, there were added 32 g. of β-methoxypropionitrile and 36.5 g. of 3-ethoxy-4,5-methylenedioxy benzaldehyde. Thereafter, the mixture was refluxed for 6.5 hours. 300 ml. of water were added and the 3-ethoxy-3,4-methylenedioxy-α-methoxymethylcinnamonitrile was extracted with methylenechloride. Upon evaporation of the solvent and vacuum distillation, the 3-ethoxy-3,4-methylenedioxy-α-methoxymethyl-cinnaminonitrile had a b.p. of 175°/0.3 mmHg and m.p. of 64°-65°.
Analysis - C 14 H 15 NO 4 Calc'd: C, 64.36; H, 5.79; N, 5.36. Found: C, 64.57; H, 5.83; N, 5.28.
EXAMPLE 4
Preparation of 3-ethoxy-4,5-methylenedioxy-α-cyanodihydrocinnamaldehyde dimethylacetal
To 6.6 g. sodium dissolved in 96 ml. of methanol, 37.5 g. of 3-ethoxy-4,5-methylenedioxy-α-methoxymethylcinnamonitrile were added. The resulting mixture was refluxed for 24 hours. The solution was poured into 400 ml. water and was extracted with methylenechloride. Upon evaporation of the solvent, the product, 3-ethoxy-4,5-methylenedioxy-α-cyanodihydrocinnamaldehyde dimethylacetal, was vacuum distilled and had a b.p. of 191°/0.4 mmHg., n D 23 = 1.5340.
Analysis - C 15 H 19 NO 5 Calc'd: C, 61.41; H, 6.53; N, 4.78. Found: C, 62.23; H, 6.17; N, 4.78.
EXAMPLE 5
Preparation of 2,4-diamino-5-(3-ethoxy-4,5-methylenedioxybenzyl)pyrimidine
30.5 g. of 3-ethoxy-4,5-methylenedioxy-α-cyanodihydrocinnamaldehyde dimethylacetal were added to 200 ml. of freshly prepared 0.2 molar solution of guanidine in methanol, and the solvent was gradually removed by distillation over an oil bath at a temperature of 120°-140°. The residue was heated for 10 minutes to 140°-160° and it completely solidified to a crystalline mass. For purification, the mass was dissolved in 100 ml. hot acetic acid and the product allowed to crystallize as an acetate upon chilling. The latter was filtered by suction, dissolved in 400 ml. of hot water and the solution alkalized with ammonia to precipitate 2,4-diamino-5-(3-ethoxy-4,5-methylenedioxybenzyl)pyrimidine as white crystals of free base having a m.p. of 202.5°-203.5°.
Analysis - C 14 H 16 N 4 O 3 Calc'd: C, 58.32; H, 5.59; N, 19.44. Found: C, 58.51; H, 5.72; N, 19.69.
The starting material 3-ethoxy-4,5-methylenedioxy benzaldehyde was obtained by methylenation of 3-ethoxy-4,5-dihydroxybenzaldehyde essentially by the method of W. Bonthrone and J. W. Cornforth, J. Chem. Soc. (C) 1202 (1969).
White crystals, m.p. of 60°-61°, b.p. of 103°-104°/0.1 mmHg.
Analysis - C 10 H 10 O 4 Calc'd: C, 61.85; H, 5.19. Found: C, 61.70; H, 5.18.
3-ethoxy-4,5-dihydroxybenzaldehyde was obtained from 3-ethoxy-4-hydroxy-5-bromobenzaldehyde, P. Mariella and J. M. Bauer, J. Org. Chem. 23: 120 (1958) in analogy to Bradley, Robinson and Schwarzenback, J. Chem. Soc. 811 (1930), white crystals, from water, m.p. of 117°-118°.
Analysis - C 9 H 10 O 4 Calc'd: C, 59.33; H, 5.53. Found: C, 59.65; H, 5.52.
EXAMPLE 6
Capsule Formulation______________________________________ Per CapsuleN.sup.1 -(3,4-dimethyl-5-isoxazolyl)-sulfanilamide 250 mg.2,4-diamino-5-(3-methoxy-4,5-methylene-dioxybenzyl)pyrimidine 25 mg.Lactose 68 mg.Corn Starch 27 mg.Talc 5 mg.Total weight 375 mg.______________________________________
Procedure:
1. The N 1 -(3,4-dimethyl-5-isoxazolyl)-sulfanilamide, 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine, lactose and corn starch are mixed in a suitable mixer.
2. The mixture is further blended by passing through a comminuting machine with a No. 1A screen with knives forward.
3. The blended powder is returned to the mixer, the talc added and blended thoroughly. The mixture is then filled into No. 4 hard shell gelatin capsules on a capsulating machine.
EXAMPLE 7
Capsule Formulation______________________________________ Per CapsuleOxytetracycline 250 mg.2,4-Diamino-5-(3-methoxy-4,5-methylene-dioxybenzyl)-pyrimidine 25 mg.Lactose 68 mg.Corn Starch 27 mg.Talc 5 mg.Total Weight 375 mg.______________________________________
Procedure:
1. The oxytetracycline, 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine, lactose and corn starch are mixed in a suitable mixer.
2. The mixture is further blended by passing through a comminuting machine with a No. 1A screen with knives forward.
3. The blended powder is returned to the mixer, the talc added and blended thoroughly. The mixture is then filled into No. 4 hard shell gelatin capsules on a capsulating machine.
EXAMPLE 8
Tablet Formulation______________________________________ Per TabletN.sup.1 -(3,4-dimethyl-5-isoxazolyl)-sulfanilamide 225 mg.2,4-Diamino-5-(3-methoxy-4,5-methylene-dioxybenzyl)pyrimidine 60 mg.Lactose 233 mg.Corn Starch 100 mg.Gelatin 12 mg.Talc 15 mg.Magnesium Stearate 5 mg.______________________________________
Procedure:
1. 2,4-Diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine, N 1 -(3,4-dimethyl-5-isoxazolyl)sulfanilamide, corn starch and lactose are thoroughly mixed in suitable blending equipment and granulated with a 10 percent gelatin solution.
2. The moist mass is passed through a No. 12 screen, and the granules are dried on paper-lined trays overnight.
3. The dried granules are passed through a No. 14 screen and placed in a suitable mixer. The talc and magnesium stearate are added and blended.
4. The granulation is compressed into tablets weighing approximately 650 mg. each, using punches having an approximate diameter of 12.7 mm. (1/2 inch). The final tablet thickness is about 5.35 mm.
EXAMPLE 9
Tablet Formulation______________________________________ Per TabletOxytetracycline 225 mg.2,4-Diamino-5-(3-methoxy-4,5-methylene-dioxybenzyl)pyrimidine 60 mg.Lactose 233 mg.Corn Starch 100 mg.Gelatin 12 mg.Talc 15 mg.Magnesium Stearate 5 mg.______________________________________
Procedure:
1. 2,4-Diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine, oxytetracycline, corn starch and lactose are thoroughly mixed in suitable blending equipment and granulated with a 10 percent gelatin solution.
2. The moist mass is passed through a No. 12 screen, and the granules are dried on paper-lined trays overnight.
3. The dried granules are passed through a No. 14 screen and placed in a suitable mixer. The talc and magnesium stearate are added and blended.
4. The granulation is compressed into tablets weighing approximately 650 mg. each, using punches having an approximate diameter of 12.7 mm. (1/2 inch). The final tablet thickness is about 5.35 mm.
EXAMPLE 10
Suspension Formulation______________________________________ Gm. Per LiterMethylparaben 0.9Propylparaben 0.5Sodium Edetate 0.1Lactic Acid 85% 8.3 cc.2,4-Diamino-5-(3-methoxy-4,5-methylene-dioxybenzyl)pyrimidine 5.1Complex magnesium aluminum silicate 26.4Sodium Benzoate 2.5Sucrose 400.0Sorbitol solution U.S.P. 110.0Tragacanth 3.5Methyl cellulose 0.3Sorbitan monolaurate 0.035N.sup.1 -(3,4-dimethyl-5-isoxazolyl)sulfanilamideUltra Fine 118.29Glycerin 125.0FD and C Yellow No. 5 0.016Banana Flavor 0.16NaOH -- 40% Solution q.s. to pH 5.1Distilled Water q.s. 1000.0 cc.______________________________________
Procedure:
1. The methyl and propyl parabens, sodium edetate and lactic acid are dissolved in 750 cc. of boiling distilled water. The 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)-pyrimidine is added with stirring.
2. The complex magnesium aluminum silicate is then added and cooked for 1 hour in a water bath at 80°-85°C.
3. The sodium benzoate is dissolved in 30 cc. of water and added to the mixture. The sucrose and sorbitol solution U.S.P. are then added.
4. The tragacanth is added to the glycerin with high shear and then added to the mixture with high mix.
5. The methyl cellulose is dissolved in 525 cc. of water, heated to 60°-65°C. and mixed for 10-15 minutes. The sorbitan monolaurate is dissolved in 15 cc. of heated water and added to the methyl cellulose solution. N 1 -(3,4-dimethyl-5-isoxazolyl)sulfanilamide is added with high shear--when this is uniform, it is added to the mixture.
6. The colors and flavors are added when needed.
7. The pH is brought to 5.1 with 40% NaOH and the mixture brought to volume.
8. The mixture stands overnight before versating and homogenizing.
EXAMPLE 11
The unexpectedly increased antibacterial activity of antibiotics and, for example, N 1 -(3,4-dimethyl-5-isoxazolyl)sulfanilamide, when combined with 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine in the treatment of various bacterial infections was demonstrated utilizing the procedure set forth hereinbelow.
Swiss albino mice weighing 18 to 20 grams were infected intraperitoneally with 100 to 1000 minimal lethal doses of the organism. The inoculum was obtained from a properly diluted overnight broth culture. In all infections except D. pneumoniae, S. pyogenes and K. pneumoniae, the inoculum was finally diluted in 5 percent hog gastric mucin.
For all infections, the test animals were treated orally by gavage with 1.0 ml. of the desired concentration of the single drug or the appropriate sulfonamide-pyrimidine combination in 1 percent carboxymethylcellulose. Treatment consisted of a total of 6 doses. Two treatments, 5 hours apart, were administered on the day of and the day following infection and one treatment on the second and third days following infection. The first dose was administered 5-10 minutes after infection. When combinations were administered, varying concentrations of sulfonamide or antibiotic were prepared in the presence of an inactive concentration of a potentiator of the invention. The experimental observation period was 14 days. Heart blood from mice succumbing during this period of time was cultured on appropriate solid media to determine the presence or absence of the infecting organism.
Results obtained are given in Tables I and II.
TABLE I__________________________________________________________________________(The antibacterial effect of N.sup.1 -(3,4-dimethyl-5-isoxazolyl)sulfanilamide in combinationwith e.g., 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidineagainstbacterial infections in mice is set forth below.) Dose: mg/kg..sup.b Increased Activity.sup.a of N.sup.1 - 2,4-diamino-5-(3-methoxy- (3,4-dimethyl-5-isoxazole) 4,5-methylenedioxybenzyl) sulfanilamide (x-fold Organism pyrimidine potentiation)__________________________________________________________________________D. pneumoniae No. 6301 50 >11.9 25 11 10 >2.3S. pyogenes 4 50 >31.3 25 3.9 10 1.4S. aureus Smith 5 2.1E. coli 257 10 >5.7K. pneumoniae A 5 2.3P. vulgaris 190 10 9.1 5 2.9S. typhosa P. 58a 5 2.5__________________________________________________________________________ Dose Sulfonamide alone.sup.a Increased Activity (x-fold) = Dose Sulfonamide in Combination .sup.b These doses of 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine when administered alone are inactive.
TABLE II__________________________________________________________________________The antibacterial effect of Penicillin or Oxytetracycline HCl incombination with 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine against bacterialinfections in mice is set forthbelow. Dose: mg/kg..sup.b Increased activity.sup.a Increased activity.sup.a 2,4-diamino-5-(3-methoxy- of Penicillin (x-fold of Oxytetracycline 4,5-methylenedioxybenzyl) potentiation) HCl (x-fold Organism pyrimidine potentiation)__________________________________________________________________________D. pneumoniae No. 6301 50 -- 4.0S. pyogenes 4 50 -- 2.7E. coli 257 50 3 3.8S. schottmuelleri 50 >4.2 10.7__________________________________________________________________________ Dose Antibiotic alone.sup.a Increased Activity (x-fold) = Dose Antibiotic in combination .sup.b These doses of 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine when administered alone are inactive | 2,4-Diamino-5-(3-alkoxy-4,5-methylenedioxybenzyl)pyrimidines, such as, for example, 2,4-diamino-5-(3-methoxy-4,5-methylenedioxybenzyl)pyrimidine, prepared from the corresponding benzaldehydes, are described. The end products are useful as potentiators of the antibacterial activity of sulfonamides, as well as antibiotics. | 2 |
RELATED APPLICATIONS
[0001] This application claims the benefit under 37 C.F.R. §119 of prior filed, co-pending Provisional Application No. 60/072,248, filed on Jan, 22, 1998.
BACKGROUND OF THE INVENTION
[0002] The present invention generally relates to displaying of physiological data on patient monitors. More particularly, the present invention relates to a method and apparatus of correcting for phase error induced by down sampling of physiological data.
[0003] Patient physiological data, such as ECG data, is commonly displayed on patient monitors as a waveform suitable for review by medical care personnel. In order for medical care personnel to correctly assess the clinical import of the displayed information, it is highly desirable that the waveforms accurately reflect the measured physiological data regardless of the monitor type, pixel resolution, the size of the window in which the waveforms or other data are displayed or the speed at which the data is sampled. Generally, this has required some specific scale factor to be employed for each monitor type, pixel resolution capacity or display window size being employed.
SUMMARY OF THE INVENTION
[0004] One source of waveform distortion results from symmetrically plotting non-uniformly spaced selected data points in down-sampled data. When down-sampling data, features of the waveform in the original data may be lost or distorted by the down-sampling process. For example, the resolution of a standard cathode ray tube (CRT) monitor is not adequate for presenting full resolution ECG data. ECG data is typically received from the patient at a rate of about 480 Hertz (Hz) 3 . The ECG data is filtered for electrical noise and other extraneous electrical information, reducing the data rate to about 240 Hz and presented to the clinician using a standard scroll rate of 25 millimeters (mm) per second (sec). A scroll rate of 25 mm/sec is a standard within the health care industry. A typical 21″ CRT monitor displays a horizontal image size of approximately 406.4 mm with a horizontal screen resolution of 1280 pixels, or 3.15 pixels/mm. At a scroll rate of 25 mm/sec, each pixel represents approximately 12.7 milliseconds (ms) of data. Thus, if data is received at a 240 Hz rate, a data point is displayed on the CRT every 4.167 ms. This means that 3.05 data points will map to the same horizontal pixel location on the CRT. If the data is received at a different rate, e.g., 120 Hz (such as is the case with blood pressure waveforms) 1.52 data points will map to the same horizontal pixel location on the CRT. Plotting data as a waveform in this manner results in the plotting of different data points on the same pixel location. As a result, important physical features of the waveform representing the data may be lost.
[0005] Accordingly, the invention provides an interface for accurately displaying non-uniformly spaced selected data points in down-sampled data for a computer monitor display.
[0006] According to one aspect of the invention, a method and apparatus for synchronously plotting non-uniformly spaced selected data points in down-sampled data is provided. A data signal is received at a first rate and separated into at least one data window. Each data window has a predetermined number of data points having respective values. At least one of either a minimum and a maximum value of the data points are identified, thus identifying a position of the one of the minimum and maximum value relative to a reference. The data point is then displayed having the one of the minimum and maximum value at the position.
[0007] The invention also provides an apparatus having an input for receiving a data signal sampled at a first rate and means for converting the data signal to a second data signal sampled at a second lower rate and for displaying the second data signal on a video monitor.
[0008] It is an advantage of the invention to provide an interface for accurately displaying non-uniformly spaced selected data points in down-sampled data for a computer monitor display.
[0009] It is another advantage of the invention to provide a method and apparatus for synchronously plotting non-uniformly spaced selected data points in down-sampled data.
[0010] Other features and advantages of the invention will become apparent to those skilled in the art upon review of the following description, claims and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] [0011]FIG. 1A illustrates a prior art waveform wherein non-uniformly spaced data is plotted at fixed, regularly spaced intervals on the CRT.
[0012] [0012]FIG. 1B illustrates the same waveform produced by use of the present invention, plotting non-uniformly spaced data at varying intervals according to the invention.
[0013] [0013]FIG. 2 is a block diagram illustrating a patient monitoring system according to the invention.
[0014] [0014]FIG. 3 is a flow chart illustrating the method of the invention.
[0015] Before one embodiment of the invention is explained in detail, it should be understood that the invention is not limited in its application to the details of the apparatus, composition or concentration of components, or to the steps or acts set forth in the following description. For example, the invention is capable of embodiments other than those adopted particularly for healthcare applications. Also, it should be understood that the phraseology and terminology used herein is for the purpose of description and should not be regarded as limiting.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0016] [0016]FIG. 2 illustrates the patient monitoring system 32 of the invention. The patient monitoring system 32 acquires and displays physiological patient data. While the monitoring system 32 can be used in connection with monitoring any kind of physiological parameter, in the preferred embodiment, the monitoring system 32 is for monitoring a patient's electrical cardiac activity and blood pressure. Monitoring system 32 is coupled to the patient 36 by an array of sensors or transducers which may include, for example, electrodes 40 mounted on the patient's chest and arm for electrocardiogram testing. Hereinafter, the term “sensor” and “transducer” will be used synonymously, and each term will be defined as including the subject matter of the other term.
[0017] The signals derived from the sensors are converted from analog form to digital form by an analog to digital converter (A/D) 44 and provided to a converter 60 that prepares the data for display on a display monitor 52 . In the embodiment in FIG. 2, the A/D 44 further includes a pre-processor. The digital conversion by the A/D 44 is done at a rate of 480 Hz. The pre-processor then separates and filters the 480 Hz data into packets to be processed by the converter 60 . Electrical noise and other extraneous electrical signals are filtered before the data is presented to the converter 60 . The data rate after pre-processing is about 240 Hz. In other embodiments (not shown), if the signal collection rate is equal to or less than the rate at which the converter processes the data, the act of separating the data into packets by the pre-processor may be avoided.
[0018] The display monitor 52 is a conventional computer-style display monitor having a generally rectangular cathode ray tube (CRT). The CRT includes a plurality of pixels. The vertical location of the pixels is defined by a Y-coordinate and the horizontal location of the pixels is defined by an X-coordinate. As is known in the art, each pixel is capable of being energized electronically so that the pixel emits light visible to the user of the monitoring system.
[0019] [0019]FIG. 3 is a flowchart illustrating the operation of the patient monitoring system. The system collects physiological data ( 56 ) and pre-processes the data to a first rate, and converts the analog physiological data to digital data using an A/D converter. The converter ( 60 ) samples the collected, pre-processed physiological data 56 at a second rate, also called the update rate. The converter 60 may be resident in a stand alone bed-side computer system, or the converter 60 may be resident in a common network computer where physiological data from multiple patients may be centrally processed. The converter 60 generates a data signal having data points that are at approximately the same position as the data points had relative to one another in the originally sampled physiological data. In the converter 60 , the data signal is typically temporarily stored ( 62 ) in a buffer until the data is processed. For ECG data, the data collection rate, or the sample rate, is about 240 Hz. For Blood Pressure (BP) data, the sample rate is about 120 Hz. The update rate operates at a predetermined speed. For all waveforms, including those composed of ECG and BP data, the update rate is about 60 Hz, although it is contemplated that other update rates may be used.
[0020] The collected physiological data is separated into portions or data windows, which are then extracted ( 64 ) from the buffer ( 62 ) to be processed. The number of data points comprising the data window is equal to the sample rate divided by the update rate. Thus, for ECG data, the data window is 240 Hz/60 Hz, or four data points. This is equal to about one point for every 16.667 ms of data.
[0021] In order to preserve the overall shape of the waveform, data points must be selected that best represent the waveform. Thus, the data window is down-sampled ( 66 ) by selecting, on the average, one data point from each data window. In one embodiment, the data point chosen is one of either a local minimum or a local maximum data point. In another embodiment, two data windows (comprising eight points) are considered together. This accommodates for situations in which it is desirable to choose more than one data point from within a single data window. If more than one data point is chosen within a single data window, no data points are chosen from the adjacent data window. Choosing more than one point in a single data window accommodates for situations in which more than one relative minimum or maximum data point occurs within a single data window, and no relative minimum or maximum data points occur in the adjacent data window. Thus, when two data windows are considered together, two of the eight data points comprising the two adjacent data windows are selected—the local minimum data point and the local maximum data point. In this manner, the overall shape of the waveform is best preserved.
[0022] In the original 240 Hz data stream, each data point is separated by a uniform 4.1667 ms, and each data window of four points is separated by a uniform 16.667 ms. However, as a result of down sampling, the resulting series of data points is not uniformly spaced. Thus, using the last data point of a data window as a reference, a time off-set for each data point is calculated ( 70 ). The time off-set is the time difference (or phase error) per point that is induced by fixed space plotting. The time off-set (in milliseconds) is calculated using the equation:
Time Off-Set ms =[( R s /R u )− i ]*1000/ R s
[0023] where, R s is the sample rate (240 Hz), R u is the update rate (60 Hz), i is the index number of the selected point, and 1000/R s is the time separation between points in ms (for ECG, 1000/240 HZ=4.167 ms). The time off-sets for ECG data sampled at 240 Hz and operating at an update rate of 60 Hz are shown below:
Data Point Selected Time Off-Set 4 0 ms 3 4.167 ms 2 8.333 ms 1 12.5 ms
[0024] A position to plot a data point is then determined ( 74 ), and plotted ( 78 ). The position to plot a data point is determined by moving from the current position by an amount equivalent to the time off-set for that data point. For example, if data point 4 is chosen from the first data window, and data point 3 is chosen from the second data window, the plot position for data point 3 is determined by moving forward the time off-set of four data points (16.667 ms), and then moving back by the time off-set of one data point (i.e., from the time of Data Point 4 to the time of Data Point 3), or 4.167 ms. Thus, data point 3 of the second data window is plotted 16.667 ms−4.167 ms, or 12.5 ms from data point 4 of the first data window. Moving forward by 16.667 ms is based on the update rate of 60 Hz. Moving forward at a constant 16.667 ms allows the multiple waveforms to be updated synchronously.
[0025] After a data point is plotted, the next data window of physiological data is extracted ( 64 ) from the buffer ( 62 ). The process is repeated until all of the data is processed.
[0026] Multiple waveforms may also be displayed in any given window. Because real time data is being displayed, a constant, periodic update is preferred. If the update to the display is not constant, a noticeable jerkiness may be apparent to the human eye. In addition, each of the waveforms on the display will potentially have different points selected within the data window. The update rate, however, is constant for all waveforms plotted. Thus, the presentation for all of the waveforms on the display is moved forward at a fixed rate, and the display is updated with all data that has occurred since the previous update.
[0027] [0027]FIG. 1A illustrates an ECG waveform 6 and a blood pressure waveform 8 wherein non-uniformly spaced 60 Hz data is plotted at fixed, regularly spaced intervals on the CRT as is done in the prior art. Plotting in such a fashion (in effect) shifts the data points relative to one another resulting in distortion of the waveform's shape.
[0028] As shown in FIG. 1A, general distortion due to small, rapid variations in the size, shape or position of observable information may occur, as indicated by the region of the waveform indicated by reference numeral 10 . Distortion of the QRS width may occur, as illustrated by reference numeral 14 . Aberrations of the size or position of tips of waveforms may also occur, as indicated by the elongated and flat tips shown by reference numeral 16 . Waveform peaks may also appear tilted or distorted, as indicated by reference numeral 20 . Further, time, amplitude, frequency or phase related jitter may be present, as indicated by the change in slope of the waveform shown by reference numeral 24 .
[0029] [0029]FIG. 1B illustrates a waveform produced using the down sampling technique of the present invention. In FIG. 1B, non-uniform data points are plotted as they occur, i.e., at uneven spacing as calculated by converter 60 . As shown, the ECG data as plotted according to the invention contains sharp QRS spikes 26 that play an important roll in the assessment of a patient's condition.
[0030] Thus, the plotting of physiological data using the present invention minimizes distortions and aberrations caused by down-sampling the rapid variations inherent in physiological data, and is more reflective of the true waveform, providing a more accurate depiction of features such as QRS width, tips and peaks present of the waveform, and slope variations of the waveform.
[0031] Various features of the invention are set forth in the following claims. | A method and apparatus of correcting a data signal sampled at a first rate to a data signal displayed on a video monitor at a second rate is claimed. A data signal is received at a first rate. The data signal is separated into data windows. The minimum and maximum values and positions of data points in data windows are identified relative to a reference, and displayed on a video monitor. | 0 |
RELATED APPLICATION
[0001] This application claims priority under 35 U.S.C. §119(e) from Provisional Application No. 61/233,600 filed Aug. 13, 2009 which is incorporated by reference in its entirety.
FIELD OF THE DISCLOSURE
[0002] This disclosure relates in general to an electronic device. In particular, it relates to a method and apparatus having a drive scheme to minimize luminescent efficiency losses.
BACKGROUND INFORMATION
[0003] Increasingly, active organic molecules are used in electronic devices. These active organic molecules have electronic or electro-radiative properties including electroluminescence. Electronic devices that incorporate organic active materials may be used to convert electrical energy into radiation and may include a light-emitting diode, light-emitting diode display, or diode laser.
[0004] One common characteristic of devices employing active organic molecules is a significant loss of luminance in the first few hours of operation, typically from 5 to 30% loss within the first 5 hours of operation. While different materials show varying degrees of initial loss of luminance, the electronic devices using these materials exhibit this effect efforts are ongoing to address this problem. One solution is to use a burn-in process to induce an initial luminance drop before the electronic devices complete the manufacturing process. This “burn-in” process can be achieved by operating the electronic device at high temperature, or high current, for a designated time to induce the required initial drop in luminance. At least two problems result from the use of the burn-in process. One being the permanent lowering of device efficiency, and the second being the additional process step required for manufacturing, resulting in higher costs for a large volume manufacturing process.
[0005] Alternatives are sought for avoiding the burn-in process to reduce costs and mitigate the efficiency loss. Applications such as organic light-emitting diode (“OLED”) displays and general lighting are just beginning to make inroads into consumer goods, and volume production will be increasing every year for many years to come.
[0006] One method of manufacturing OLED devices involves forming discreet pixel areas comprising several layers, including organic active material. These pixels can be a single pixel, or composed of two or more sub-pixels, for example, red, green and blue sub-pixels can be used to form a single pixel in a display application. These pixels are typically connected directly to a power bus to provide a voltage potential across the pixel and resultant luminescence
[0007] There continues to be a need for improved devices for reducing initial drop in luminance in display and lamp applications.
SUMMARY
[0008] In one embodiment the apparatus and method provide for a first and second electrode, with one of the electrodes being an anode and one electrode being a cathode. An organic active material, described in more detail below, forms an electrical connection with the first and second electrodes to form a unit. In one embodiment this unit is a pixel. Each pixel can be formed from at least two sub-pixels, and in one embodiment three sub-pixels form a pixel, with red, green and blue emissive spectrums. Electrical power is delivered non-continuously, or pulsed, to the unit. In one embodiment the pulsing can be distinct for each pixel, sub-pixel or set of pixels. The pulsing rate can vary from 50 Hz up to 1,000 Hz, and the duty cycle, or percentage of time the power is “ON” is 30 to 95%. In one embodiment the pulsing rate and duty cycle can produce many different scenarios, including alternating cycles of “ON-OFF”, or several cycles of “ON” followed by one or more cycles of “OFF”, and various other combinations to produce the stated pulsing rate and duty time.
[0009] In one embodiment the apparatus and method can be an Organic Light Emitting Diode (OLED) as a display for electronic devices such as cell phones, PDA's, GPS's, music devices, desktop and laptop computers. In another embodiment the OLED can be a lamp for general lighting purposes in either indoor or outdoor applications.
[0010] In one embodiment, a substrate (such as glass) is useful as a base for the electronic device. The term “organic electronic device” or sometimes just “electronic device”, is intended to mean a device including one or more organic semiconductor layers or materials. An organic electronic device includes, but is not limited to: (1) a device that converts electrical energy into radiation (e.g., a light-emitting diode, light emitting diode display, diode laser, or lighting panel), (2) a device that detects a signal using an electronic process (e.g., a photodetector, a photoconductive cell, a photoresistor, a photoswitch, a phototransistor, a phototube, an infrared (“IR”) detector, or a biosensors), (3) a device that converts radiation into electrical energy (e.g., a photovoltaic device or solar cell), (4) a device that includes one or more electronic components that include one or more organic semiconductor layers (e.g., a transistor or diode), or any combination of devices in items (1) through (4).
BRIEF DESCRIPTION OF THE FIGURES
[0011] FIG. 1 is an illustration of an electronic device.
[0012] FIG. 2 is an illustration of one embodiment of waveforms used to produce pulsed electrical power.
[0013] FIG. 3 is an illustration of one embodiment where pulsed power is compared to continuous power application.
[0014] FIG. 4 is an illustration of one embodiment where improvement in duty cycles vs. continuous power is provided for initial luminance drop values.
DETAILED DESCRIPTION
[0015] One example of an electronic device comprising an organic light-emitting diode (“OLED”), is shown in FIG. 1 and designated 100 . The device has an anode layer 110 , a buffer layer 120 , a photoactive layer 130 , and a cathode layer 150 . Adjacent to the cathode layer 150 is an optional electron-injection/transport layer 140 . Between the buffer layer 120 and the photoactive layer 130 , is an optional hole-injection/transport layer (not shown).
[0016] As used herein, the term “buffer layer” or “buffer material” is intended to mean electrically conductive or semiconductive materials and may have one or more functions in an organic electronic device, including but not limited to, planarization of the underlying layer, charge transport and/or charge injection properties, scavenging of impurities such as oxygen or metal ions, and other aspects to facilitate or to improve the performance of the organic electronic device. Buffer materials may be polymers, oligomers, or small molecules, and may be in the form of solutions, dispersions, suspensions, emulsions, colloidal mixtures, or other compositions. The term “hole transport” when referring to a layer, material, member, or structure, is intended to mean such layer, material, member, or structure facilitates migration of positive charges through the thickness of such layer, material, member, or structure with relative efficiency and small loss of charge. The term “electron transport” when referring to a layer, material, member or structure, is intended to mean such a layer, material, member or structure that promotes or facilitates migration of negative charges through such a layer, material, member or structure into another layer, material, member or structure. The term “hole injection” when referring to a layer, material, member, or structure, is intended to mean such layer, material, member, or structure facilitates injection and migration of positive charges through the thickness of such layer, material, member, or structure with relative efficiency and small loss of charge. The term “electron injection” when referring to a layer, material, member, or structure, is intended to mean such layer, material, member, or structure facilitates injection and migration of negative charges through the thickness of such layer, material, member, or structure with relative efficiency and small loss of charge.
[0017] The device may include a support or substrate (not shown) that can be adjacent to the anode layer 110 or the cathode layer 150 . Most frequently, the support is adjacent the anode layer 110 . The support can be flexible or rigid, organic or inorganic. Generally, glass or flexible organic films are used as a support. The anode layer 110 is an electrode that is more efficient for injecting holes compared to the cathode layer 150 . The anode can include materials containing a metal, mixed metal, alloy, metal oxide or mixed oxide. Suitable materials include the mixed oxides of the Group 2 elements (i.e., Be, Mg, Ca, Sr, Ba, Ra), the Group 11 elements, the elements in Groups 4, 5, and 6, and the Group 8-10 transition elements. If the anode layer 110 is to be light transmitting, mixed oxides of Groups 12, 13 and 14 elements, such as indium-tin-oxide, may be used. As used herein, the phrase “mixed oxide” refers to oxides having two or more different cations selected from the Group 2 elements or the Groups 12, 13, or 14 elements. Some non-limiting, specific examples of materials for anode layer 110 include, but are not limited to, indium-tin-oxide (“ITO”), aluminum-tin-oxide, gold, silver, copper, and nickel. The anode may also comprise an organic material such as polyaniline, polythiophene, or polypyrrole. The IUPAC number system is used throughout, where the groups from the Periodic Table are numbered from left to right as 1-18 (CRC Handbook of Chemistry and Physics, 81 st Edition, 2000).
[0018] In one embodiment, the buffer layer 120 comprises hole transport materials. Examples of hole transport materials for layer 120 have been summarized for example, in Kirk-Othmer Encyclopedia of Chemical Technology, Fourth Edition, Vol. 18, p. 837-860, 1996, by Y. Wang. Both hole transporting molecules and polymers can be used. Commonly used hole transporting molecules include, but are not limited to: 4,4′,4″-tris(N,N-diphenyl-amino)-triphenylamine (TDATA); 4,4′,4″-tris(N-3-methylphenyl-N-phenyl-amino)-triphenylamine (MTDATA); N,N′-diphenyl-N,N′-bis(3-methylphenyl)[1,1′-biphenyl]-4,4′-diamine (TPD); 1,1-bis[(di-4-tolylamino) phenyl]cyclohexane (TAPC); N,N′-bis(4-methylphenyl)-N,N′-bis(4-ethylphenyl)[1,1′-(3,3′-dimethyl)biphenyl]-4,4′-diamine (ETPD); tetrakis-(3-methylphenyl)-N,N,N′,N′-2,5-phenylenediamine (PDA); α-phenyl-4-N,N-diphenylaminostyrene (TPS); p-(diethylamino)benzaldehyde diphenylhydrazone (DEH); triphenylamine (TPA); bis[4-(N,N-diethylamino)-2-methylphenyl](4-methylphenyl)methane (MPMP); 1-phenyl-3-[p-(diethylamino)styryl]-5-[p-(diethylamino)phenyl]pyrazoline (PPR or DEASP); 1,2-trans-bis(9H-carbazol-9-yl)cyclobutane (DCZB); N,N,N′,N′-tetrakis(4-methylphenyl)-(1,1′-biphenyl)-4,4′-diamine (TTB); N,N′-bis(naphthalen-1-yl)-N,N′-bis-(phenyl)benzidine (α-NPB); and porphyrinic compounds, such as copper phthalocyanine. Commonly used hole transporting polymers include, but are not limited to, poly(9,9,-dioctyl-fluorene-co-N-(4-butylphenyl)diphenylamine), and the like, polyvinylcarbazole, (phenylmethyl)polysilane, poly(dioxythiophenes), polyanilines, and polypyrroles. It is also possible to obtain hole transporting polymers by doping hole transporting molecules such as those mentioned above into polymers such as polystyrene and polycarbonate.
[0019] The photoactive layer 130 may typically be any organic electroluminescent (“EL”) material, including, but not limited to, small molecule organic fluorescent compounds, fluorescent and phosphorescent metal complexes, conjugated polymers, and mixtures thereof. Examples of fluorescent compounds include, but are not limited to, pyrene, perylene, rubrene, coumarin, derivatives thereof, and mixtures thereof. Examples of metal complexes include, but are not limited to, metal chelated oxinoid compounds, such as tris(8-hydroxyquinolato)aluminum (Alq3); cyclometalated iridium and platinum electroluminescent compounds, such as complexes of iridium with phenylpyridine, phenylquinoline, or phenylpyrimidine ligands as disclosed in Petrov et al., U.S. Pat. No. 6,670,645 and Published PCT Applications WO 03/063555 and WO 2004/016710, and organometallic complexes described in, for example, Published PCT Applications WO 03/008424, WO 03/091688, and WO 03/040257, and mixtures thereof. Electroluminescent emissive layers comprising a charge carrying host material and a metal complex have been described by Thompson et al., in U.S. Pat. No. 6,303,238, and by Burrows and Thompson in published PCT applications WO 00/70655 and WO 01/41512. Examples of conjugated polymers include, but are not limited to poly(phenylenevinylenes), polyfluorenes, poly(spirobifluorenes), polythiophenes, poly(p-phenylenes), copolymers thereof, and mixtures thereof.
[0020] The particular material chosen may depend on the specific application, potentials used during operation, or other factors. The EL layer 130 containing the electroluminescent organic material can be applied using any number of techniques including vapor deposition, solution processing techniques or thermal transfer. In another embodiment, an EL polymer precursor can be applied and then converted to the polymer, typically by heat or other source of external energy (e.g., visible light or UV radiation).
[0021] Optional layer 140 can function both to facilitate electron injection/transport, and can also serve as a confinement layer to prevent quenching reactions at layer interfaces. More specifically, layer 140 may promote electron mobility and reduce the likelihood of a quenching reaction if layers 130 and 150 would otherwise be in direct contact. Examples of materials for optional layer 140 include, but are not limited to, metal chelated oxinoid compounds, such as tris(8-hydroxyquinolato)aluminum (Alq3), bis(2-methyl-8-quinolinolato)(para-phenyl-phenolato)aluminum(III) (BAIQ), and tetrakis-(8-hydroxyquinolinato)zirconium (IV) (ZrQ); and azole compounds such as 2-(4-biphenylyl)-5-(4-t-butylphenyl)-1,3,4-oxadiazole (PBD), 3-(4-biphenylyl)-4-phenyl-5-(4-t-butylphenyl)-1,2,4-triazole (TAZ), and 1,3,5-tri(phenyl-2-benzimidazole)benzene (TPBI); quinoxaline derivatives such as 2,3-bis(4-fluorophenyl)quinoxaline; phenanthrolines such as 4,7-diphenyl-1,10-phenanthroline (DPA) and 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (DDPA); and mixtures thereof. Alternatively, optional layer 140 may be inorganic and comprise BaO, LiF, Li 2 O, or the like.
[0022] The cathode layer 150 is an electrode that is particularly efficient for injecting electrons or negative charge carriers. The cathode layer 150 can be any metal or nonmetal having a lower work function than the first electrical contact layer (in this case, the anode layer 110 ). As used herein, the term “lower work function” is intended to mean a material having a work function no greater than about 4.4 eV. As used herein, “higher work function” is intended to mean a material having a work function of at least approximately 4.4 eV.
[0023] Materials for the cathode layer can be selected from alkali metals of Group 1 (e.g., Li, Na, K, Rb, Cs,), the Group 2 metals (e.g., Mg, Ca, Ba, or the like), the Group 12 metals, the lanthanides (e.g., Ce, Sm, Eu, or the like), and the actinides (e.g., Th, U, or the like). Materials such as aluminum, indium, yttrium, and combinations thereof, may also be used. Specific non-limiting examples of materials for the cathode layer 150 include, but are not limited to, barium, lithium, cerium, cesium, europium, rubidium, yttrium, magnesium, samarium, and alloys and combinations thereof.
[0024] In other embodiments, additional layer(s) may be present within organic electronic devices. For example, a layer (not shown) between the buffer layer 120 and the EL layer 130 may facilitate positive charge transport, band-gap matching of the layers, function as a protective layer, or the like. Similarly, additional layers (not shown) between the EL layer 130 and the cathode layer 150 may facilitate negative charge transport, band-gap matching between the layers, function as a protective layer, or the like. Layers that are known in the art can be used. In addition, any of the above-described layers can be made of two or more layers. Alternatively, some or all of inorganic anode layer 110 , the buffer layer 120 , the EL layer 130 , and cathode layer 150 , may be surface treated to increase charge carrier transport efficiency. The choice of materials for each of the component layers may be determined by balancing the goals of providing a device with high device efficiency with the cost of manufacturing, manufacturing complexities, or potentially other factors.
[0025] The different layers may have any suitable thickness. In one embodiment, inorganic anode layer 110 is usually no greater than approximately 500 nm, for example, approximately 10-200 nm; buffer layer 120 , is usually no greater than approximately 250 nm, for example, approximately 50-200 nm; EL layer 130 , is usually no greater than approximately 100 nm, for example, approximately 50-80 nm; optional layer 140 is usually no greater than approximately 100 nm, for example, approximately 20-80 nm; and cathode layer 150 is usually no greater than approximately 100 nm, for example, approximately 1-50 nm. If the anode layer 110 or the cathode layer 150 needs to transmit at least some light, the thickness of such layer may not exceed approximately 100 nm. In organic light emitting diodes (OLEDs), electrons and holes, injected from the cathode 150 and anode 110 layers, respectively, into the EL layer 130 , form negative and positively charged polar ions in the polymer. These polar ions migrate under the influence of the applied electric field, forming a polar ion exciton with an oppositely charged species and subsequently undergoing radiative recombination. A sufficient potential difference between the anode and cathode, usually less than approximately 12 volts, and in many instances no greater than approximately 5 volts, may be applied to the device. The actual potential difference may depend on the use of the device in a larger electronic component. In many embodiments, the anode layer 110 is biased to a positive voltage and the cathode layer 150 is at substantially ground potential or zero volts during the operation of the electronic device. A battery or other power source(s) may be electrically connected to the electronic device as part of a circuit but is not illustrated in FIG. 1 .
[0026] FIG. 2 illustrates two embodiments of waveforms used to provide pulsed electrical power. In one embodiment the OFF period can be characterized as zero voltage. In another embodiment the OFF period can be characterized by a negative voltage, such as −5 volts. Typical OFF voltages can be from zero to −8 volts. The supplied current can be any value to provide desired luminescent intensity, in the embodiments shown the current is 160 mA/cm 2 . Typical frequencies range from 50-1000 Hz with duty cycles ranging from 30-95%.
[0027] FIG. 3 illustrates one example of differences in initial luminance drop associated with a direct, also called continuous, power supply and the pulsed system. A single substrate is used to minimize variation between pixels, while direct current (DC) is supplied to one pixel, while a pulsed current at 100 Hz and 95% duty cycle is supplied to a second pixel. Both pixels receive 160 mA/cm 2 while in the ON state. The differences in the first 20 hours of operation, indicated by the circled portion of FIG. 3 , demonstrates a smaller initial drop in luminance for the pulsed arrangement, and maintenance of a higher luminance for subsequent time of operation. The time axis for the pulsed system is adjusted, to equate the ON time for the direct and pulsed systems.
[0028] FIG. 4 illustrates several repetitions of the comparison discussed in FIG. 3 , for performance measurements using several pixels on one substrate. T 97 and T 70 indicate the difference in pixel luminance for 97% of initial luminance and 70% of initial luminance, respectively. The magnitude of the initial drop is largest during the first stage of operation, and differences between direct and pulsed operation are also largest at this stage, as indicated by the T 97 results. The pulsed drive data indicates lower initial luminance drop values than that of continuous power application, with 2 to 10 times performance improvement. In addition, no burn-in is required for high volume manufacturing, saving both time and money using a pulsed drive scheme.
[0029] For a radiation-emitting organic active layer, suitable radiation-emitting materials include one or more small molecule materials, one or more polymeric materials, or a combination thereof. A small molecule material may include any one or more of those described in, for example, U.S. Pat. No. 4,356,429 (“Tang”); U.S. Pat. No. 4,539,507 (“Van Slyke”); U.S. Patent Application Publication No. US 2002/0121638 (“Grushin”); or U.S. Pat. No. 6,459,199 (“Kido”). Alternatively, a polymeric material may include any one or more of those described in U.S. Pat. No. 5,247,190 (“Friend”); U.S. Pat. No. 5,408,109 (“Heeger”); or U.S. Pat. No. 5,317,169 (“Nakano”). An exemplary material is a semiconducting conjugated polymer. An example of such a polymer includes poly(paraphenylenevinylene) (PPV), a PPV copolymer, a polyfluorene, a polyphenylene, a polyacetylene, a polyalkylthiophene, poly(n-vinylcarbazole) (PVK), or the like. In one specific embodiment, a radiation-emitting active layer without any guest material may emit blue light.
[0030] For a radiation-responsive organic active layer, a suitable radiation-responsive material may include a conjugated polymer or an electroluminescent material. Such a material includes, for example, a conjugated polymer or an electro- and photo-luminescent material. A specific example includes poly(2-methoxy,5-(2-ethyl-hexyloxy)-1,4-phenylene vinylene) (“MEH-PPV”) or a MEH-PPV composite with CN-PPV.
[0031] For a hole-injecting layer, hole-transport layer, electron-blocking layer, or any combination thereof, a suitable material includes polyaniline (“PANI”), poly(3,4-ethylenedioxythiophene) (“PEDOT”), polypyrrole, an organic charge transfer compound, such as tetrathiafulvalene tetracyanoquinodimethane (“TTF-TCQN”), a hole-transport material as described in Kido, or any combination thereof.
[0032] For an electron-injecting layer, electron transport layer, hole-blocking layer, or any combination thereof, a suitable material includes a metal-chelated oxinoid compound (e.g., Alq 3 or aluminum(III)bis(2-methyl-8-quinolinato)4-phenylphenolate (“BAIq”)); a phenanthroline-based compound (e.g., 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (“DDPA”) or 9,10-diphenylanthracence (“DPA”)); an azole compound (e.g., 2-tert-butylphenyl-5-biphenyl-1,3,4-oxadiazole (“PBD”) or 3-(4-biphenyl)-4-phenyl-5-(4-t-butylphenyl)-1,2,4-triazole (“TAZ”); an electron transport material as described in Kido; a diphenylanthracene derivative; a dinaphthylanthracene derivative; 4,4-bis(2,2-diphenyl-ethen-1-yl)-biphenyl (“DPVBI”); 9,10-di-beta-naphthylanthracene; 9,10-di-(naphenthyl)anthracene; 9,10-di-(2-naphthyl)anthracene (“ADN”); 4,4′-bis(carbazol-9-yl)biphenyl (“CBP”); 9,10-bis-[4-(2,2-diphenylvinyl)-phenyl]-anthracene (“BDPVPA”); anthracene, N-arylbenzimidazoles (such as “TPBI”); 1,4-bis[2-(9-ethyl-3-carbazoyl)vinylenyl]benzene; 4,4′-bis[2-(9-ethyl-3-carbazoyl)vinylenyl]-1,1′-biphenyl; 9,10-bis[2,2-(9,9-fluorenylene)vinylenyl]anthracene; 1,4-bis[2,2-(9,9-fluorenylene)vinylenyl]benzene; 4,4′-bis[2,2-(9,9-fluorenylene)vinylenyl]-1,1′-biphenyl; perylene, substituted perylenes; tetra-tert-butylperylene (“TBPe”); bis(3,5-difluoro-2-(2-pyridyl)phenyl-(2-carboxypyridyl) iridium III (“F(Ir)Pic”); a pyrene, a substituted pyrene; a styrylamine; a fluorinated phenylene; oxidazole; 1,8-naphthalimide; a polyquinoline; one or more carbon nanotubes within PPV; or any combination thereof.
[0033] For an electronic component, such as a resistor, transistor, capacitor, etc., the organic layer may include one or more of thiophenes (e.g., polythiophene, poly(alkylthiophene), alkylthiophene, bis(dithienthiophene), alkylanthradithiophene, etc.), polyacetylene, pentacene, phthalocyanine, or any combination thereof.
[0034] Examples of an organic dye include 4-dicyanmethylene-2-methyl-6-(p-dimethyaminostyryl)-4H-pyran (DCM), coumarin, pyrene, perylene, rubrene, a derivative thereof, or any combination thereof.
[0035] Examples of an organometallic material include a functionalized polymer comprising one or more functional groups coordinated to at least one metal. An exemplary functional group contemplated for use includes a carboxylic acid, a carboxylic acid salt, a sulfonic acid group, a sulfonic acid salt, a group having an OH moiety, an amine, an imine, a diimine, an N-oxide, a phosphine, a phosphine oxide, a β-dicarbonyl group, or any combination thereof. An exemplary metal contemplated for use includes a lanthanide metal (e.g., Eu, Tb), a Group 7 metal (e.g., Re), a Group 8 metal (e.g., Ru, Os), a Group 9 metal (e.g., Rh, Ir), a Group 10 metal (e.g., Pd, Pt), a Group 11 metal (e.g., Au), a Group 12 metal (e.g., Zn), a Group 13 metal (e.g., Al), or any combination thereof. Such an organometallic material includes a metal chelated oxinoid compound, such as tris(8-hydroxyquinolato)aluminum (Alq 3 ); a cyclometalated iridium or platinum electroluminescent compound, such as a complex of iridium with phenylpyridine, phenylquinoline, or phenylpyrimidine ligands as disclosed in published PCT Application WO 02/02714, an organometallic complex described in, for example, published applications US 2001/0019782, EP 1191612, WO 02/15645, WO 02/31896, and EP 1191614; or any mixture thereof.
[0036] Examples of a conjugated polymer include a poly(phenylenevinylene), a polyfluorene, a poly(spirobifluorene), a copolymer thereof, or any combination thereof.
[0037] Selecting a liquid medium can also be an important factor for achieving one or more proper characteristics of the liquid composition. A factor to be considered when choosing a liquid medium includes, for example, viscosity of the resulting solution, emulsion, suspension, or dispersion, molecular weight of a polymeric material, solids loading, type of liquid medium, boiling point of the liquid medium, temperature of an underlying substrate, thickness of an organic layer that receives a guest material, or any combination thereof.
[0038] In some embodiments, the liquid medium includes at least one solvent. An exemplary organic solvent includes a halogenated solvent, a hydrocarbon solvent, an aromatic hydrocarbon solvent, an ether solvent, a cyclic ether solvent, an alcohol solvent, a glycol solvent, a glycol ether solvent, an ester or diester solvent, a glycol ether ester solvent, a ketone solvent, a nitrile solvent, a sulfoxide solvent, an amide solvent, or any combination thereof.
[0039] An exemplary halogenated solvent includes carbon tetrachloride, methylene chloride, chloroform, tetrachloroethylene, chlorobenzene, bis(2-chloroethyl)ether, chloromethyl ethyl ether, chloromethyl methyl ether, 2-chloroethyl ethyl ether, 2-chloroethyl propyl ether, 2-chloroethyl methyl ether, or any combination thereof.
[0040] An exemplary colloidal-forming polymeric acid includes a fluorinated sulfonic acid (e.g., fluorinated alkylsulfonic acid, such as perfluorinated ethylenesulfonic acid) or any combinations thereof.
[0041] An exemplary hydrocarbon solvent includes pentane, hexane, cyclohexane, heptane, octane, decahydronaphthalene, a petroleum ether, ligroine, or any combination thereof.
[0042] An exemplary aromatic hydrocarbon solvent includes benzene, naphthalene, toluene, xylene, ethyl benzene, cumene (iso-propyl benzene) mesitylene (trimethyl benzene), ethyl toluene, butyl benzene, cymene (iso-propyl toluene), diethylbenzene, iso-butyl benzene, tetramethyl benzene, sec-butyl benzene, tert-butyl benzene, anisole, 4-methylanisole, 3,4-dimethylanisole, or any combination thereof.
[0043] An exemplary ether solvent includes diethyl ether, ethyl propyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, methyl t-butyl ether, glyme, diglyme, benzyl methyl ether, isochroman, 2-phenylethyl methyl ether, n-butyl ethyl ether, 1,2-diethoxyethane, sec-butyl ether, diisobutyl ether, ethyl n-propyl ether, ethyl isopropyl ether, n-hexyl methyl ether, n-butyl methyl ether, methyl n-propyl ether, or any combination thereof.
[0044] An exemplary cyclic ether solvent includes tetrahydrofuran, dioxane, tetrahydropyran, 4 methyl-1,3-dioxane, 4-phenyl-1,3-dioxane, 1,3-dioxolane, 2-methyl-1,3-dioxolane, 1,4-dioxane, 1,3-dioxane, 2,5-dimethoxytetrahydrofuran, 2,5-dimethoxy-2,5-dihydrofuran, or any combination thereof.
[0045] An exemplary alcohol solvent includes methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-1-propanol (i.e., iso-butanol), 2-methyl-2-propanol (i.e., tert-butanol), 1-pentanol, 2-pentanol, 3-pentanol, 2,2-dimethyl-1-propanol, 1-hexanol, cyclopentanol, 3-methyl-1-butanol, 3-methyl-2-butanol, 2-methyl-1-butanol, 2,2-dimethyl-1-propanol, 3-hexanol, 2-hexanol, 4-methyl-2-pentanol, 2-methyl-1-pentanol, 2-ethylbutanol, 2,4-dimethyl-3-pentanol, 3-heptanol, 4-heptanol, 2-heptanol, 1-heptanol, 2-ethyl-1-hexanol, 2,6-dimethyl-4-heptanol, 2-methylcyclohexanol, 3-methylcyclohexanol, 4-methylcyclohexanol, or any combination thereof.
[0046] A glycol ether solvent may also be employed. An exemplary glycol ether solvent includes 1-methoxy-2-propanol, 2-methoxyethanol, 2-ethoxyethanol, 1-methoxy-2-butanol, ethylene glycol monoisopropyl ether, 1-ethoxy-2-propanol, 3-methoxy-1-butanol, ethylene glycol monoisobutyl ether, ethylene glycol mono-n-butyl ether, 3-methoxy-3-methylbutanol, ethylene glycol mono-tert-butyl ether, propylene glycol monomethyl ether (PGME), dipropylene glycol monomethyl ether (DPGME), or any combination thereof.
[0047] An exemplary glycol solvent includes ethylene glycol, propylene glycol, or any combination thereof.
[0048] An exemplary glycol ether ester solvent includes propylene glycol methyl ether acetate (PGMEA).
[0049] An exemplary ketone solvent includes acetone, methylethyl ketone, methyl iso-butyl ketone, cyclohexanone, isopropyl methyl ketone, 2-pentanone, 3-pentanone, 3-hexanone, diisopropyl ketone, 2-hexanone, cyclopentanone, 4-heptanone, iso-amyl methyl ketone, 3-heptanone, 2-heptanone, 4-methoxy-4-methyl-2-pentanone, 5-methyl-3-heptanone, 2-methylcyclohexanone, diisobutyl ketone, 5-methyl-2-octanone, 3-methylcyclohexanone, 2-cyclohexen-1-one, 4-methylcyclohexanone, cycloheptanone, 4-tert-butylcyclohexanone, isophorone, benzyl acetone, or any combination thereof.
[0050] An exemplary nitrile solvent includes acetonitrile, acrylonitrile, trichloroacetonitrile, propionitrile, pivalonitrile, isobutyronitrile, n-butyronitrile, methoxyacetonitrile, 2-methylbutyronitrile, isovaleronitrile, N-valeronitrile, n-capronitrile, 3-methoxypropionitrile, 3-ethoxypropionitrile, 3,3′-oxydipropionitrile, n-heptanenitrile, glycolonitrile, benzonitrile, ethylene cyanohydrin, succinonitrile, acetone cyanohydrin, 3-n-butoxypropionitrile, or any combination thereof.
[0051] An exemplary sulfoxide solvent includes dimethyl sulfoxide, di-n-butyl sulfoxide, tetramethylene sulfoxide, methyl phenyl sulfoxide, or any combinations thereof.
[0052] An exemplary amide solvent includes dimethyl formamide, dimethyl acetamide, acylamide, 2-acetamidoethanol, N,N-dimethyl-m-toluamide, trifluoroacetamide, N,N-dimethylacetamide, N,N-diethyldodecanamide, epsilon-caprolactam, N,N-diethylacetamide, N-tert-butylformamide, formamide, pivalamide, N-butyramide, N,N-dimethylacetoacetamide, N-methyl formamide, N,N-diethylformamide, N-formylethylamine, acetamide, N,N-diisopropylformamide, l-formylpiperidine, N-methylformanilide, or any combinations thereof.
[0053] A crown ether contemplated includes any one or more crown ethers that can function to assist in the reduction of the chloride content of an epoxy compound starting material as part of the combination being treated according to the invention. An exemplary crown ether includes benzo-15-crown-5; benzo-18-crown-6; 12-crown-4; 15-crown-5; 18-crown-6; cyclohexano-15-crown-5; 4′,4″(5″)-ditert-butyldibenzo-18-crown-6; 4′,4″(5″)-ditert-butyldicyclohexano-18-crown-6; dicyclohexano-18-crown-6; dicyclohexano-24-crown-8; 4′-aminobenzo-15-crown-5; 4′-aminobenzo-18-crown-6; 2-(aminomethyl)-15-crown-5; 2-(aminomethyl)-18-crown-6; 4′-amino-5′-nitrobenzo-15-crown-5; 1-aza-12-crown-4; 1-aza-15-crown-5; 1-aza-18-crown-6; benzo-12-crown-4; benzo-15-crown-5; benzo-18-crown-6; bis((benzo-15-crown-5)-15-ylmethyl)pimelate; 4-bromobenzo-18-crown-6; (+)-(18-crown-6)-2,3,11,12-tetra-carboxylic acid; dibenzo-18-crown-6; dibenzo-24-crown-8; dibenzo-30-crown-10; ar-ar′-di-tert-butyldibenzo-18-crown-6; 4′-formylbenzo-15-crown-5; 2-(hydroxymethyl)-12-crown-4; 2-(hydroxymethyl)-15-crown-5; 2-(hydroxymethyl)-18-crown-6; 4′-nitrobenzo-15-crown-5; poly-[(dibenzo-18-crown-6)-co-formaldehyde]; 1,1-dimethylsila-11-crown-4; 1,1-dimethylsila-14-crown-5; 1,1-dimethylsila-17-crown-5; cyclam; 1,4,10,13-tetrathia-7,16-diazacyclooctadecane; porphines; or any combination thereof.
[0054] In another embodiment, the liquid medium includes water. A conductive polymer complexed with a water-insoluble colloid-forming polymeric acid can be deposited over a substrate and used as a charge-transport layer.
[0055] Many different classes of liquid medium (e.g., halogenated solvents, hydrocarbon solvents, aromatic hydrocarbon solvents, water, etc.) are described above. Mixtures of more than one of the liquid medium from different classes may also be used.
[0056] The liquid composition may also include an inert material, such as a binder material, a filler material, or a combination thereof. With respect to the liquid composition, an inert material does not significantly affect the electronic, radiation emitting, or radiation responding properties of a layer that is formed by or receives at least a portion of the liquid composition.
[0057] It is to be appreciated that certain features of the invention which are for clarity, described above in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention that are, for brevity described in the context of a single embodiment, may also be provided separately or in any subcombination. Further, reference to values stated in ranges includes each and every value within that range. | An apparatus and method for producing a luminescent device using a pulsed electrical power feed. The pulsed feed produces a lower initial drop in luminescent efficiency compared to a constant power feed. This method and apparatus avoid traditional processes such as burn-in, used to establish more uniform device performance. | 6 |
TECHNICAL FIELD
This invention relates to paving apparatus and more particularly to apparatus for management of the material flow in paving machines.
BACKGROUND ART
Paving machines are commonly employed in the laying of bituminous roadway mat. The typical paving machine employs a "floating screed" for spreading and compressing the bituminous material to form a smooth surfaced roadway mat. While in the past it has been common to use a floating screed of fixed width, for example, on the order of eight feet or ten feet in width, it has been discovered that the efficiency of the paving machine can be increased and the number of trips required to generate a road surface can be decreased by employing a floating screed having an operator selectable width. This may be accomplished by providing a series of extensions which may be affixed to the main body of the floating screed to a predetermined fixed width. However, a more advantageous arrangement of the floating screed includes one, or more typically two, screed extensions which are slidingly attached to the main body of the floating screed. These screed extensions are typically connected to a linear power source such as a bi-directional hydraulic cylinder or other similar activator, which is selectively operable in response to controls disposed at the operator's control station. This permits the operator to control the position of the screed extensions in response to changing requirements as the paving machine progresses. For example, this permits the screed operator to accommodate obstacles in the path of the paving machine such as sewer drains and manhole covers, and also to permit overwidth paving of the road surface to accommodate driveway entrances and other similar areas where overwidth paving of the roadway mat is desired.
The floating screed type paving machine is typically a self-propelled tractor unit providing a storage means for receiving and containing a discreet quantity of loose bituminous aggregate and a material flow means for conveying the bituminous aggregate to the roadbed where the loose bituminous aggregate is then displaced laterally in front of the floating screed. As the paving machine progresses along the roadbed, the floating screed engages the loose bituminous aggregate, plowing under and compressing the bituminous aggregate into the desired roadway mat. It is common to provide endgates on the outer, distal ends of the screed extensions to ensure that the loose bituminous aggregate disposed in front of the screed extensions is not merely shunted aside beyond the width of the floating screed. The means most commonly used for providing the lateral disposition of the loose bituminous aggregate is a flighted auger providing two oppositely directed flights from the centerline of the paving machine to provide disposition of an equal amount of bituminous aggregate toward the outer edges of the floating screed. While this means has proved to be generally satisfactory, a difficulty exists in ensuring that the appropriate desired amount of loose bituminous aggregate is provided to the screed extensions. This problem is exacerbated by the fact that paving machines are often operated under less than ideal conditions, and it is often necessary to operate one screed extension at a different width than the other screed extension as obstacles are passed or width changes in the roadway mat must be accommodated as the paving machine moves forward. It is necessary for the screed operator to ensure that a suitable proportion of loose bituminous aggregate is available to ensure satisfactory completion of the roadway mat in connection with the furthest extended screed extension, and this causes an undesirable accumulation of bituminous aggregate in front of the less far extended screed extension, due to the fact that there is a reduced amount of area to be covered under that floating screed extension. Furthermore, even where the screed extensions are extended to similar widths, it is undesirably difficult for the screed operator to assure that the desired amount of loose bituminous aggregate is provided for the floating screed. In the operation of current paving machines, the screed operator must cause a suitable flow of loose bituminous aggregate to the auger to ensure that a sufficient amount of aggregate will cascade across the floating screed to reach and fill the area in front of the floating screed to the minimum requisite depth required for the pavement mat. However, the screed operator must be possessed of a substantial amount of skill and expertise to accomplish this result due to the fact that the primary means of controlling the amount of aggregate available to the floating screed is in the conveyance means from the tractor unit of the paving machine.
Therefore, it is an object of the present invention to provide an improved material flow management system for a paving machine.
It is another object of the present invention to provide such a material flow management system as will provide improved control of the aggregate available to the floating screed.
It is a further object of the present invention to provide such a material flow management system as will provide improved control of the material flow to the screed extension.
It is yet another object of the present invention to provide such a material flow management system as will be selectively controllable by the screed operator.
It is yet a further object of the present invention to provide such a material flow management system as will relatively inexpensive to manufacture.
It is another object of the present invention to provide such a material flow management system as will be readily applied to paving machines and such as will not require substantial modification of a paving machine.
It is yet a further object of the present invention to provide such a material flow management system as will be inexpensive to maintain and will be durable.
It is yet a further object of the present invention to provide such a material flow management system as will provide an intermediate boundary to aid a screed operator in controlling the disposition of loose bituminous aggregate in front of the floating screed of a paving machine.
SUMMARY OF THE INVENTION
The subject invention is comprised of a selectively controllable and operator positionable flow gate disposed at each distal end of the main screed of a floating screed for permitting selective operator controlled dispersion of bituminous aggregate from the lateral dispersal means of a paving machine to permit a selectively controlled flow from the main screed to a screed extension of the floating screed unit of a paving machine.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a paving machine including a material flow management apparatus according to the subject invention.
FIG. 2 shows a partial top view of the paving machine including the material flow management apparatus according to the subject invention as taken along line 2--2 of FIG. 1.
FIG. 3 shows an enlarged partial side view of the paving machine and the material flow management apparatus according to the subject invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
A paving machine or apparatus including the present invention is shown generally in FIG. 1 and referred to by the reference number 10.
The paving machine 10 includes a frame 12 which is supported by and transported upon a plurality of transport wheels 14 oppositely disposed on axles 16 which extend underneath the frame 12 transverse to the direction of motion of the paving machine 10. A hopper 20 is disposed on the forward portion of the frame 12. The hopper 20 includes sides 22 extending vertically from the frame 12 so that the hopper 20 can receive discreet quantities of fume-emitting bituminous aggregate material from transport vehicles such as dump trucks, and retain that bituminous aggregate material in the hopper 20 pending its disposition on the surface to be paved. Towards the rear of the frame 12, an operator station 24 is provided so that an operator seated at the operator's chair 26 can control the operation of the paver by way of the controls provided in the control panel 28. Also disposed toward the rear of the frame 12 is an engine housing 30 on which is provided an exhaust stack 32 for exhausting the combustion by-products of the prime mover contained in the engine housing 30. Between the hopper 20 and the engine housing 30 a walkway area 34 is provided to permit access by the paving machine operator or members of the paving crew from side to side of the paving machine or to the engine housing 30 or other machinery and components disposed or mounted upon the paver 10.
A floating screed sub-assembly 40 is pivotally connected to the frame 12 by two screed support arms 42. The screed support arms 42 are substantially parallel and horizontal, being disposed along the frame 12 and pivotally connected to the frame 12 at the arm pivot 44 which has a horizontal axis transverse to the direction of travel of the paver 10, thus permitting vertical movement of the screed assembly 40. Typically, as is known to those skilled in the art, a means is provided for controlling and limiting the vertical movement of the screed sub-assembly 40, and as these components do not comprise any part of the subject invention, they are not shown or disclosed herein. The floating screed sub-assembly 40 as shown is comprised of a main screed body 46 and laterally positionable screed extensions 48 which are disposed behind and parallel to the main screed body 46.
An aggregate disposition means 50 is also provided. This disposition means 50 includes a flighted auger 52 disposed adjacent the rear of the frame 12 in a horizontal and axially transverse position with respect to the direction of travel of the paver 10. Also shown in a representational manner is an auger support means 54 for controlling the position of the auger 52.
Those skilled in the art will understand that the paver 10 and components thereof, including the floating screed sub-assembly 40 and the aggregate disposition means 50, as described herein, are exemplary only, and that the drawing figures are not scale representations of any particular paver apparatus 10. The paver 10 as described herein is not intended to be limiting but rather to be illustrative of apparatus and applications in which the present invention is preferably to be employed. For example, although the paver 10 is described as a wheel-type paver, the subject invention may be equally suitably employed on a track-type paver.
The transport wheels 14 of the paver 10 operate on and along a prepared roadbed surface 60 with the hopper 20 facing the direction of travel so as to receive and contain a portion of aggregate material. A quantity of aggregate material is deposited at a selected volumetric flow rate from the paver 10 in a main material reservoir 62 preceding the main screed body 46, as shown in FIG. 2. The aggregate disposition means 50 operates on the deposited aggregate material to move a portion of the material from the main material reservoir 62 to a secondary material reservoir 66 preceding the screed extensions 48.
As shown in FIGS. 1 and 3, the paver 10 further includes a material flow management means 70 disposed on the main screed body 46. The material flow management means 70 includes a flow control gate 72 pivotally mounted on a flow gate spindle 76 which are substantially horizontal, extending transversely from the screed main body 46 at the outer end thereof. The flow gate spindle 76 extends through a flow gate bearing 78 disposed adjacent the upper end of the flow control gate 72 for permitting a rotational pivotal mounting of the flow gate 72 with respect to the main screed body 46.
The material flow management means 70 is also provided with a flow gate actuator means 80. The flow gate actuator means 80 includes an actuator body 82 pivotally mounted by a first actuator means mounting pin 84 to a screed arm 42 for permitting a relative rotational motion between the actuator means 80 and the screed arm 42. An actuator plunger 86 operates within the plunger body 82 in a linear reciprocating manner to permit a greater or lesser extension of the actuator means 80. The actuator plunger 86 is connected by a second actuator means connecting pin 92 to a flow gate yoke 94 at an upper corner of the flow gate 72, disposed at a distance from the flow gate spindle 76. At least one or more actuator control lines, one of which is shown at 96 are connected to a control means (not shown) for selectively controlling the operation of the flow gate actuator means 80. It is believed that those skilled in the art will appreciate the various types of typical control means which may be suitable for application to the material flow management means 70. For example, the flow gate actuator means 80 may be a hydraulic cylinder operated in response to a controlled flow of hydraulic fluid through the control line 96, or alternatively may be an electrically operated motor responsive to electrical signals transmitted through control line 96.
The actuator plunger 86 operates reciprocally with the actuator body 82 through a distance D between a maximum extension and a minimum extension of the actuator means 80. As shown in FIG. 3, when the actuator plunger 86 is at its maximum extension, the flow control gate 72 is actuated to the fully open position A, and is disposed immediately adjacent to the main screed body 46, and when the actuator plunger 86 is at its minimum extension, the flow control gate 72 is moved to the fully closed position B. In the fully closed position B, at least a portion of the flow control gate 72 extends in front of the main screed body 46, to prevent a flow of aggregate material from the main material reservoir 62 to the secondary material reservoir 66 adjacent the main screed body 46.
In operation, material is transported to and deposited in the main material reservoir 62, as shown in FIG. 2, by the paver 10 while the paver 10 is operated along the roadbed surface 60 for laying an aggregate road surface. The position of each screed extension 48 is independently variable, and is selected by the paver operator to a position between the minimum extension E1 to the maximum extension E2 thereof. The area of each secondary material reservoir 66 is that area adjacent the main material reservoir 62 and the main screed body 46, and preceding the extended portion of the screed extension 48.
When the screed extension 48 is operated to the minimum extension E1, the secondary material reservoir 66 is at its minimum area of coverage. Therefor, the flow gate actuator means 80 is operated to the minimum extension when the screed extension is at the minimum extension position E1. This pivots the flow control gate 72 to the fully extended closed position B to prevent flow from the main material reservoir 62 to the secondary material reservoir 66.
On the other hand, when the screed extension 48 is actuated to the fully extended position E2, the flow control gate actuator means 80 is actuated to the fully extended position of the actuator plunger 86, driving the flow control gate 72 to the fully open position A, and permitting the maximum volumetric flow of material from the main material reservoir 62 to the secondary material reservoir 66.
At intermediate positions of the screed extension 48 between the fully retracted position E1 and the fully extended position E2, the flow gate actuator means 80 is actuated to an intermediate position to permit a volumetric flow rate of material corresponding to the relative width to be covered by the screed extension 48. Furthermore, where there are variations in the roadbed surface 60 requiring a reduction in material provided to the screed extension 48, the flow control gate 72 can be actuated by the actuator means 80 to an intermediate position which provides relatively less material to the secondary material reservoir 66 from the main material reservoir 62, assuring that the desired volumetric rate of material flow is achieved.
Preferably, the components of the material flow management means 70 will be formed from metals such as steel or other durable alloys to ensure that the material flow management means 70 is sufficiently durable and resistant to wear and abrasion from the material used in the paving process, and also to assure that the material flow management means 70 is not adversely affected by the relatively higher temperatures at which such paving materials are typically maintained.
Several advantages inherent in the material management means 70 according to the present invention are readily apparent. First, the material flow management means 70 assures that the proper volumetric flow rate of material is attained from the main material reservoir 62 to the secondary material reservoir 66. Second, the material flow management means 70 is independently operable to permit the independent control of the screed extension 48 so as to permit the paver 10 to perform asymmetrical paving operations, with one screed extension 48 at an extension which is at variance with the other screed extension 48. Third, the material flow management means 70 ensures that excessive material is not provided to the secondary material reservoir 66, thus avoiding unnecessary cleanup or waste of material which might otherwise be pushed aside and left unused by the paver 10. Fourth, the material flow management means 70 is easy to operate and inexpensive to manufacture, install, and maintain. Therefore, it can be seen that the present invention presents substantial improvements over the prior art. These and other advantages will be readily apparent to those skilled in the art.
Modifications to the preferred embodiment of the subject invention will be apparent to those skilled in the art within the scope of the claims that follow: | Material flow management apparatus for a paving machine having a screed assembly, including at least one pivotally mounted flow control gate operably connected to a selectively controllable actuator for actuating the flow control gate to a flow preventing position and flow permitting positions, the flow control gate mounted immediately adjacent the outer edge of the main body of the screed assembly to variably control the volumetric flow of paving aggregate from the main material reservoir preceding the screed main body and ensure a suitable volumetric material supply to the secondary material reservoir preceding the variably extensible screed extension body. | 4 |
CLAIM OF PRIORITY
This application claims priority, pursuant to 35 U.S.C. §119, to that patent application entitled “TIME DIVISION MULTIPLEXING FRAME FOR MULTIPLEXING DIFFERENT SYNCHRONOUS SIGNALS AND METHOD FOR TRANSMITTING AND RECEIVING THE SAME,” filed in the Korean Intellectual Property Office on Jan. 30, 2004 and assigned Ser. No. 2004-6177, the contents of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an FTTH (Fiber To The Home) systems, and more particularly to a TDM (Time Division Multiplexing) frame applicable for digital broadcast data transmission in an FTTH (Fiber To The Home) system and a method for transmitting and receiving the TDM frame.
2. Description of the Related Art
A broadcast services and communication services are currently provided independently to the home or office. Research on convergence of broadcast services and communication services is presently being conducted. Bi-directional HFC (Hybrid Fiber Coaxial) type system, and IP (Internet Protocol)-based system using an xDSL (x Digital Subscriber Line) network are known broadcast/communication systems. A system based on an FTTH (Fiber To The Home) is also be considered.
Because the broadcast/communication convergence system of the bi-directional HFC type uses a coaxial cable, there is a problem in that the bandwidth is limited due to a physical limit of the coaxial cable and a complex modulation scheme, such as a subcarrier modulation scheme, must be used. Moreover, as the IP-based broadcast/communication convergence system using the xDSL network that performs a transmission operation in units of packets, it is difficult for the broadcast service to be seamlessly provided. In this case, since a process for linking the packet units is required, time delay is incurred and a real-time broadcast service cannot be appropriately provided, such that QoS (Quality of Service) cannot be satisfied. In addition, because the xDSL uses a copper line as a transmission medium, there is a drawback in that a bandwidth is limited due to physical properties of the copper line.
For this reason, the broadcast/communication convergence system using the FTTH system is popular because of a wider bandwidth and faster transmission speed.
The broadcast/communication convergence system using the FTTH system uses a TDM transmission technique for convergence of the broadcast service and communication service. Here, the TDM transmission technique is to ensure a plurality of time slots is available and that there is appropriate transmission of desired data at each time slot. If a processing operation associated with the time slots is appropriately performed, broadcast streams can be seamlessly transmitted.
Where a digital broadcast based on the FTTH system is transmitted using the TDM transmission technique, synchronization between transmission data units is an important factor. In particular, transmission clock synchronization for a digital broadcast can be different for each broadcast provider or broadcast program. Where various clock signals are inputted, a need exists for a TDM frame format capable of synchronizing the different clock signals.
SUMMARY OF THE INVENTION
Therefore, one aspect of the present invention is to provide a TDM (Time Division Multiplexing) frame using a stuff bit and a method for transmitting and receiving the TDM frame that can transmit and receive a plurality of digital broadcast data units having different synchronous clocks using a simple format.
In accordance with another aspect of the present invention, a TDM (Time Division Multiplexing) frame for multiplexing digital broadcast and communication signals based on different synchronous signals in a broadcast/communication convergence system using an FTTH (Fiber To The Home) is provided and includes a framing bit field for identifying a start and end of the TDM frame seamlessly provided, two MPTS (Multiple-Program Transport Stream) fields respectively having at least one bit assigned for digital broadcast data transmission wherein an amount of input digital broadcast data is adjusted according to a difference between a multiplexing rate and an input rate associated with the digital broadcast data in the digital broadcast data transmission, and a fast Ethernet field having at least one bit assigned for communication data transmission.
In accordance with another aspect of the present invention, a method for transmitting a TDM (Time Division Multiplexing) frame in which different synchronous signals are multiplexed is provided and includes the steps of dividing data to be inputted to the TDM frame in a predetermined bit unit and inserting the divided data into the TDM frame, comparing an input rate of the data inserted in the predetermined bit unit with a multiplexing rate, and inserting a stuffing control field indicating a corresponding rate difference at every input data of the predetermined bit unit, and adjusting the number of last transmission bits of the TDM frame according to a value of the stuffing control field and carrying out a transmission operation.
In accordance with yet another aspect of the present invention, a method for receiving a TDM (Time Division Multiplexing) frame in which different synchronous signals are multiplexed is provided and includes the steps of comparing an input rate of transmission data inputted to the TDM frame with a multiplexing rate, extracting a stuffing control field indicating a corresponding rate difference, and confirming the number of bits included in the received TDM frame and extracting the transmission data from the received TDM frame according to the confirmed number of bits.
BRIEF DESCRIPTION OF THE DRAWINGS
The above features and other advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic block diagram illustrating a broadcast/communication convergence system based on an FTTH (Fiber To The Home) system to which the present invention is applied;
FIG. 2 shows a format of a TDM (Time Division Multiplexing) frame in accordance with an embodiment of the present invention; and
FIG. 3 shows MPTS (Multiple-Program Transport Stream) fields for accommodating a plurality of digital broadcast data units based on different synchronous signals in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Now, embodiments of the present invention will be described in detail with reference to the annexed drawings. In the drawings, the same or similar elements are denoted by the same reference numerals even though they are depicted in different drawings. For the purposes of clarity and simplicity, a detailed description of known functions and configurations incorporated herein will be omitted as it may make the subject matter of the present invention unclear.
FIG. 1 is a schematic block diagram illustrating a broadcast/communication convergence system based on an FTTH (Fiber To The Home) system to which the present invention is applied. As shown, the broadcast/communication convergence system based on the FTTH system to which the present invention is applied, includes an OLT (Optical Line Terminal) 11 serving as a subsystem positioned between users and a service node, an ONT (Optical Network Terminal) 12 serving as a device of a user side, and an optical cable connected between the OLT 11 and the ONT 12 . The OLT 11 electro-optically converts a plurality of broadcast and communication signals received from broadcast and communication providers into different wavelength signals λ 1 , λ 2 , . . . λ n , multiplexes the different wavelength signals into a single optical signal and sends the single optical signal so that broadcast/communication services such as digital broadcast, analog broadcast, voice telephone, video service, high-speed Internet, etc. can be provided to users. The ONT 12 transfers information received from the OLT 11 to the users in the form of time slot signals.
More specifically, the OLT 11 includes a plurality of E/O (Electrical-Optical) converters 101 - 1 to 101 -n each electro-optically converting a broadcast or communication signal; and an optical multiplexer 102 for multiplexing electro-optically converted signals based on a plurality of wavelengths into the single optical signal and transmitting the single optical signal. Moreover, the ONT 12 includes an optical demultiplexer 103 for demultiplexing the transmitted single optical signal into the electro-optically converted signals based on the plurality of wavelengths; and O/E (Optical-Electrical) converters 104 - 1 to 104 -n each converting the electro-optically converted signal into an electrical signal corresponding to the broadcast or communication signal. Hence, the broadcast signal and the communication signal are transferred to the ONT 12 and ONT 12 selects and switches the broadcast signal desired by a user and then delivers a TDM frame to the user.
FIG. 2 illustrates a format of a TDM (Time Division Multiplexing) frame in accordance with an embodiment of the present invention. In this illustrative embodiment of the present invention the frame format is capable of multiplexing two 27-Mbps MPEG-2 (Motion Picture Expert Group-2) TSs (Transport Streams) and 100-BASE-X fast Ethernet data, as will be more clearly explained.
As shown, the TDM frame in accordance with the present invention operates preferably at 162 MHz, and the TDM frame's length is 486 bits. In detail, the TDM frame includes an 8-bit framing bit field 201 necessary for identifying a start and end of the frame; a 2-bit scramble seed field 202 indicating scramble information associated with four types of polynomial expressions for scrambling; an 88-bit MPTS-1 (Multiple-Program Transport Stream-1) field 203 and an 88-bit MPTS-2 field 204 for transporting broadcast streams; and a 300-bit fast Ethernet field 205 for transporting communication data. In another aspect, the scramble seed field 202 can be replaced with other information in the TDM frame.
In a one specific embodiment, 8-bit framing bit field 201 is set to a value “10101010” (AA 16 ) and allows a demultiplexing stage to easily identify the start and end of the frame, and further allows an optical detection stage to easily perform a CDR (Clock and Data Recovery) operation. Of course, the set value “10101010” is only an example in the embodiment of the present invention. In the present invention, those skilled in the art can understand that a value of the framing bit field 201 is not limited to the value “10101010”.
Because the digital broadcast stream and fast Ethernet, i.e., communication, data include a plurality of consecutive 1's or 0's, respectively, a scrambling operation must be performed when an optical transmission operation is carried out. In accordance with the embodiment of the present invention, the 2-bit scramble seed field 202 is used for a stable scrambling operation and the four types of polynomial expressions are sequentially used, such that a stream of the consecutive 1's or 0's can be avoided. Scrambling is well-known in the communications art and need not be described in detail herein.
In order to include the two 27-Mbps MPEG-2 T Ss and the 100-BASE-X fast Ethernet data, the TDM frame includes the two 88-bit MPTS fields 203 and 204 and the 300-bit fast Ethernet field 205 . Here, in order to accommodate digital broadcast data units based on different synchronous signals, the MPTS fields include six stuffing control bits and one stuff bit in accordance with the present invention, respectively. The 88-bit MPTS fields are shown in FIG. 3 .
FIG. 3 shows MPTS fields for accommodating digital broadcast data units based on different synchronous signals in accordance with an embodiment of the present invention. As shown, the MPTS field in accordance with the present invention includes a basic format consisting of six 12-bit data fields 301 for digital broadcast streams based on different synchronous signals and six stuffing control fields 302 necessary for a stuffing control operation according to a result of a determination as to synchronization in the data fields 301 , and a 1-bit stuff field 303 for compensating for broadcast data not synchronized with a 9-bit data field.
In accordance with the present invention, stuffing modes include three modes such as a normal mode, a positive mode and a negative mode.
With regard to the normal mode, this mode corresponds to the case wherein a broadcast signal input rate and a multiplexing rate are the same. In this normal mode, a transmission operation is carried out for a frame in which the last 9-bit data field is filled with data and the 1-bit stuff field 303 is empty. In FIG. 3 , the frame referred to as (a) indicates a frame format in case of the normal mode.
With regard to the positive mode, this mode corresponds to the case wherein the broadcast signal input rate is higher than the multiplexing rate. In this positive mode, a transmission operation is carried out for a frame including the last 10-bit data field in which the 1-bit stuff field is filled with data. In FIG. 3 , the frame referred to as (b) indicates a frame format in the case of the positive mode.
With regard to the negative mode, this mode corresponds to the case where the broadcast signal input rate is lower than the multiplexing rate. In this negative mode, a transmission operation is carried out for a frame including the 8-bit data field and the 2-bit stuff field 303 in which a 1-bit data field and a 1-bit stuff field are empty. In FIG. 3 , the frame referred to as (c) indicates a frame format in the case of the negative mode.
As described above, the three modes are determined by the stuffing control fields 302 . Each of the stuffing control fields 302 used in the present invention is interleaved and inserted into the MPTS field every 12-bit data field. Exemplary values of the stuffing control fields 302 for discriminating the three modes are shown in the following Table 1.
TABLE 1
Mode
Mode detection condition
Pattern
Positive
Number of 1's is equal to or larger than 5
111111
Normal
Number of 1's is 2, 3 or 4
101010
Negative
Number of 1's is 0 or 1
000000
Because a reception stage carrying out a demultiplexing operation detects a transmission mode using the number of 1's and the number of 0's in the six 1-bit stuffing control fields 302 as shown in the above Table 1, the error rate can be reduced.
In order to constitute a TDM (Time Division Multiplexing) frame so that digital broadcast signals including the stuff bit based on different synchronous clocks can be accommodated, data is inserted in a unit of 12 bits and a plurality of input digital broadcast signals are multiplexed. In this case, a multiplexing time and a broadcasting time are compared with each other. If the broadcasting time is earlier than the multiplexing time, a value of the stuffing control field 302 is set to “1”. All values of the stuffing control fields 302 are confirmed from the MPTS field 203 or 204 . If the mode detection condition corresponds to the positive mode, for example, if the number of 1's is equal to or larger than 5, a transmission operation is carried out for a frame including the last 10-bit field consisting of the 10-bit data field. Further, if the mode detection condition corresponds to the normal mode, for example, if the number of 1's is 2, 3 or 4, a transmission operation is carried out for a frame including the last 10-bit field consisting of the 9-bit data field and the 1-bit stuff field 303 . Furthermore, the mode detection condition corresponds to the negative mode, for example, if the number of 1's is 1 or 0, a transmission operation is carried out for a frame including the last 10-bit field consisting of the 8-bit data field and the 2-bit stuff field 303 .
Therefore, the reception stage confirms the stuffing control fields 302 from the transmitted MPTS fields 203 and 204 , and a transmission mode is confirmed. The last 10-bit field included in the MPTS field 203 or 204 is determined according to a corresponding mode, and a result of the determination is processed by the reception stage.
As apparent from the above description, the present invention can carry out a multiplexing operation for different digital broadcast signals based on different synchronous clocks using a simple format-based frame in a broadcast/communication convergence system for combining a plurality of digital broadcast signals and transmitting a result of the combining.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope of the invention. Therefore, the present invention is not limited to the above-described embodiments, but the present invention is defined by the claims which follow, along with their full scope of equivalents.
In accordance with the embodiment of the present invention, there have been described a TDM (Time Division Multiplexing) frame including an 8-bit framing field, a 2-bit scramble seed field, two 88-bit MPTS (Multiple-Program Transport Stream) fields and a 300-bit fast Ethernet field, each 88-bit MPTS field including six 12-bit data fields, a 9-bit data field, six 1-bit stuffing control fields and a 1-bit stuff field. This description is only an example, and the present invention is not limited thereto.
That is, those skilled in the art can understand that bits of the TDM frame can be differently assigned according to an MPTS bandwidth and a fast Ethernet bandwidth. | A TDM (Time Division Multiplexing) frame applicable to digital broadcast data transmission in an FTTH (Fiber To The Home) system and a method for transmitting and receiving the TDM frame is disclosed. The TDM frame and methods are applicable to transmit a plurality of digital broadcast data units having different synchronous clocks using a simple format. The TDM frame for multiplexing digital broadcast and communication signals having different synchronous signals in a broadcast/communication convergence system using an FTTH system comprises a framing bit field for identifying a start and end of the TDM frame seamlessly provided; two MPTS (Multiple-Program Transport Stream) fields respectively having at least one bit assigned for digital broadcast data transmission wherein an amount of input digital broadcast data is adjusted according to a difference between a multiplexing rate and an input rate associated with the digital broadcast data in the digital broadcast data transmission; and a fast Ethernet field having at least one bit assigned for communication data transmission. | 7 |
The invention relates to a feed table for feeding slivers by way of a conveyor to a textile-processing machine.
Arrangements are known wherein individual slivers are drawn out of the spinning cans by way of roller pairs disposed thereabove and supplied by way of a number of support rollers or other guide means to a subsequent textile-processing machine, for example, a drawframe. The slivers are combined therein to form a web and supplied by a pair of rollers to the drawframe.
A disadvantage of such facilities is that the slivers are guided only at a few places along their feed path and sag freely elsewhere. There is, therefore, a risk of the slivers tearing between the individual guides.
When a sliver breaks or runs out, the drawframe must be stopped and a new sliver fed in manually.
DE-AS 2 230 644 discloses an apparatus which obviates some of these disadvantages and, in which the sliver to be processed, referred to herein briefly as the "sliver", is drawn off from a spinning can by way of draw-off rollers and placed on a conveyor belt for forward conveyance. A reserve can is associated, in line, with each operating can to form a pair. The sliver of the reserve can, hereinafter briefly called the "reserve sliver", is retained in a standby position by way of a pair of draw-off rollers. The draw-off roller pairs for the sliver and for the reserve sliver are, as considered in the direction of conveyance, disposed in line one after another. In the event of a sliver breaking or running out, control mechanism acts to start the draw-off means of the associated reserve sliver.
This ensures automatic feeding-in of a reserve sliver in the event of a sliver breaking or running out.
A disadvantage of this construction is that the slivers and reserve slivers experience a number of sharp deflections before being guided onto the conveyor belt.
The risk of a sliver breaking is, therefore, increased and there is a substantial evolution of dust. Also, the conveyor belt has no lateral guidance for the slivers or the reserve slivers, so that problems may arise when a reserve sliver has to be fed in or joined onto the sliver.
SUMMARY OF THE INVENTION
It is the object of this invention to obviate the disadvantages of the known arrangements and to provide an apparatus and a method where a sliver or a reserve sliver can be placed on a conveyor without substantial deflections in its path, remains in the predetermined conveyance position, and is suitable for the controlled feeding-in of a reserve sliver.
According to the invention, to provide a simple feeding-in of the reserve slivers the conveyor belts for the slivers and the conveyor belts for the reserve slivers are disposed parallel to one another and in pairs.
Advantageously, these paired conveyor belts are controlled by a common control.
The use of individual conveyor belts enables the lengths of the conveyor belts to be such as not to exceed the necessary dimension, i.e., it is proposed that each individual conveyor belt begins above the associated spinning can and terminates at a common delivery station.
The moving parts of the conveyor belt can, therefore, be kept to a necessary minimum, so that less driving power is required and there is less eddying of dust.
Having the deflecting or reversing rollers of the conveyor belts at the entry cooperate with pivoted pressing rollers to form draw-off means for the slivers leads to a compact arrangement, and the slivers are guided directly onto the conveyor belt for forward conveyance without substantial deflections.
A further embodiment of the invention provides two rows of sensors to detect the sliver end and the sliver start and facilitate satisfactory control of the feeding of the slivers and of the automatic feeding-in of the reserve slivers.
According to another embodiment of the invention, to make the start of a fed-in reserve sliver converge on a running-out sliver, guide means for producing such convergence are provided after the delivery station of the conveyor belts.
Driving the conveyor belts by way of clutches disposed coaxially on a common drive shaft leads to a compact and simple drive.
Advantageously, for accurate positioning of the slivers, brake facilities are associated with the individual clutches.
Of special significance is the inventive concept of mounting the individual conveying belts on respective special frame work portions or supports. The frame work can then be assembled from modules depending upon the prevailing requirements. In this respect, it has proved advantageous that the individual support has, at one end, a drive roll and, at the other end, a diverting or deflecting roll. Both the latter and the drive roll can be made axially movable on the support to form tensioning rolls for the conveying belt.
The support is preferably manufactured as a tubular section with a U-shaped section mounted thereon. One run of the conveying belt can be movably mounted in a protective manner in the interior of the U-shaped section.
For the other run of the conveying belt, a tubular or trough-shaped projection is provided below the tubular section, and also support rolls are provided in order to prevent sagging.
It is of special significance that the support can be assembled from axial support sections which are jointly enclosed by the conveying belt; these support sections are prefabricated in predetermined variable lengths comprising, preferably, a basic length, one and a half times the basic length, and a double length.
Several parallel supports are grasped by at least one common transverse carrier as a part of the frame of the feed table so that this frame is assembled from only few individual components.
In accordance with a further embodiment of the invention, the drive of the conveyor belt is provided in a drive unit mounted as a module on the support. The drive unit comprises a drive roll, projecting into the return section of the conveyor belt. In order to improve feeding in of the fiber sliver, at least one pressure roll is pivotable onto the circumference of the drive roll. The pressure roll forms a part of the drive unit, is mounted externally of the drive unit on the support thereof, or on the adjacent support which projects over the first mentioned support in a direction opposed to the transport direction.
Further advantages, features and details of the invention will be apparent from the following description of preferred embodiments and from the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
These show the following schematic illustrations:
FIG. 1 is a plan view of a feed table of a textile machine with conveying belts of varying lengths arranged parallel to each other;
FIG. 1a is a plan view of another embodiment of the invention wherein the conveyor belts are disposed on two vertical levels;
FIG. 2 is a side view of the arrangement according to FIG. 1;
FIG. 2a is a side view of the arrangement according to FIG. 1a;
FIG. 3 is a plan view, on a larger scale than that used in FIG. 1, of a transfer region between the conveyor belts of the feed table and a transport belt following the conveyor belts;
FIG. 4 is a plan view of two feed tables with a common transfer region;
FIG. 5 is a schematic plan view of a feed table comprising supports, assembled from modules, for the conveyor belts, which have been only partially illustrated;
FIG. 6 is a side view, on a smaller scale, of an arrangement according to FIG. 5 with the supports forming parts of a frame,
FIG. 7 is an enlarged detail from FIG. 6 showing two modules;
FIG. 8 is an enlarged detail from FIG. 7;
FIG. 9 is a plan view of FIG. 7;
FIG. 10 is a plan view of FIG. 8;
FIG. 11 is a transverse view of a support of the frame forming part of FIG. 8 and is illustrated in enlarged elevation;
FIG. 12 is a view of a further embodiment of the transverse support according to FIG. 11;
FIG. 13 is a sectional view of FIG. 12, taken along lines XIII--XIII;
FIG. 14 is a detailed sectional view of a deflecting roll for a conveyor belt, illustrated in partially sectioned plan; and
FIG. 15 is an enlarged side view of a drive wheel for a conveyor belt illustrated as an enlarged detail of an arrangement according to FIG. 7.
DETAILED DESCRIPTION OF THE INVENTION
The individual slivers 2 and reserve slivers 7 are drawn out of respective spinning cans 9, 9a by means of respective draw-off roller pairs 10, 10a and move onto individual conveyor belts 8, 8a, respectively (as seen in FIGS. 1 and 2).
The belts 8, 8a extend to a common delivery station 11. The belts 8, 8a are driven by a motor 12, driving a transverse drive shaft 13. The belts 8, 8a have inwardly directed toothed profiles which are not shown in great detail and which mesh with the external toothed profile of a driving roller 14, 14a and drawoff roller 15, 15a.
The drive connection between the shaft 13 and the rollers 14, 14a is by way of individual clutch units (not shown in greater detail) in the drive rollers. To stop the various belts 8, 8a brake devices (not shown in detail) are provided in addition to the various clutches.
For the sake of clarity, the connections to the stationary machine frame of the various bearings or units are not shown.
Two rows of sensors 18, 19 are disposed across and above the conveyor belts 8, 8a between the delivery station 11 and the draw-off roller pair 10a nearest the drawframe. The rows 18, 19 have sensors 20, 21 sensing the various slivers 2, 7, as can be seen in FIG. 3. Disposed further on, and below the delivery station 11, is a conveyor belt 3 on which the slivers 2 are placed and supplied by way of a feed condenser 4 and a conveying roller 5 to a drawframe.
The condenser 4 condenses the parallel moving slivers 2 into a web 22 at the roller 5.
Guide plates 24, 25 are provided above the conveyor belt 3 in addition to the lateral guides 23, 23a of the condenser 4.
The lateral guides 23, 23a and/or the guide plates 24, 25 could also be guide belts rotating around vertical axes.
The drive for the belt 3 is derived from the drive of the motor 12 (not shown). The sensors 20, 21, the clutches 16, the brake devices 17 and the motor 12 are connected for control purposes to a control unit 26.
The control or operation of this facility is as follows:
With the motor 12 on and the clutches 16 engaged, the slivers 2 are placed on the rotating conveyor belts 8; the slivers 2 are moved automatically or manually between the draw-off roller pairs 10, the clamping rollers 27 being pivotable or displaceable.
The slivers thus placed on the rotating belts 8 move consecutively or simultaneously into the detection zone of the sensors 21 of the row 19. The drive of the belts 8, i.e., the control of the clutches 16, is actuated so that when a sensor 21 detects the leading end of a sliver, the clutch of the corresponding conveyor belt 8 disengages and the same is stopped immediately by the corresponding brake device. An accurately defined initial position of the sliver leading end is therefore ensured.
The control is such that when the sensors 21 have detected all the leading ends of the slivers, all the clutches 16 of the belts 8 re-engage simultaneously and their brake devices release simultaneously. This ensures that all the slivers 2 arrive simultaneously on the conveyor belt 3. Conveyor belts convey the slivers 2 forward to a conveying roller 5 which delivers the slivers 2, combined to form a web 22, to a drafting arrangement (not shown in detail). On their way to the roller 5 the slivers 2 enter a condenser 4 whose side guides 23, 23a cause the slivers 2 to converge. Further guide plates 24, 25 to guide the slivers 2 and the reserve slivers 7 are disposed in the condenser 4.
The reserve slivers 7 drawn out of the cans 9a pass like the slivers 2 by way of a draw-off roller pair 10a to the conveyor belts 8a. Conveyance of the reserve slivers 7 is interrupted, i.e., the clutches 16 of the conveyor belts 8a disengage, whenever the sensors 21 associated with the conveyor belts 8a detect the leading end of a reserve sliver 7. When the clutches 16 of the belts 8a disengage; the operative brake devices 17 stop the belts 8a very rapidly.
The starting of any of the conveyor belts 8a, i.e., the feeding-in of a reserve sliver 7, occurs only when the sensor row 18, i.e., the sensors 20, detects the run-out or interruption of a sliver 2.
The starting of the belts 8a is delayed by an amount depending upon the distance between the sensor rows 18 and 19.
For lateral guidance of the slivers 2, 7 on the belts 8, 8a the provision of guides 28 above the conveyor belts are provided. The corresponding guides 28 are rigidly connected to a frame part and are disposed over some or all of the length of the belts 8, 8a. The guides 28 might, in some circumstances, have an additional guide for the conveyor belt.
Another embodiment of lateral guidance of the slivers and reserve slivers is for the conveyor belts 8, 8a to have rotating guides disposed on them.
The piecing-up of the reserve slivers 7 by way of the draw-off roller pair 10a can proceed simultaneously with the piecing-up of the slivers 2.
Referring now to FIGS. 1a and 2a wherein conveyor belts 8 are arranged vertically above conveyor belts 8a with the reserve slivers being conveyed by conveyor belts 8a. Conveyor belts 8 and 8a deliver their slivers to a common delivery station 11, in the same manner as in the embodiment of FIGS. 1 and 2. In this embodiment, two rows of sensors 18, 19 are disposed on each level of conveyors.
FIG. 3 shows the running-out of a sliver 2 and the feeding-in of a reserve sliver 7. The actual piecing-up of the spare sliver 7 to the running-out end of the sliver 2 is performed when the reserve sliver 7 reaches the side guide 23 of the condenser 4. In the example shown, the arrival on the side guide 23 is associated with a slight overlapping between the end of the sliver 2 and the leading end of the reserve sliver 7.
Another embodiment is to butt-join the start of the reserve sliver 7 to the running-out end of the sliver 2.
Also, additional horizontal or vertical pressing rollers may be provided near the place where the slivers and reserve slivers converge, with a view to increasing the adhesion of the joint between them. After the piecing-up of the reserve sliver 7, it becomes a sliver 2 and a new reserves sliver 7 is fed in manually or automatically on the now empty conveyor belt 8. The start of the new reserve sliver moves into he region of the sensor 21 so that, as previously described, the drive of the corresponding belt 8 is interrupted and the new reserve sliver 7 remains in this standby position.
As can be gathered from the procedure hereinbefore described, the sensor row 19 is effective to detect the leading end of the sliver and the sensor row 18 is effective to detect a running-out sliver 2, 7.
Another embodiment is for the sliver end to be detected as early as the roller pair 10, 10a, in which event the first sensor row 18 could be omitted.
The various conveyor belts 8, 8a need not necessarily be guided parallel to one another but can be guided so as to converge towards the delivery station 11, or to radiate therefrom.
FIG. 4 shows a corresponding embodiment in which the feed table has been divided into two segments 1a, 1b arranged to diverge from one another at an angle x and y respectively to the feed direction into the drawframe 6. The angles x, y can be up to 90°. In the latter case the deflection in the feed zone to the drawframe 6 is also 90° and calls for a known device to change the feeding direction or some other special kind of deflecting facility.
In the example shown in FIG. 4, the angles x, y are each in the range of approximately 30° so that the provision of guide plates 23b, 24, 25 suffices for entry into the drawframe 6, i.e., to make the slivers and reserve slivers converge. Since the slivers are fed at an angle x or y, a central guide plate 23b is necessary to ensure a parallel entry of the slivers into the drawframe.
In contrast to FIG. 1, a sensor row 18, 19 and a drive motor 12 are associated with each feed table segment 1a and 1b.
Control of the feeding of the slivers and of the feeding-in of the reserve slivers corresponds to the embodiment shown in FIGS. 1 and 3 and will not be further described here. For starting and in operation the two motors 12 are electrically interconnected to ensure simultaneous or uniform feeding of the slivers into the drawframe 6.
Another embodiment of the invention provides for the conveyor belt 8a associated with the reserve sliver 7 to be disposed vertically above or below the belt 8 associated with the sliver 2 (not shown). The leading end of the reserve sliver then converges with the running-out end of the sliver 2 immediately after the delivery station 11.
The construction according to the invention is suitable for the uniform mixing of various fiber components, for example, of cotton and synthetic fibers.
The division of the conveyors into individual conveyor belts arranged in groups enables the divided feed zone to be better adapted to conditions of space, i.e., the apparatus can be adapted even to relatively small spaces. In the case of a division, for example, into two groups, each group can be provided for a particular fiber component to make a mix.
The division of the conveyor belts into two groups, for example, prevent errors in the feeding-in of reserve cans and the control is better.
FIGS. 5 to 15 show details of the feed table 1 with its conveyor belts 8, 8a which are separate from each other, guided on deflecting rolls 30 and moved in the conveying direction z by drive rollers 32. The conveying belts 8, 8a have a breadth b of, for example, 40 mm.
Unlike the arrangement shown in FIG. 1, the drive roller 32 is not arranged near the motor 12 at the transfer location 11, but instead forms part of a module-like drive unit 34. This unit 34 comprises its own integrated drive means. Drive unit 34 is located at the infeed end 35 of a substantially horizontal support 38 which is made up from a plurality of support sections 38a, 38b, 38c. In accordance to FIG. 5, these sections are provided in three different lengths, N 1 , N 2 and N 3 in order to be able to assemble as many different overall lengths N of this support 38 as possible. The length N 1 of the support section 38a corresponds to half the length N 3 of the support section 38c, and the length N 2 of the support section 38b corresponds to one and a half times the length N 1 .
The supports 38 are assembled in graduated overall lengths N from these support sections 38a, 38b, 38c, and these supports rest on common transverse carriers 40, 40a. In the embodiment according to FIG. 11, the transverse carrier 40 comprises a carrier plate 41 and yokes 42 and this transverse carrier rests on two vertical posts 44. In contrast, the transverse carrier 40a in FIG. 12 is made in one piece and is screwed to a post 44 in the region of a support surface 43.
Each support 38 forms an exchangeable unit comprising the drive unit 34 and the deflector roll 30 mounted at the opposite end. This support 38, together with the transverse carriers 40, 40a and the vertical posts 44 (the foot portions of which have been omitted from the drawings), form part of a frame work 46 of the feed table 1.
The lower run 8t of the conveyor belt 8 or 8a running between the deflector roll 30 and drive roll 32 rests in the region of the transverse carriers 40, 40a on support rollers 48 which prevent sagging of the unsupported lengths of the slivers.
In the arrangement according to FIG. 11, these supports 38 or support sections 38a, 38b, 38c have a supporting tubular section 50 underneath of which a tubular or trough-shaped projection 52 is riveted or screwed. This projection receives each supporting roll 8. A U-shaped section 54 is mounted on the tubular section 50 and has leg elements 55, 55a, flanking the upper run 8h of the conveyor belt 8, 8n running in the interior 58 of the section 54. These elements also protect the fiber sliver 20 resting on the upper run 8h. The trough-projection 52 protects the lower run 8t in the same way. The section of the one section element 55 of the U-shaped section 54 is longer than that of the other section element 55a and a bentover portion 56 of this element 55 projects over the edge of the neighboring section element 55a in order to form an interlinked unit with the U-shaped section 54 having this element 55a.
In FIG. 11, the supports 38 are screwed to the carrier plate 41, whereas in FIG. 12 they are inserted between projections 39 of the transverse carrier 40a. These projections form a castellated shape. Furthermore, it is apparent from FIG. 11 that the tubular or trough-shaped projections 52 extend only over a portion of the support length N or N 1 , N 2 , N 3 . In the illustrated example, they are arranged one after the other in the transport direction z with mutually overlapping cross sections.
In order to tension the conveyor belt 8, 8a (as seen in FIG. 14), the deflector roll 30 is mounted in fork-shaped bearing members 60 of an adjustable arm 62 supported on the tubular profile 50 and axially movable along the longitudinal axis M thereof. The arm can be fixed in place for example by screws which are received in a mounting portion 66 and extend through a longitudinal slot 64 of the tubular section 50. The deflector roll 30 can, for example, have a diameter d of 50 mm and a circumferential breadth e of, in this case, 42 mm.
The adjusting arm 62 is divided in the longitudinal direction in order to enable easier exchangeability of the deflector roll 30 provided between two cheek plates 61 of the bearing members 60 (FIG. 14).
As can be seen especially from FIG. 15, the drive unit is secured to the feed end 35 of a tubular section 50. A pressure roll 68 rests on the circumference of the drive roll 32 of the unit 34 (or on a fiber sliver 20 running over this drive roll 32) and is linked by means of a pivot arm 70 to a lug 72 of the adjacent support 50b. A sensor 74 integrated in the drive unit 34 or, in accordance with FIG. 8, otherwise arranged in the infeed region, controls the belt movement in dependence upon the throughput of fiber sliver 2.
In changing of the conveyor belt 8, 8a, the support 38 is lifted away from its transverse carrier 40, 40a and the variably positioned diverter roll 30, which serves as a tensioning roll, is released. After mounting of a new conveyor belt 8, the new belt is tensioned by the diverter roll 30 and the support 38 is then reset in place. | The invention relates to a feed table for feeding slivers by way of a conveyor to a textile processing machine. The slivers are drawn off from associated spinning cans by way of draw-off devices and placed on the conveyor. In the event of a sliver running out or breaking, reserve slivers are fed in automatically by way of draw-off devices specifically devised for this purpose. The conveyor comprises individual conveyor belts associated with each sliver and each reserve sliver and have a draw-off devices, each conveyor belt being drivable by way of a controllable drive, the conveyor belts being a part of the draw-off devices. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Continuation Application of prior U.S. patent application Ser. No. 10/345,432 filed Jan. 14, 2003, which claims priority under 35 U.S.C. §119 to Korean Application No. 30804/2002 filed on May 31, 2002, whose entire disclosure is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a service of high quality digital image through internet, and particularly, to a method for providing various information through interactive user interface, wherein image data and each kind of professional data commonly used in daily life are provided to enhance utilization of image data.
[0004] 2. Description of the Background Art
[0005] In the related art, since data such as an advertising leaflet, a propaganda is booklet, a handbill, a pamphlet, and etc. are almost used for one time, advertisement and publicity effect is not great and the data did not last for a long time. Also, professional data include each kind of works of art, photo works exhibited in an art gallery and a pavilion. The data provide simple information and there was an inconvenience to visit an art gallery or a pavilion to appreciate the corresponding works.
[0006] In the related art, even if an art gallery or gallery service are provided through internet and various internet-album services are performed, enormous image corresponding to hundreds of sheets or ten thousands of sheets and enormous image corresponding to scores of MB or hundreds of MB were not processed in a constant network bandwidth, thereby limiting quality and size of service image. That caused image quality to be degraded and made it almost impossible to provide additional information (moving image, sound, and etc.) with image. That is resulted from that a limitation about a method for providing huge image real time through network is not overcame. Also, since image information is downloaded and then displayed on a screen, it was impossible for users to appreciate high quality works real time.
SUMMARY OF THE INVENTION
[0007] Therefore, an object of the present invention is to provide a method for utilizing high quality image as a synthetic medium, wherein general image data such as a photo, an advertising leaflet, a handbill, a propaganda booklet, a pamphlet, and etc. and professional image data such as art works and professional photo works are digitally made into huge and high quality, thereby providing the contents into high quality image through wire and wireless network and connecting the contents with relevant additional information.
[0008] To achieve these and other advantages and in accordance with the purpose of the present invention, as embodied and broadly described herein, there is provided a method for providing real time service of huge and high quality digital image on internet, wherein a server system for communicating with a plurality of client systems on internet and providing information by a request of the client system, comprises a high quality image conversion system for converting digital image into high quality image data format; an editing system for editing and reconstructing the converted data; and a database for storing the edited data, the system comprising the steps of editing and reconstructing the converted data; storing the edited data; and transmitting the stored data to the client system on internet at the time of request by the client system.
[0009] The foregoing and other objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention.
[0011] In the drawings:
[0012] FIG. 1 is a pattern diagram showing layered data;
[0013] FIG. 2 is a pattern diagram showing a process in which huge image is divided and transmitted.
[0014] FIG. 3 is a flow chart showing an overall process of a system for high quality digital image internet service according to the present invention;
[0015] FIG. 4 a is a pattern diagram showing graphic user interface (GUI) of high quality image edit program;
[0016] FIG. 4 b is a pattern diagram showing GUI of a menu region of high quality image edit program;
[0017] FIG. 4 c is a pattern diagram showing GUI of a working region of high quality image edit program;
[0018] FIG. 5 is a pattern diagram showing one embodiment of GUI of high quality digital image service according to the present invention;
[0019] FIG. 6 a is a screen capture showing one embodiment of GUI of a cyber gallery according to the present invention;
[0020] FIG. 6 b is a screen capture showing one embodiment of zoomed-in GUI of a cyber gallery according to the present invention;
[0021] FIG. 7 a is a screen capture showing one embodiment of GUI in which a user transmits a photo to a server in an internet album according to the present invention;
[0022] FIG. 7 b is a screen capture showing one embodiment of GUI showing completed album lists in an internet album according to the present invention;
[0023] FIG. 7 c is a screen capture showing one embodiment of GUI of an internet album according to the present invention; and
[0024] FIG. 7 d is a screen capture showing one embodiment of zoomed-in GUI of an internet album according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0025] Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings.
[0026] In a method for providing real time service of huge and high quality digital image on network, are processed small images transformed to be suitable to a main memory unit of a general personal computer. Accordingly, any huge image can be displayed in a user computer real time, and hyperlink such as another huge image, animation, and other media files can be provided with the huge image.
[0027] To this end, a new client/server model for transmitting huge image on internet is installed.
[0028] Characteristics of the present invention are as followings.
[0029] First, image encoding based on partial access.
[0030] Second, temporal storage (caching) of image information corresponding to a display screen in a client system where image information is transmitted and removal of unnecessary image.
[0031] Third, intellectual queuing and pipelining of a server which provides image information.
[0032] Image Encoding
[0033] Partial access divides very huge image into small sub cells, and converts into layered data having multiple zoom levels. That is, in the present invention, sub cells converted into high quality image data are transmitted instead of transmitting an overall huge image, thereby improving image-processing speed. Since users do not look an entire huge image by high resolution, only sub cells displayed on a screen are transmitted from database and displayed in the client system. Accordingly, amount of unnecessary data transmitted through network is largely reduced, thereby fast transmitting and displaying. Image division and layered data generation in the partial access will be later described.
[0034] Client System
[0035] If a user is connected to a server through internet, a client application is automatically transmitted from a server system to a client system. The application tracks a user's input contents and determines a position of a view pointer of which movement is determined on a screen by moving a mouse. According to that, necessary corresponding sub cells are all transmitted from the server and displayed. To minimize a loading on network, the client system temporarily stores sub cells around the view pointer. When a user searches image around the view pointer, relevant sub cells already exist in a memory. Therefore, a request for additionally transmitting image file is not needed.
[0036] If a user moves the view pointer, the client application requests sub cells regarding to a new image to the server. In the process, time delay can be generated at the time of transmitting data on network and processing in the server. However, if a user moves the view pointer and requests a new image, sub cells regarding to previous image are not needed any longer. The client application can additionally request the server to delete the sub cells, and by the request, load on network can be reduced.
[0037] Server System
[0038] Queue is a data structure in computer programming for removing data according to input orders. According to an intellectual queuing in the present invention, input and display are minimized in dealing with image request from numerous clients. For example, if a client A requests sub cells 1 , 2 , 3 and 4 and a client B requests 3 , 4 , 5 and 6 , a queuing layer receives the sub cells 1 , 2 , 3 , 4 , 5 and 6 as one order without overlapping the sub cells 3 and 4 . Accordingly, if numerous clients simultaneously request overlapped information, processing amount in the server is reduced, thereby processing fast.
[0039] In the meantime, the server system asynchronously processes numerous requests from the client by using pipelining. Generally, if users request to the server, they wait a response from the server for a while. If the server can not perform one request, a series of requests from the client are interrupted. In the present invention, a client can simultaneously transmit numerous requests to a server through pipelining.
[0040] A pipeline means that movement of command words towards a processor or an arithmetical step by the processor to perform the command words are consecutive and overlapped. If a pipeline does not exist, a processor in computer takes first command words from a memory, performs a calculation requested by the command words, then takes next command words from the memory. While taking the command words, an arithmetical calculation part of the processor has to rest with waiting for next command words to arrive.
[0041] If the pipeline is used, it is possible to take next command words while the processor performs an arithmetical calculation and bring the words to a buffer around the processor until next command words are performed. A step for bringing command words is continuously repeated. As a result, a number of command words performed in a set time is increased.
[0042] In the present invention, the server allocates a special address for each request transmitted from numerous clients, and immediately transmits a response to the client as soon as the request is performed. At this time, the transmitting order needs not to be equal to an order which the server receives a request. By the pipelining, the server can respond to the client system faster than a user's expectation.
[0043] Image Encoding
[0044] In the present invention, digital information including huge image information is converted into high quality digital image data on the basis of partial access by the following processes.
[0045] (1) converting huge image into multiple layered data with levels
[0046] (2) dividing the huge image into numerous sub cells
[0047] (3) compressing the images into divided cell units
[0048] To convert into high quality image data, general image files such as BMP, GIF, PNG, JPG, etc. are used as original text contents. Also, some advertisement data made by PDF are converted into image file for use.
[0049] Layered Data Generation
[0050] In the present invention, image data having a layered structure are generated so as to provide high quality image in which images of multimedia digital publication and etc. transmitted real time on network are magnified or contracted fast and accurately according to levels. That is, a plurality of data layers converted with ½″, . . . , ¼, ½, 1 times, etc. of an original image are generated.
[0051] FIG. 1 is a pattern diagram showing layered data with magnification or contraction levels. As shown in FIG. 1 , high quality individual images are constituted by layers according to displayed levels at the time of magnification or contraction, and respective layers 70 , 80 , and 90 are used in magnification or contraction steps. That is, in case of magnifying, images are displayed from upper data 70 to bottom data 90 via middle data 80 . On the contrary, in case of contracting, images are displayed in reverse order. Also, it is possible to change the displayed screen discontinuously.
[0052] A number of layers in the layered structure are determined by graphic user interface (GUI). In FIG. 1 , data layers of three steps are illustrated, but if graphic user interface can provide a function of magnification or contraction with four steps, image data are converted to have four layers.
[0053] Division of Huge Image
[0054] The generated data layers are divided into a plurality of sub cells. By dividing the data, huge image is fast transmitted. Division units of the huge image into a plurality of sub cells are determined by a processing ability of a client system and a transmittance speed on network. At this time, a number of sub cells are determined within an optimum scope. Indexes are endowed to each cell of the divided images, and the images are integrated by positions or orders. The integrated cells exist as one file, but only corresponding cells of the huge image are transmitted by a client's request. According to this, a client can fast see his wanted image.
[0055] Referring to FIG. 2 , a process for displaying the divided image data real time on network will be explained. Individual image data 110 and 120 stored in database consist of sub cells respectively. In Figure, Eij and Fij represent sub cells of i line and j column.
[0056] As aforementioned, dividing image data into each sub cell unit and then storing is determined by a processing ability of a client system and a transmittance speed on network. At this time, if a large number of sub cells are divided, a processing speed in a central processing unit of a client system is down, and if few sub cells are divided, a transmittance speed on network is down. Therefore, it is important to divide the sub cells within an optimum scope.
[0057] For example, supposing that screen display resolution is 1024.times.768 pixel, images displayed on a screen-are divided into 5 horizontal sub cells and 4 vertical sub cells. The cells divided at an optimum condition prevent delay in a transmitting process or in a display process, and transmit image fast.
[0058] The divided sub cells are compressed, and endowed with indexes, so that positions and coordinates etc. in an overall image are recorded. Then, the sub cells are integrated into one file and stored in database.
[0059] High quality image data according to the present invention are stored as a compressed form so as to improve a transmittance speed.
[0060] It is preferable to compress data into each divided sub cell unit. At this time, compression technique such as widely known JPEG, GIFE are used. Each sub cell can be compressed with a same method independently, or compressed with different methods. For example, in case of data having a figure and a picture together, GIF compression is used at the figure and JPEG compression is used at the picture. By doing so, it is possible to improve compression efficiency of an image.
[0061] The compressed sub cells are integrated according to orders and positions, and are endowed with indexes respectively, then stored in database. The indexes can include not only base information of sub cells but also additional information relevant to the sub cells. A server system is connected to the indexes and selects sub cells of a wanted image, thereby fast transmitting.
[0062] Hereinafter, the present invention will be explained in detail with reference to preferred embodiments.
[0063] FIG. 3 is a flow chart showing an overall process of a system for high quality digital image internet service according to the present invention. First of all, contents are collected from an advertiser, a painter, a photographer, or individual users ( 160 ). In the contents-collecting step, additional information regarding to each content, for example, moving image file, sound file, text explanation data, etc. are together included. The collected contents are converted into image files, or scanned to be converted into digital information, thereby being made into high quality image data according to the present invention ( 170 ). The high quality image data can be edited in a temporarily stored state ( 180 ). High quality image data having completed edition are respectively stored in image database and additional information database ( 190 ), and transmitted from the server to the client system through internet by a client's request. The process will be explained as follows.
[0064] All kinds of contents off line, for example, a general photo, an advertising leaflet, a propaganda booklet, a pamphlet, a work of art, and etc. are scanned or converted into a digital photo, thereby being made into high quality digital image data. High quality data can be constituted with index data including additional information (moving image, sound, flash animation, and web page, etc.) or individually extracted keywords necessary to search.
[0065] The completed high quality digital image can be individually stored or stored by reconstructing the relevant contents as one package form. In the case, a separate program for edition can be used. Details for that will be later explained.
[0066] The server system transmits corresponding image regions (sub cells corresponding to parts requested by users) according to users' requests through internet by a program (client application) for real time serving the converted contents into high quality image data. In the client system, contents can be real time browsed by a browser such as internet explorer, and etc.
[0067] A method for a user to generate high quality image data according to the present invention includes a download method and a method using a server program.
[0068] In the download method, high quality image conversion program is downloaded to be installed in a user's computer system, then, general image data are converted into high quality image, thereby uploading to an internet server. In the method using a server program, a user uploads a general image to the server, then directly makes high quality image on internet by using programs installed to the server. In the present invention, a user and a server are interactive by communicating each other, thereby more satisfying a user's request and maximizing a service effect by a user's participation.
[0069] The high quality image data made in the above process are stored in a temporal storage unit of the server.
[0070] A method of the present invention includes an editing process for directly constituting a gallery or an internet album site by using high quality image data besides a making process for making high quality image data by a user. The temporarily stored high quality image passes an editing process shown in FIG. 4 a or 4 c.
[0071] FIG. 4 a is a pattern diagram showing one embodiment of GUI of high quality image editing program. The editing program consists of a menu region 210 , a working region 220 , and a tool-collecting region 230 . FIG. 4 b shows one embodiment of the menu region 210 . The menu region includes menus such as canvas, edition, panel, view, help, and etc., or can include sub menus according to each function.
[0072] The working region 220 is a space where high quality image is brought to perform various workings.
[0073] In the tool-collecting region 230 , shortened icons of frequently used menus and special menus are made, thereby making the working convenient.
[0074] A user can store image data as individual image by using an editing program, or can store as a canvas unit by constituting the necessary image data as one package form. Also, it is possible to add a panel to each high quality image data, and to connect multimedia additional information such as moving image, sound, flash, and etc. with a text. In case of storing image data as a canvas unit, as shown in FIG. 4 c, several high quality images 260 a and 260 b are brought in one canvas (working region) 250 , then a user sets and changes size, color, multimedia additional information, text, position, and etc.
[0075] High quality image or canvas completed by using the editing program are stored in a separate database.
[0076] Since the editing program is performed in a server, a user is connected to the server to use the editing program and then the completed high quality image lo or canvas are stored in a separate database.
[0077] FIG. 5 is a pattern diagram showing a user interface for displaying high quality image display. The user interface consists of a function button region 310 , a section menu and searching region 320 , and an image display region 330 .
[0078] The function button region 310 includes a tool for selecting contents according to kinds, a tool for selecting a part of displayed image, a tool for displaying the selected region, and a scrap function for storing the selected region or individual images as another file.
[0079] In the section menu and searching region 320 , contents are sub-classified by constructions, and corresponding image information is included. The searching region consists of a part for inputting a searching keyword and a part for showing a searching result. The searching result is shown at a bottom of the section menu as a list form.
[0080] In the image display region 330 , selected images are displayed. GUI shown in FIGS. 4 a and 5 is only one embodiment, and other transformed GUI will possibly be provided.
[0081] FIGS. 6 a and 6 b are preferred embodiments according to the present invention showing a digital gallery to which a method of the present invention is applied.
[0082] In the meantime, FIGS. 7 a and 7 b are preferred embodiments according to the present invention showing a digital album to which a method of the present invention is applied.
[0083] FIG. 7 a is a screen capture showing one embodiment of GUI in which a user transmits a photo to a server in an Internet album according to the present invention. FIG. 7 b is a screen capture showing one embodiment of GUI showing completed album list in an internet album according to the present invention. FIG. 7 c is a screen capture showing one embodiment of GUI of an internet album according to the present invention. FIG. 7 d is a screen capture showing one embodiment of zoomed-in GUI in an internet album according to the present invention.
[0084] High quality image transmitted from database of the server can be displayed by various methods.
[0085] High quality image data are transmitted with only regions displayed on a screen by a user's request. That is, if a user moves images by using a mouse, only newly displayed region is transmitted from the database and displayed. Therefore, the user moves high quality digital image to any wanted directions. Also, if the user clicks a wanted part with a mouse, the part can automatically move to a center of a screen.
[0086] Image magnification or contraction function is performed by locating a mouse cursor to a wanted part and clicking. The magnification or contraction can be performed by a layer unit step by step, or can be performed at one time from the highest step to the lowest step. At this time, the new data are displayed by receiving data from the server. In case of magnifying or contracting image, various effects can be simultaneously realized by using contents such as sound, image, text, and flash animation, etc.
[0087] In case that hyper-linked additional information exists at a special position of image, the corresponding information is displayed on a screen real time. At this time, the additional information can be displayed on a current window, or on a new window. Additional information data that will be used with high quality image includes moving image file, sound file, flash animation, another high quality image file, text information, and web page address, etc.
[0088] The present invention has the following advantages. According to the real time service of high quality multimedia digital gallery and the method of the present invention, image data and additional data interactive to one another are provided by one graphic user interface. As a result, a user can simultaneously obtain various information easily, can fast search wanted information on an image screen which is fast displayed, and can obtain the same resolution even if at the time of magnifying the screen to search minute information. Therefore, a user is provided with individual images close to intuition and can use various additional information.
[0089] As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, unless otherwise specified, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the metes and bounds of the claims, or equivalence of such metes and bounds are therefore intended to be embraced by the appended claims. | A method for providing real time service of huge and high quality digital image on internet is disclosed, wherein data relevant to a general life such as a general photo, an advertising leaflet, and a pamphlet and professional image data exhibited in an art gallery, exhibition grounds, a pavilion are made into huge and high quality digital image or scanned and photographed to be digital, thereby processing real time service as an interactive browsing form. In the present invention, data are directly made, edited, constructed, and uploaded on internet, thereby providing various additional information with image through hyperlink and processing high quality digital image service on network without speed delay for huge image. | 7 |
BACKGROUND OF THE INVENTION
1. Field of Invention
This invention relates to a method of improving the memory of living animals with certain arylamidoazabicycloalkanes. The invention contemplates the treatment of memory deficiencies and disorders associated with Alzheimers disease and other forms of sinility.
2. Information Disclosure Statement
Various chemicals such as physostigmine, arecholine, choline or piracetam have been reported to facilitate memory in animals, KIRK OTHMER, ENCYCL. CHEM. TECHNOL., 3rd Ed. (1981) Vol. 15, pp 132-142 and ANNUAL REPORTS IN MEDICINAL CHEMISTRY (1984) Vol. 19, pp 31-43. The cardiovascular drug procainamide has been tested for learning enhancement activity in experimental animals of different ages and has been said to improve learning deficits in aging rats KIRK OTHMER ibid p. 139. Ergoloid Mesylates have been used in treatment of impaired mental function in the elderly. The ergoloid mesylates may in some cases give rise to nausea during treatment for mental impairment and may possess α-adrenergic blocking activity. THE MERCK INDEX 10th Ed. 3596 and PHYSICIANS DESK REF., 38th Ed. 1984, pp 911-912. In contrast, certain of the compounds of the formula used in the present invention have antinauseant properties and are not α-adrenergic blocking agents, cholinomimetics, cholinesterase inhibitors or stimulants.
2-Alkoxy-N-(1-azabicyclo[2.2.2]oct-3-yl)benzamides and thiobenzamides and their use in a method for increasing gastric emptying and alleviating emesis, particularly emesis due to administration of platinum and anticancer drugs such as cisplatin are disclosed in copending U.S. application Ser. No. 597,275 filed Apr. 6, 1984. Certain of these 2-alkoxy-N-(1-azabicyclo[2.2.2]oct-3-yl)benzamides are also disclosed in Fr. Pat. No. 2.529.548 and European Patent application No. 099.789A and their use as gastrointestinal motility accelerators and as potentiators for medicaments, especially analgesics such as aspirin and paracetamol is also disclosed. Certain of the compounds are also disclosed as useful as analgesics-antipsychotics in Brit. Patent application No. 2,125,398A.
Syntheses of certain N-(1-azabicyclo[2.2.2]oct-3-yl)benzamides have been reported by E. E. Mikhalina, et al., in KHIM-FARM. Zh. (1973) 7 (8) p. 20-24: C.A. 79 146358a. The compounds were reported to possess narcotic, nerve center blocking and hypotensive activity.
The compound 4-amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-3-chloro-5-trifluoromethyl-benzamide has been reported in U.S. Pat. No. 4,093,734 in a class of compounds said to be anxiolytics, anticonvulsants, antiemetics and antiulcerogenics.
Certain of the compounds encompassed by Formula I and useful in the method of the present invention and exemplified by N-(7-octahydroindolizinyl)benzamides and N-(1 and 2-quinolizinyl)benzamides are disclosed by structure, method of synthesis and characterization in U.S. Pat. No. 4,213,983 as being useful in treating gastro-intestinal misfunctions. Still other compounds of Formula I useful in the present invention and exemplified by 4-amino-4-chloro-2-methoxy-N-[4'-α,β-(1'-aza-2'-α-phenyl-6'-α-N-bicyclo[4,3,0]decyl)]benzamide and 4-amino-5-chloro-2-methoxy-N-[7'β-(9'β-methyl-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide are disclosed by structure, method of synthesis and characterization in European patent application 0067565A1 as dopamine antagonists for treating impaired gastric motility.
SUMMARY OF THE INVENTION
The arylamidoazabicycloalkanes useful in the method of this invention for improving memory or correcting memory deficiency have the general formula: ##STR2## wherein , n 1 , n 2 , n 3 and n 4 =0 to 3
R 1 , R 2 , R 3 , and R 4 =H, loweralkyl or phenyl
R 5 =H or loweralkyl
X=O or S ##STR3## Y=H, loweralkoxy, loweralkylthio, halo, tri fluoromethyl, amino, loweralkylamino, dialkylamino, arylamino, acyl, aminosulfonyl, loweralkylsulfonyl, nitro or aminocarbonyl;
m=1 to 3
Z=amino, loweralkylamino or diloweralkylamino;
the optical isomers; and the pharmaceutically acceptable acid addition salts, including hydrates and alcoholates thereof.
The compounds are administered using usual pharmaceutical procedures and carriers as described hereinbelow.
In the further definition of symbols and in the formulas hereof and where they appear elsewhere throughout this specification and in the claims, the terms have the following significance.
The term "loweralkyl" as used herein, unless otherwise specified, includes straight ond branched chain radicals of up to eight carbons inclusive and is exemplified by such groups as methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, tert-butyl, amyl, isoamyl, hexyl, heptyl and octyl radicals and the like. The term "loweralkoxy" has the formula --O--loweralkyl.
The term "halo" or "halogen" when referred to herein includes fluorine, chlorine, bromine and iodine unless otherwise stated.
"Pharmaceutically acceptable salts" include acid addition salts and hydrates and alcoholates thereof which are physiologically compatible in living animals. The acid addition salts may be formed by either strong or weak acids. Representative of strong acids are hydrochloric, hydrobromic, sulfuric and phosphoric acids. Representative of weak acids are fumaric, maleic, mandelic, tartaric, citric, oxalic, succinic, hexamic and the like.
The test relied upon to test for memory enhancement involves a passive avoidance procedure with trained mice as described hereinbelow under "Pharmacological Testing."
DETAILED DESCRIPTION OF THE INVENTION
The memory enhancing agents of Formula I above, useful in the method of this invention, may be prepared generally by methods for preparing such amides as described in copending U.S. application Ser. No. 597,275 mentioned above in French Pat. No. 2.529.548, European patent application ED No. 67565 and U.S. Pat. No. 4,213,984. Two principal general methods, A and B, are illustrated in the following equations for preparation of arylamidoazabicycloalkanes: ##STR4##
Method A is illustrated by Examples 5, 6, 7, and 9. ##STR5##
Method B is illustrated by Examples 1, 3 and 8.
Compounds of Formula I wherein Ar has a primary amino substituent may also be prepared from a compound prepared by Methods A or B wherein the substituent is nitro by catalytic reduction of the nitro group to the amino group. Alternatively, such amino compounds may be prepared by Method A, utilizing a starting aroyl halide wherein the amino substituent has been protected and thereafter deprotected.
Amide formation may also be accomplished by heating an arylacid ester with the amine in an inert solvent.
The acid addition salts of compounds of Formula I may be prepared in conventional manner by reacting a free base with a pharmaceutically acceptable acid as described above.
The free base of an acid addition salt may be obtained by partitioning the salt in an organic solvent such as methylene chloride and a weak basic aqueous solution and thereafter separating and evaporating the organic solvent layer.
Compounds in this invention may exist in racemic form or they may be separated into optical isomers by procedures described in Fr. Pat. No. 2,529,548. Thus, this invention encompasses racemic and optically active forms.
Preparation of Thioarylamides
The preparation of the thioarylamide compounds encompassed by Formula I may be accomplished by mixing and reacting a benzamide compound of Formula I with a mixture of phosphorus pentasulfide (P 2 S 5 ) and potassium sulfide (K 2 S) or by mixing and reacting 3-aminoquinuclidine with an appropriately substituted arylaldehyde and sulfur. The reaction sequences are illustrated by the following equations: ##STR6##
A preferred group of compounds encompassed by Formula I useful in the method of this invention have the formula: ##STR7## wherein Am is amino (i.e., --NH 2 ) or methylamino.
The following examples are provided merely by way of illustrating the methods of preparation of compounds useful in the method of the invention and are not to be construed as limiting in nature.
EXAMPLE 1
4-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-5-chloro-2- methoxybenzamide, fumarate [1:1]
In a closed system equipped with an oil bubbler, 30 ml of tetrahydrofuran was added to a mixture of 4-amino-5-chloro-2-methoxybenzoic acid, 2.02 g, (0.010 mole) and 1,1'-carbonyldiimidazole, 1.62 g (0.010 mole) with stirring. When evolution of carbon dioxide ceased, nitrogen was bubbled through the reaction mixture for 1 hr. A solution of 3-aminoquinuclidine, 1.26 g, (0.010 mole) in 10 ml tetrahydrofuran was added dropwise to the stirred reaction mixture and stirring at room temperature continued for 3 hrs. TLC analysis (3% conc. ammonium hydroxide solution in methanol) showed some product formation. The mixture was heated at reflux temperature for 18 hours and then concentraded to an oil. TLC analysis showed the presence of the product, imidazole, and 3-aminoquinuclidine. The oil was dissolved in methylene chloride (75 ml) and washed twice with 50 ml portions of aqueous sodium bicarbonate solution. The methylene chloride layer was dried over anhydrous magnesium sulfate and concentrated to yield 2.0 g (67%) of a glassy amorphous solid, the free base of the title compound.
In another reaction on a 0.020 mole scale, 5.18 g (83.8%) of the product as the free base was obtained.
The products were combined, dissolved in methanol (20 ml) and the solution and treated with a solution of fumaric acid (2.73 g) in methanol (50 ml). Absolute ether was added to precipitate the salt which was collected by filtration and recrystallized from methanol-water (200:20) with isopropyl ether added to the point of incipient cloudiness. The recrystallized salt (5.38 g) melted at 223°-225° C.
Analysis: Calculated for C 19 H 24 N 3 O 6 Cl: C, 53.59; H, 5.68; N, 9.89. Found: C, 53.35; H, 5.72; N, 9.95.
EXAMPLE 2
4-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxybenzamide, hydrochloride, hydrate (1:1:1)
To an isopropyl alcohol solution of the free base of the title compound such as was obtained by the procedure midway through Example 1 is added in equal molar amount of 37% (conc.) hydrochloric acid. A salt is separated by addition of acetone followed by filtration which is recrystallized from acetone-water to give the title compound, m.p. 158°-160° C.
EXAMPLE 3
N-(1-Azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxy-4-methylaminobenzamide, fumarate [1:1]
To a mixture of 1,1'-carbonyldiimidazole, 1.23 g (0.00756 mole) and 5-chloro-2-methoxy-4-methylaminobenzoic acid, 1.63 g (0.00756 mole) was added 50 ml of tetrahydrofuran. Nitrogen was bubbled into the solution for 30 minutes to remove any carbon dioxide that was present. To the solution was added 3-aminoquinuclidine, 0.95 g, (0.00756 mole) in one portion, and the reaction mixture was stirred at ambient temperature for 16 hours. The reaction mixture was concentrated to an oil which was shown to be 1:1 mixture of the free base of the product and imidazole. The mixture was dissolved in 20 ml methanol and treated with a solution containing 0.47 g fumaric acid in 20 ml of hot methanol. Upon cooling, 1.52 g of white solid formed. Recrystallization from water-methanol gave 0.84 g of the product as a white solid; m.p. 237°-238° C.
Analysis: Calculated for C 20 H 26 N 3 O 6 Cl: C, 54.61; H, 5.96; N, 9.55. Found: C, 54.61; H, 5.98; N, 9.51.
EXAMPLE 4
N-(1-Azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxy-4-(methylamino)-benzamide, hydrochloride (1:1)
To an isopropyl alcohol solution of the free base of the title compound, such as was obtained by the procedure of Example 3, is added an equal molar amount of 37% (conc.) hydrochloric acid. The crude salt is separated by filtration and recrystallized from ethanol-water to give the title compound, m.p. 255°-258° C.
EXAMPLE 5
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-methoxybenzamide, fumarate [1:1]hemihydrate
In a closed system equipped with an oil bubbler, a solution of 2-methoxybenzoyl chloride, 2.76 g (0.0016 mole) in 50 ml absolute ether was added dropwise over 10 min to a stirred solution of 3-aminoquinuclidine, 1.81 g (0.0144 mole) in 100 ml absolute ether. After the addition was completed, the mixture was stirred at room temperature for an additional 2 hrs. The solid hydrochloride salt was collected by filtration under nitrogen. The salt (3.83 g) was dissolved in sodium bicarbonate solution and extracted twice with 25 ml portions of methylene chloride. The extract was dried over magnesium sulfate and concentrated to yield 1.25 g clear oil (33.3%). TLC analysis (3% conc. ammonium hydroxide in methanol) showed the free base to be pure. A solution of 1.17 g of the free base in 5 ml methanol was treated with a solution of 0.52 g fumaric acid in 10 ml methanol. Isopropyl ether was added to give approximately 100 ml of solution from which the fumarate salt precipitated. The salt was collected under nitrogen and dried in a vacuum oven at 60° C. overnight. NMR and elemental analyses showed that the product was a hemihydrate.
Analysis: Calculated for C 19 H 25 N 2 O 6 .5 : C, 59.21; H, 6.54; N, 7.27. Found: C, 59.18; H, 6.30; N, 7.25.
EXAMPLE 6
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2,4-dimethoxybenzamide hydrochloride [1:1]
A mixture of 3-aminoquinuclidine dihydrochloride, 6.95 g, (0.0349), 2,4-dimethoxybenzoyl chloride, 700 g, (0.0349 mole), anhydrous sodium carbonate, 36.99 g, (0.349 mole), 175 ml water, and 175 ml chloroform was stirred rapidly to achieve good mixing of the 2 layers for 20 hrs. The chloroform layer was then separated, washed with water, dried over anhydrous magnesium sulfate, and concentrated to an impure oil. The oil was triturated twice with 20 ml portions of petroleum ether to remove some impurities. The oil was then dissolved in ether and filtered to remove a small amount of insoluble material. The filtrate was treated with ethereal hydrogen chloride and the resulting salt collected to yield 2.70 g (23.7% yield) white solid. The salt was recrystallized from ethanol-isopropyl ether. Further recrystallization from methanol-ethyl ether yielded a white solid, m.p. 211°-212° C. The NMR analysis was satisfactory.
Analysis: Calculated for C 16 H 23 N 2 O 3 Cl: C, 58.80; H, 7.09; N, 8.57. Found: C, 58.38; H, 7.13; N, 8.44.
EXAMPLE 7
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2,4-dimethoxybenzamide, sulfate [1:1]
In a closed system equipped with an oil bubbler, a solution of 2,4-dimethoxybenzoyl chloride, 13.08 g, (0.0652 mole) in 200 ml absolute ether was dded dropwise over 30 minutes to a stirred solution of 3-aminoquinuclidine, 7.80 g, (0.0619 mole) in 200 ml absolute ether. The mixture was stirred overnight, and the solid hydrochloride salt of the product was filtered under nitrogen. The material was dried in a vacuum oven at 40° C. to give 18.70 g (92%). A 2.94 g (0.009 mole) portion of the hydrochloride salt in 20 ml methanol was treated with a solution of sodium methoxide prepared from 0.23 g (0.010 mole) sodium metal and 10 ml methanol. After standing a few minutes, the mixture was filtered and the filtrate concentrated on a rotary evaporator, and the residue was triturated with 75 ml methylene chloride. After filtering to remove some insuluble solids, the filtrate was concentrated to yield 2.53 g of the free base of the title compound (97% recovery from the hydrochloride salt). The free base was dissolved in 100 ml acetone and concentrated sulfuric acid (0.483 ml) added dropwise with stirring. The solid that formed was collected under nitrogen to give 2.76 g of the salt which recrystallized from methanol-isopropyl ether and dried in a vacuum oven at 60° C. for 2 hrs and then overnight at 78° C.; m.p. 223°-225° C.
Analysis: Calculated for C 16 H 24 N 2 O 7 S: C, 49.47; H, 6.23; N, 7.23. Found: C, 49.41; H, 6.30; N, 7.25.
EXAMPLE 8
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2,4-dimethoxybenzamide, fumarate [1:1.5]
In a closed system equipped with an oil bubbler, tetrahydrofuran, 100 ml, was added to a mixture of 2,4-dimethoxybenzoic acid, 3.64 g (0.020 mole) and 1,1'-carbonyldimidazole, 3.24 g (0.020 mole). No evolution of carbon dioxide was observed and after stirring for 3 hrs, TLC (ethyl acetate) and mass spectral analysis showed that the starting material had reacted to form (2,4-dimethoxybenzoyl) imidazole and imidazole. A solution of 3-aminoquinuclidine, 2.52 g (0.020 mole) in 10 ml tetrahydrofuran was added to the mixture, and the solution was heated to reflux temperature for 1 hr and then allowed to stand overnight at room temperature. A solution of fumaric acid, 2.32 g (0.020 mole in 50 ml methanol was added to the reaction mixture. Tetrahydrofuran was added until the solution became slightly turbid. The solution was chilled in a refrigerator. The solid which precipitated from solution was collected by filtration and found to be a fumarate salt of 3-aminoquinuclidine. The filtrate was concentrated to an oil and triturated with tetrahydrofuran. The solid precipitate which formed on standing was filtered and shown by TLC (3% concentrated ammonium hydroxide in methanol) to be the desired product plus traces of imidazole and 3-aminoquinuclidine. Recrystallization from methanol-iropropyl ether gave 5.41 g white crystalline solid (67% yield calculated as the monofumarate). NMR and elemental analysis showed the salt to contain less than one equivalent of fumaric acid. The salt was dissolved in boiling methanol (50 ml) and treated with an additional 0.77 g (0.0066 mole) fumaric acid in 10 ml hot methanol. Isopropyl ether was added until the hot solution became turbid. The solid obtained on cooling was collected, recrystallized from methanol-isopropyl ether and dried in a vacuum oven at 78° C. overnight. NMR and elemental analysis showed the salt to be a 1.5 fumarate, m.p. 192°-192.5° C.
Analysis: Calculated for C 22 H 28 N 2 O 9 : C, 56.89; H, 6.08; N, 6.03. Found: C, 56.81; H, 6.13; N, 6.04.
EXAMPLE 9
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-propoxybenzamide hydrochloride [1:1]
To a solution of 3.82 g (0.0192 mole) of 3-amino quinuclidine dihydrochloride in about 25 ml of carbon dioxide-free water was added 8 g (0.025 mole) of barium hydroxide octahydrate. The mixture was warmed for 5 minutes and then dried to a powder on a rotary evaporator. While protecting from contamination with carbon dioxide in the atmosphere, the powder was extracted in sequence with hot benzene and a 1:1 mixture of benzene-methylene chloride solution. The combined extracts were dried over magnesium sulfate and the mixture filtered. To the filtrate with agitation was added dropwise a solution of 3.4 g (0.0171 mole) of 2-propoxybenzoyl chloride in 50 ml of methylene chloride. The mixture was warmed on a steam bath to evaporate about 75% of the methylene chloride. Ligroin (60-110) was added and the mixture solidified. The solid was recrystallized from anhydrous ethyl alcohol to give 3.9 g (62.0%), m.p. 210°-211° C.
Analysis: Calculated for C 17 H 25 N 2 O 2 Cl: C, 62.86; H, 7.75; N, 8.62. Found: C, 62.62; H, 7.59; N, 8.54.
EXAMPLE 10
N-(1-Azabicyclo[2.2.2]oct-3-yl)-3-methoxy-2-naphthalenecarboxamide, hydrochloride [1:1]
A solution of 1.69 g (0.00768 mole) of 3-methoxy-2-naphthoic acid chloride in 15 ml of methylene chloride was added dropwise to a stirred solution of 0.97 g (0.00768 mole) of 3-aminoquinuclidine in 25 ml of methylene chloride in a closed system equipped with an oil bubbler. The reaction mixture was stirred overnight at ambient temperature, and then concentrated to give an off-white glassy solid. Two recrystallizations from methanol-isopropyl ether gave 1.95 g (73.4%) of the product as an off-white solid which was vacuum dried at ambient temperature, m.p. 248°-252° C.
Analysis: Calculated for C 19 H 23 N 2 O 2 Cl: C, 65.79; H, 6.68; N, 8.08. Found: C, 65.40; H, 6.72; N, 8.01.
EXAMPLE 11
4-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxythiobenzamide fumarate
One half mole of 4-amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxybenzamide fumarate is partitioned between dilute sodium hydroxide and 400 ml of benzene. The benzene solution is dried with sodium sulfate and distilled to a volume of 250 ml. To this is added a finely-ground mixture of 9 g of phosphorous pentasulfide and 9 g of potassium sulfide. The mixture is refluxed for 4 hr. and an additional 9 g of phosphorous pentasulfide is added and reflux continued for 2 hr. The benzene is decanted off. The solid is dissolved in a suitable solvent and reacted with fumaric acid to give the title compound.
EXAMPLE 12
N-(1-Azabicyclo[2.2.2]oct-3-yl)-4-nitrobenzamide hydrochloride hydrate [1:1:0.75]
A solution of 3-aminoquinuclidine dihydrochloride (5.0 g, 0.0246 mole) in ca. 15 ml methanol/5 ml water was treated with barium hydroxide octahydrate (9.0 g, 0.0286 mole), warmed over steam for ca. 10 min, then taken to dryness on the rotary evaporator at 40°-45° C./35 mm. The resultant dry powder was repeatedly extracted with ca. 6×50 ml dry tetrahydrofuran. The tetrahydrofuran solution was concentrated by boiling until an 80-90 ml volume remained. This clear solution was added dropwise with stirring to a hot solution of 4-nitrobenzoyl chloride (4.36 g., 0.235 mole) in benzene. The solid produced was recrystallized from anhydrous methanol several times to yield 5.13 g of solid, melting at 277°-279° C. Microanalysis and NMR showed 0.75 mole of water present. Mass spec. and IR were satisfactory, yield of title compound was 0.186 mole (79.4%).
Analysis: Calculated for C 56 H 78 Cl 4 N 12 O 15 : C, 51.70; H, 6.04; N, 12.92. Found: C, 51.48; H, 5.93; N, 12.91.
EXAMPLE 13
4-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)benzamide Hydrochloride
A solution of N-(1-azabicyclo[2.2.2]oct-3-yl)-4-nitrobenzamide hydrochloride (11.55 g., 0.037 mole) in 170 ml of 80% aqueous methanol was shaken in a hydrogen atmosphere with a platinum oxide catalyst on the Parr hydrogenator. The calculated volume of hydrogen was taken up in one hour. The catalyst was filtered off through Celite and the filtrate taken to dryness via rotary evaporator. Several recrystallizations of the colorless crystalline residue from 70% aqueous methanol produced a solid melting above 310° C. NMR, MS, and IR supported the proposed structure. Yield of title compound was 8.43 g. (81.2%).
Analysis: Calculated for C 14 H 20 N 3 OCl: C, 59.67; H, 7.15; N, 14.91. Found: C, 59.26; H, 7.11; N, 14.87.
EXAMPLE 14
5-Aminosulfonyl-N-(1-azabicyclo[2.2.2]oct-3-yl)-2-methoxybenzamide Hydrochloride Hydrate [1:1:0.25]
A solution of 3-aminoquinuclidine dihydrochloride (2.5 g, 0.0126 mole) in 25 ml of water was treated with approximately 5 g of KOH and the resultant slurry/solution taken to complete dryness on the rotary evaporator at 50°/35 mm. The dry residue was carefully extracted by repeated triturations with warm tetrahydrofuran until a total volume of 130 ml had been collected and dried over magnesium sulfate. This solution of 3-aminoquinuclidine base was treated with a solution of 2-methoxy-5-sulfamylbenzoyl chloride (2.92 g, 0.0117 mole) in 50 ml of dry tetrahydrofuran by dropwise addition under nitrogen. The resultant very turbid solution was refluxed gently for about 30 min, then freed of tetrahydrofuran by allowing it to evaporate. The residue was taken up in 90% ethanol containing a few drops of ethereal hydrogen chloride, filtered and chilled. The solid produced was then recrystallized again to yield 4.3 g (97%), m.p. 233°-234° C. NMR, MS, and IR were in support of the structure proposed.
Analysis: Calculated for C 60 H 90 Cl 4 N 12 O 17 S 4 : C, 47.37; H, 5.96; N, 11.05. Found: C, 47.28; H, 5.93; N, 10.87.
EXAMPLE 15
2-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)benzamide Dihydrochloride
The free base was liberated from 3-aminoquinuclidine dihydrochloride (4.0 gm, 0.020 mole) using barium hydroxide and keeping the process under dry nitrogen. The base thus obtained (0.018 mole) was dissolved in dry tetrahydrofuran, treated with isatoic anhydride (2.04 gm, 0.018 mole) and brought to reflux. The clear, dark brown solution within five minutes became tan-turbid. Reflux was continued for 1 hr, the excess tetrahydrofuran distilled off, and the residue added to boiling ethanol. A small amount of insoluble solid was filtered off. Chilling produced 3.8 g (68%) crystalline amine base, m.p. 241°-243° C. The base was converted to the hydrochloride salt by reacting with ethereal hydrogen chloride and recrystallized from either hot water-isopropanol or methanol-methylethylketone (1:1) to yield a crystalline solid melting 280.5°-283.5° C. NMR, MS, and IR were satisfactory. MW 318.249.
Analysis: Calculated for Cl 2 N 3 OC 14 H 21 : C, 52.84; H, 6.65; N, 13.20. Found: C, 52.90; H, 6.54; N, 13.24.
EXAMPLE 16
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-pyridinecarboxamide Fumarate [1:1]
Tetrahydrofuran (50 ml) was added to a mixture of picolinic acid (2.46 g, 0.020 mole) and 1,1'-carbonyldiimidazole (3.24 g, 0.020 mole) and the mixture stirred in a closed system equipped with an oil bubbler until evolution of carbon dioxide ceased. Nitrogen was then bubbled through the reaction mixture to sweep out any remaining carbon dioxide. 3 Aminoquinuclidine (2.52 g, 0.020 mole) was added to the reaction mixture in one portion and the mixture heated at reflux temperature for 1 hr while continuing to saturate the mixture with nitrogen. After cooling, the mixture was concentrated to a brown oil containing the product, imidazole, and a small amount of 3-aminoquinuclidine. The oil was dissolved in methylene chloride (50 ml) and washed 3 times with 50 ml portions of water. The methylene chloride solution was dried over anhydrous magnesium sulfate and concentrated to an oil. The oil was dissolved in ether and filtered to remove a small quantity of insoluble material. The filtrate was concentrated to give 2.38 g free base (51.4%) which was redissolved in 100 ml ether and treated with a solution of fumaric acid (1.20 g) in 50 ml methanol and the mixture triturated to induce crystallization. The solid salt was collected under nitrogen to yield 3.14 g of white solid. TLC analysis (3% conc. ammonium hydroxide solution in methanol) showed only a trace of impurity.
Mass spectrum (EI)-m/e (% relative intensity): 231 (19), 161 (16), 125 (22), 109 (80), 106 (28), 98 (24), 96 (29), 79 (29), 78 (73), 70 (100), 45 (22), 42 (45), and 41 (20).
Analysis: Calculated for C 17 H 21 N 3 O 5 : C, 58.78; H, 6.09; N, 12.10. Found: C, 58.58; H, 6.10; N, 12.04.
EXAMPLE 17
N-(1-Azabicyclo[2.2.2]oct-3-yl)benzamide, Fumarate [1:1]
In a closed system equipped with an oil bubbler, a solution of benzoyl chloride (3.51 g, 0.020 mole) in 100 ml absolute ether was added dropwise over 10 min to a stirred solution of 3-amino-quinuclidine (2.52 g, 0.020 mole) in 100 ml absolute ether. After the addition was completed, the mixture was stirred an additional 1.5 hr, and the solid hydrochloride salt was filtered under nitrogen. The salt was dissolved in methanol and treated with a solution of sodium methoxide prepared from 0.58 g sodium metal (0.025 ml) in 20 ml methanol. The mixture was concentrated and the residual material triturated with methylene chloride (50 ml), filtered, and the filtrate concentrated to give a yellow solid. The solid was triturated with a small amount of acetone and then with 50 ml boiling toluene. The resulting solution was decanted away from some insoluble gummy material. Isooctane was added to the hot toluene solution until the solution was turbid. After standing overnight, the solid free base was collected (2.23 g). The filtrate was concentrated and the residual solid recrystallized from toluene-isooctane to yield an additional 0.35 g of the free base, m.p. 159°-160° C., total yield 2.58 g (56%). The free base was dissolved in 100 ml acetone and treated with a solution of fumaric acid (1.30 g, 0.0112 mole) in 30 ml methanol. The solution was concentrated to give a solid residue which was recrystallized from methanol-isopropyl ether to give 3.03 g of the product, m.p. 187°-190° C. Mass spectrum (E.I.) m/e (% relative intensity) 230 (14), 125 (16), 109 (76), 105 (90), 98 (23), 96 (21), 84 (17), 77 (69), 70 (100), 51 (23), 95 (25), 42 (42).
Analysis: Calculated for C 18 H 22 N 2 O 5 : C, 62.42; H, 6.40; N, 8.09. Found: C, 62.01; H, 6.46; N, 7.99.
EXAMPLE 18
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-furancarboxamide Hydrochloride
In a closed system equipped with an oil bubbler, a solution of 3-amino-quinuclidine (2.52 g, 0.020 mole) in 10 ml anhydrous ether was added dropwise to a stirred solution of furoyl chloride (3.26 g, 0.025 mole) in 100 ml anhydrous ether. After the addition was completed (5 min), the mixture was stirred an additional hour and the solid collected under nitrogen to give 4.73 g (73.7% yield) of the hydrochloride salt. TLC (3% concentrated ammonium hydroxide in methanol) showed a small amount of impurity which was not removed by recrystallization. The salt was dissolved in 20 ml of water, basified with 6N sodium hydroxide solution, and extracted three times with 20 ml portions of methylene chloride. The combined extract was dried over magnesium sulfate and concentrated to yield 2.37 g viscous yellow oil. The oil was dissolved in 20 ml methanol, treated with excess ethereal hydrogen chloride solution and diluted with 100 ml anhydrous ether. The salt crystallized on trituration and was collected under nitrogen to give 1.84 g off-white solid. This solid was recrystallized from methanol-isopropyl ether to give 1.63 g white solid, m.p. 249°-251° C. Mass spectrum (E.I.)-m/e (% relative intensity): 220 (19), 109 (74), 96 (29), 95 (100), 84 (14), 70 (83), 42 (52), 41 (20), 39 (47).
Analysis: Calculated for C 12 H 17 N 2 O 2 Cl: C, 56.14; H, 6.67; N, 10.91. Found: C, 56.06; H, 6.69; N, 10.77.
EXAMPLE 19
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-fluorobenzamide, Monohydrochloride
In a closed system, a solution of 3-aminoquinuclidine (2.52 g, 0.020 mole) in 10 ml anhydrous ether was added dropwise to a stirred solution of 2-fluorobenzoyl chloride (3.13 g, 0.020 mole) in 100 ml anhydrous ether. After the addition was complete, the mixture was stirred another hour and the solid product (as the hydrochloride salt) was collected by filtration under nitrogen to give 4.75 g (84%). TLC analysis (3% conc. ammonium hydroxide in methanol) showed the presence of 3-aminoquinuclidine. The salt was dissolved in 10 ml water, basified with 6N sodium hydroxide solution, and extracted three times with 50 ml portions of methylene chloride. The combined extract was dried over magnesium sulfate and concentrated to give 3.67 g of the product as the free base. Recrystallization from tolueneisooctane gave 2.33 g of a white solid (some toluene insoluble material was removed by decanting the hot toluene solution). The solid free base was dissolved in 10 ml methanol, treated with excess ethereal hydrogen chloride and 100 ml isopropyl ether was added. The salt separated from solution as an oil, but crystallized on trituration. The white solid was collected under nitrogen to give 2.60 g; m.p. 233°-234° C. Mass spectrum (E.I.) m/e (% relative intensity): 248 (15), 125 (13), 123 (100), 109 (80), 96 (24), 95 (45), 84 (14), 75 (19), 70 (64), 42 (44), 41 (18).
Analysis: Calculated for C 14 H 18 N 2 OFCl: C, 59.05; H, 6.37; N, 9.84. Found: C, 58.78; H, 6.40; N, 9.86.
EXAMPLE 20
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-thiophenecarboxamide Monohydrochloride
Tetrahydrofuran (30 ml) was added with stirring to a mixture of 2-thiophene carboxylic acid (2.56 g, 0.020 mole) and 1,1'-carbonyldiimidazole (3.24 g, 0.020 mole). When solution of carbon dioxide ceased, nitrogen was bubbled through the solution for 1 hr to free the solution of carbon dioxide. 3-Aminoquinuclidine (2.52 g, 0.020 mole) was added in one portion and the mixture heated to reflux temperature for one hour while continuing to saturate the reaction mixture with nitrogen. After cooling, the mixture was concentrated, the residual oil dissolved in 40 ml methylene chloride, and washed three times with 20 ml portions of water. The methylene chloride solution was dried over magnesium chloride and concentrated to yield 2.57 g (54.4%) gummy white material. The amide was dissolved in a methanol-ether mixture treated with ethereal hydrogen chloride and diluted with ether, causing the salt to separate an oil which crystallized on trituration. The salt was collected under nitrogen (2.22 g) and recyrstallized from methanol-isopropyl ether to give 1.81 g white crystalline solid, m.p. 245°-246° C. Mass spectrum (E.I.)-m/e (% relative intensity): 236 (17), 125 (19), 111 (100), 109 (65), 96 (23), 84 (18), 83 (24), 82 (17), 70 (84), 42 (45), 41 (20), 39 (43).
Analysis: Calculated for C 12 H 17 N 2 OSCl: C, 52.84; H, 6.28; N, 10.27. Found: C, 52.88; H, 6.34; N, 10.36.
EXAMPLE 21
N-(1-Azabicyclo[2.2.2]oct-3-yl)2,6-dimethoxybenzamide Monohydrochloride
In a closed system equipped with an oil bubbler, a solution of 2,6-dimethoxybenzoyl chloride (1.89 g, 0.0095 mole) in 20 ml diethyl ether was added dropwise to a stirred solution of 3-aminoquinuclidine (1.26 g, 0.010 mole) in 50 ml of diethyl ether. After the addition was completed, the reaction mixture was stirred for 15 min, and the precipitate that had formed was filtered under nitrogen. The wet (hygroscopic) solid was immediately recrystallized from methanol-isopropyl ether to give 1.85 g (60%) of the product. The material was vacuum dried for 4 hr at 98° C., m.p. 266°-268° C.
Analysis: Calculated for C 16 H 23 N 2 O 3 Cl: C, 58.80; H, 7.09; N, 8.57. Found: C, 58.44; H, 7.17; N, 8.51.
EXAMPLE 22
N-(1-Azabicyclo[2.2.2]oct-3-yl)-1H-indole-5-carboxamide
Tetrahydrofuran (50 ml) was added to a mixture of indole-5-carboxylic acid (2.42 g, 0.016 mole) and 1,1'-carbonyldiimidazole (2.43 g, 0.015 mole). The mixture was stirred for 1 hr while nitrogen was bubbled through the solution to remove the carbon dioxide that was evolved. Then 3-aminoquinuclidine (1.89 g, 0.015 mole) was added in one portion, and the mixture was stirred for 60 hr at room temperature. The solid product was collected by filtration to yield 3.75 g (86.8%). Recrystallization from methanol-isopropyl ether (with chilling) gave 1.89 g of the product as an off-white solid; m.p. 293°-295° C. The solid was vacuum dried at 82° C. for 16 hr, m.p. 293°-295° C.
Analysis: Calculated for C 16 H 19 N 3 O: C, 71.35; H, 7.11; N, 15.60. Found: C, 70.96; H, 7.15; N, 15.38.
EXAMPLE 23
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-methoxy-5-(methylsulfonyl)-benzamide, Monohydrochloride
A solution of 3-aminoquinuclidine (1.50 g, 0.0119 mole) in 20 ml of tetrahydrofuran was added dropwise to a stirred solution of 2-methoxy-5-methanesulfonylbenzoyl chloride (2.95 g, 0.0119 mole) in 100 ml tetrahydrofuran. The mixture was stirred at ambient temperature for 20 hr and filtered to yield 4.00 g (89.7%) of the product as the hydrochloride salt. The material was heated in 100 ml of boiling absolute ethanol and 50 ml methanol was added to give a clear solution. The solution was evaporated to a volume of 100 ml and cooled. The precipitate which formed was collected by filtration and vacuum dried at 110° C. for 8 hr; m.p. 219°-221° C.
Analysis: Calculated for C 16 H 23 N 2 O 4 SCl: C, 51.26; H, 6.18; N, 7.47. Found: C, 51.19; H, 6.6; N, 7.35.
EXAMPLE 24
N-(1-Azabicyclo[2.2.2]oct-3-yl)-5-bromo-2,4-dimethoxybenzamide Monohydrochloride
A solution of 3-aminoquinuclidine (1.12 g, 0.0089 mole) in 20 ml tetrahydrofuran was added dropwise to a stirred solution of 5-bromo-2,4-dimethoxybenzoyl chloride (2.50 g, 0.0089 mole) in 100 ml tetrahydrofuran. The mixture was stirred at ambient temperature for 65 hr, and the solid was collected by filtration to yield 2.77 g. Recrystallization from methanol-isopropyl ether gave 1.45 g (40.2%), m.p. 240°-243° C.
Analysis: Calculated for C 16 H 21 N 2 O 3 Br: C, 47.37; H, 5.47; N, 6.90. Found: C, 47.23; H, 5.62; N, 6.85.
EXAMPLE 25
N-(1-Azabicyclo[2.2.2]oct-3-yl)-3-methoxybenzamide, Monohydrochloride
In a closed system, a solution of 3-methoxybenzoyl chloride (7.18 g, 0.04206 mole) in 30 ml ether was added dropwise to a stirred solution of 3-aminoquinuclidine (5.30 g, 0.04206 mole) in 100 ml of ether. The reaction mixture was stirred at ambient temperature for 16 hr. The solid hydrochloride salt was collected under nitrogen and dried in vacuo at ambient temperature to give 11.12 g (87.1%) of the product. The material was recyrstallized from absolute ethanol-isopropyl ether to give 7.69 g. The product was vacuum dried for 20 hr over refluxing ethanol, and then for 24 hr over refluxing isooctane; m.p. 214°-215° C.
Analysis: Calculated for C 15 H 21 N 2 O 2 Cl: C, 60.70; H, 7.13; N, 9.44. Found: C, 60.45; H, 7.15; N, 9.40.
EXAMPLE 26
N-(1-Azabicyclo[2.2.2]oct-3-yl)-3-fluorobenzamide, Monohydrochloride
In a closed system, a solution of 3-fluorobenzyl chloride (7.93 g, 0.050 mole) in 30 ml ether was added dropwise to a stirred solution of 3-aminoquinuclidine (6.3 g, 0.050 mole) in 100 ml ether. After the addition was completed, the mixture was stirred at ambient temperature for 16 hr. The solid hydrochloride salt was collected under a nitrogen atmosphere and vacuum dried for 2 hr, to yield 13.11 g (92.1%). The salt was recrystallized from absolute ethanol-isopropyl ether to give 8.87 g of a white solid. The material was recrystallized from ethanol, and vacuum dried for 12 hr at 70° C., m.p. 257°-258° C.
Analysis: Calculated for C 14 H 18 N 2 OFCl: C, 59.05; H, 6.37; N, 9.84. Found: C, 59.05; H, 6.41; N, 9.80.
The preparations of certain compounds encompassed by Formula I and useful in the present invention listed in the following Example 27 a to n are demonstrated and illustrated by structure in U.S. Pat. No. 4,213,983.
EXAMPLE 27 (A)-(N)
(a) 4-Acetylamino-4-chloro-2-methoxy-N-(2-quinolizidinyl)benzamide. (Compound identified in Ex. 1 of U.S. Pat. No. 4,213,983).
(b) 4-Amino-5-chloro-2-methoxy-N-(2-quinolizidinyl)benzamide (Compound identified in Ex. 2 of U.S. Pat. No. 4,213,983).
(c) 4-Acetylamino-5-chloro-2-methoxy-N-(7-octahydroindolizidinyl)benzamide. (Compound identified in Ex. 3 of U.S. Pat. No. 4,213,983).
(d) 4-Amino-5-chloro-2-methoxy-N-(7-octahydroindolizidinyl)benzamide. (Compound identified in Ex. 4 of U.S. Pat. 4,213,983).
(e) 4-Acetylamino-5-chloro-2-methoxy-N-(3-quinolizidinyl)benzamide. (Compound identified in Ex. 5 of U.S. Pat. No. 4,213,983).
(f) 4-Amino-5-chloro-2-methoxy-N-(3-quinolizidinyl)benzamide. (Compound identified in Ex. 6 of U.S. Pat. No. 4,213,983).
(g) 4-Acetylamino-5-chloro-2-methoxy-N-(1-quinolizidinyl)benzamide. (Compound identified in Ex. 7 of U.S. Pat. No. 4,213,983).
(h) 4-Amino-5-chloro-2-methoxy-N-(1-quinolizidinyl)benzamide. (Compound identified in Ex. 8 of U.S. Pat. No. 4,213,983).
(i) 4-Acetylamino-5-chloro-2-methoxy-N-(2-pyrido[1,2-a]pyrazinyl)benzamide. (Compound identified in Ex. 11 of U.S. Pat. No. 4,213,983).
(j) 4-Acetylamino-5-chloro-2-methoxy-N-(2-octahydroindolizinyl)benzamide. (Compound identified in Ex. 13 of U.S. Pat. No. 4,213,983).
(k) 4-Amino-5-chloro-2-methoxy-N-(2-octahydroindolizinyl)benzamide. (Compound identified in Ex. 14 of U.S. Pat. No. 4,213,983).
(l)4-Acetylamino-4-chloro-2-methoxy-N-(6-methyl-2-quinolizidinyl)benzamide. (Compound identified in Ex. 15 of U.S. Pat. No. 4,213,983).
(m) 4-Amino-5-chloro-2-methoxy-N-(6-methyl-2-quinolizidinyl)benzamide. (Compound identified in Ex. 16 of U.S. Pat. No. 4,213,983). and, (n) 4-Amino-5-chloro-2-methoxy-N-(6-methyl-2-quinolizidinyl)benzamide. (Compound identified in Ex. 17 of U.S. Pat. No. 4,213,983).
The preparation of certain compounds encompassed by Formula I and useful in the present invention listed in the following Example 28 a to z and Example 29 a and b are demonstrated and illustrated by structure in European patent application publication No. 0067565A1 as follows:
EXAMPLE 28 (A)-(Z)
(a) 4-Amino-5-chloro-2-methoxy-N-[4'α,β-(1'-aza-2'-α-phenyl-6'-α-H-bicyclo[4,3,0]decyl)]benzamide (compound isentified in Example 5 of European Pat. No. 0067565).
(b) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9'β-methyl-1'-aza-5.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 6 of European Pat. No. 0067565).
(c) 4-Acetamido-5-chloro-2-methoxy-N-[7'α-(9'β-methyl-1'-aza-5'.alpha.-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 7 of European Pat. No. 0067565).
(d) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'β-methyl-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 8 of European Pat. No. 0067565).
(e) 4-Amino-5-chloro-2-methoxy-N-[7'α-(9'β-methyl-1'-aza-5'-α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 9 of European Pat. No. 0067565).
(f) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9''-methyl-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 10 of European Pat. No. 0067565).
(g) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'α-methyl-1'-aza-5α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 11 of European No. 0067565).
(h) 4-Acetamido-5-chloro-2-methoxy-N-[7'α-(9'-α-methyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 12 of European No. 0067565).
(i) 4-Amino-5-chloro-2-methoxy-N-[n'α-(7'-α-(9'-α-methyl-1'-aza-5α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 13 of European No. 0067565).
(j) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9',9'dimethyl)-1'-aza-5'.alpha.H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 14 of European No. 0067565).
(k) 4-Amino-5-chloro-2-methoxy-N-(7'β-(9,9'-dimethyl)-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 15 of European No. 0067565).
(l) 4-Acetamido-5-chloro-2-methoxy-N-[7'α-(9',9'-dimethyl-1'-aza-5'-.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 16 of European No. 0067565).
(m) 4-Amino-5-chloro-2-methoxy-N-[7'α-(9',9'-dimethyl)-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 17 of European No. 0067565).
(n) 4-Acetamido-5-chloro-2-methoxy-N-[7'β(9'-methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide, Isomer I (compound identified in Example 18 of European No. 0067565).
(o) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'-methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide monohydrochloride, Isomer I (compound identified in Example 19 of European No. 0067565).
(p) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9'-methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl]benzamide, Isomer 2 (compound identified in Example 20 of European No. 0067565).
(q) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide, Isomer 2 (compound identified in Example 21 of European No. 0067565).
(r) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9'-methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide, Isomer 3 (compound identified in Example 22 of European No. 0067565).
(s) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'-methyl-3'-phenyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl]benzamide, Isomer 3 (compound identified in Example 23 of European No. 0067565).
(t) 4-Amino-5-chloro-2-methoxy-N-[4'β-(7'β-methyl-1'-aza-6'α-H-bicyclo[4,4,0]decyl)]benzamide (compound identified in Example 25 of European No. 0067565).
(u) 4-Acetamido-5-chloro-2-methoxy-N-[4'α-(7'β-methyl-1'aza-6'.alpha.-H-bicyclo[4,4,0]decyl)]benzamide with 10% 4'β isomer (mixture identified in Example 26 of European No. 0067565.
(v) 4-Amino-5-chloro-2-methoxy-N-[4'α-(7'β-methyl-1'-aza-6'α-H-bicyclo[4,4,0]decyl)]benzamide with 10% 4'β-isomer (mixture identified in Example 27 of European No. 0067565).
(w) 4-Acetamido-5-chloro-2-methoxy-N-[4'β-(7'β-(7'α-methyl-1'-aza-6'α-H-bicyclo[4,4,0]decyl)]benzamide (compound identified in Example 28 of European No. 0067565).
(x) 4-Amino-5-chloro-2-methoxy-N-[4'β-(7'α-methyl-1'-aza-6'α-H-bicyclo[4,4,0]decyl]benzamide (compound identified in Example 29 of European No. 0067565).
(y) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(5'α-methyl-1'-aza-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 30 of European No. 0067565).
(z) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9'α-ethyl-1'-aza-5'-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 32 of European No. 0067565).
EXAMPLE 29(a)-(b)
(a) 4-Amino-5-chloro-2-methoxy-N-[7'β-(9'α-ethyl-1'-aza-5'α-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 33 of European No. 0067565).
(b) 4-Acetamido-5-chloro-2-methoxy-N-[7'β-(9'α-isopropyl-1'-aza-5'.alpha.-H-bicyclo[4,3,0]nonyl)]benzamide (compound identified in Example 34 of European No. 0067565).
EXAMPLE 30
N-(1-Azabicyclo[2.2.2]oct-3-yl)-6-methoxy-1H-benzotriazole-5-carboxamide
Following the procedure of Example 22, 6-methoxy-1H-benzotriazole-5-carboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
EXAMPLE 31
N-(1-Azabicyclo[2.2.2]oct-3-yl)-6-methoxy-1H-indole-5-carboxamide
Following the procedure of Example 22, indole-6-methoxy-5-carboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
EXAMPLE 32
N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-(dimethylamino)-4-methoxy-5-pyrimidinecarboxamide
Following the procedure of Example 22, 2-(dimethylamino)-4-methoxy-5-pyrimidinecarboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
EXAMPLE 33
N-(1-Azabicyclo[2.2.2]oct-3-yl)-4-methoxy-2-(methylamino)-5-pyrimidinecarboxamide
Following the procedure of Example 22, 4-methoxy-2-(methylamino)-5-pyrimidinecarboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
EXAMPLE 34
2-Amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-4-methoxy-5-pyrimidinecarboxamide
Following the procedure of Example 22, 2-amino-4-methoxy-5-pyrimidinecarboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
EXAMPLE 35
N-(1-Azabicyclo[2.2.2]oct-3-yl)-1,3-benzodioxole-5-carboxamide
Following the procedure of Example 22, 1,3-benzodioxole-5-carboxylic acid, 1,1'-carbonyldiimidazole and 3-aminoquinuclidine are reacted to give the title compound.
Pharmacological Testing
(Mice)
The test relied upon to indicate effectiveness of the compounds in the method of this invention as follows involves a passive avoidance procedure which is the type of procedure most often used to evaluate compounds for their effect on memory and learning.
There are three phases to the behavioral procedure: adaptation, training and testing. Following 24 hrs of water deprivation, the mice are given an adaptation session during which they are allowed to freely explore the chamber and learn the location of the drinking spout. The session is terminated when the animals have completed 5 seconds of drinking. The mice are then given free access to water for 1.5 hrs in their home cages. During the training session, 24 hrs later, the mice are permitted 5 seconds access to the drinking tube after which time the shock circuit is automatically activated and all subsequent contracts with the tube are punished. The training session is terminated when the mice either fail to touch the tube for a 60 seconds period or receive the maximum number of shocks (5). The latency to complete the initial 5 seconds of drinking, as well as the number of shocks each animal receives is recorded. The animals are then returned to their home cages and given free access to water for the next 24 hrs.
Retention is tested 48 hrs later by once again placing the mice into the lick-suppression chamber and recording the time it takes each animal to complete the 5 seconds of drinking from the water spout. Mice failing to complete the 5 seconds of drinking within 2000 seconds are removed from the apparatus and assigned a maximum test latency score of 2000. Test compound or saline are given 30 minutes prior to the retention task.
As indicated in Table 1, the compound of Example 2; namely, 4-amino-N-(1-azabicyclo[2.2.2]oct-3-yl)-5-chloro-2-methoxybenzamide hydrochloride hydrate[1:1:1], significantly increases the time required to complete the drinking task. This increased latency is a measure of memory improvement in the trained animals.
It should be noted that the increased latency is not due to a general debilitation of the animals since untrained animals treated with the same doses of the compound of Example 2 do not show a similar delayed latency to drinking.
TABLE 1______________________________________Effects on Memory in Mice Dose Latency to Complete 5 sec.Compound (mg/kg, i.p.) of Drinking (.sup.-- X ± SE) pH______________________________________Saline 0 413 ± 69 --Example 2 56 511 ± 193 nsExample 2 75 354 ± 88 nsExample 2 100 1182 ± 222 p 0.02Example 2 130 1347 ± 160 p 0.002______________________________________
Pharmaceutical Compositions
The pharmaceutical compositions used in the method of this invention for administration to animals and humans are comprised of, as active ingredients, at least one of the compounds of Formula I, according to the invention, in association with a pharmaceutical carrier or excipient. The compounds are thus presented in a therapeutic composition for oral, parenteral, subcutaneous, intramuscular, intraperitoneal, intravenous, or rectal administration. Thus, for example, compositions for oral administration can take the form of elixirs, capsules, tablets, or coated tablets containing carriers conveniently used in the pharmaceutical art. Suitable tableting excipients include lactose, potato and maize starches, talc, gelatin, stearic and silicic acids, magnesium stearate and polyvinyl pyrrolidones.
For parenteral administration, the carrier or excipient can be comprised of a sterile parenterally acceptable liquid; e.g., water or arachis oil contained in ampoules.
In compositions for rectal administration, the carrier can be comprised of a suppository base; e.g., cocoa butter or a glyceride.
Advantageously, the compositions are formulated as dosage units, each unit being adapted to supply a fixed dose of active ingredients. Tablets, coated tablets, capsules, ampoules and suppositories are examples of preferred dosage forms according to the invention. It is only necessary that the active ingredient constitute an effective amount; i.e., such that a suitable effective dosage will be consistent with the dosage form employed in single or multiple unit doses. The exact individual dosages, as well as daily dosages, will of course be determined according to standard medical principles under the direction of a physician or veterinarian. Generally, the pharmacology tests on mice suggest an effective dose for a small animal will be in the range of about 75-130 mg/kg of body weight for a compound such as that of Example 2. Generally, for humans, in the absence of actual testing the amount projected to be required appears to be about 10-100 mg/kg of body weight to produce memory enhancement in humans; for example, in impaired memory of the elderly.
Based on the foregoing projection for effective dosages for humans, daily dosages of about 2 to 4 times the effective dose appear to be reasonable for a total daily dosage range of 20-400 mg/kg of body weight. Obviously, the effective dosage amount may be administered by a variety of unit dosage sizes. The scope of the invention in relation to human dosage is not to be limited by the foregoing projections due to uncertainty in transposing from animal data to human dosages. | A pharmaceutical method for improving memory or correcting memory deficiency is disclosed, utilizing compounds having the formula: ##STR1## wherein n 1 , n 2 , n 3 , and n 4 =0 to 3; R 1 , R 2 , R 3 , and R 4 =H, loweralkyl or phenyl; R 5 =H or loweralkyl; X=O or S; Ar=phenyl, substituted phenyl, pyridinyl, furanyl, thienyl, methoxy-1H-benzotriazolyl, indolinyl, methoxyindolinyl, methoxypyrimidinyl, amino-methoxypyrimadinyl, 1,3-benzodioxolyl, or naphthalenyl, and the pharmaceutically acceptable acid addition salts, hydrates and alcoholates thereof. | 0 |
BACKGROUND OF THE INVENTION
Trauma to the brain or spinal cord caused by physical forces acting on the skull or spinal column, by ischemic stroke, arrested breathing, cardiac arrest, Reye's syndrome, cerebral thrombosis, cerebral embolism, cerebral hemorrhage, encephalomyelitis, hydrocephalus, post-operative brain injury, cerebral infections, AIDS virus, various concussions and elevated intracranial pressure results in edema and swelling of the affected tissues. This is followed by ischemia, hypoxia, necrosis, temporary or permanent brain and/or spinal cord injury and may result in death. The tissue mainly affected are classified as grey matter, more specifically astroglial cells. The specific therapy currently used for the treatment of the medical problems described include various kinds of diuretics (particularly osmotic diuretics), steroids (such as, 6-α-methylprednisolone succinate) and barbiturates. The usefulness of these agents is questionable and they are associated with a variety of untoward complications and side effects. Thus, the compounds of this invention comprise a novel and specific treatment of medical problems where no specific therapy is available.
Two recent publications, one entitled "Agents for the Treatment of Brain Injury" 1. (Aryloxy)alkanoic Acids, by Cragoe et al, J. Med. Chem., (1982) 25, 567-579 and the other, "Agents for the Treatment of Brain Edema 2. [(2,3,9,9a-tetra-hydro-3-oxo-9a-substituted-1H-fluoren-7-yl)-oxy]alkanoic Acids and Their Analogs", by Cragoe et al, J. Med. Chem., 29, 825-841 (1986), report recent experimental testing of agents for treatment of brain injury and review the current status of treatment of brain injury. Additionally, U.S. Pat. Nos. 4,316,043, 4,317,922, 4,337,354, 4,356,313, 4,356,314, 4,389,417, 4,394,385, 4,463,208, 4,465,850, 4,579,869, and 4,604,396 disclose certain alkanoic acids, cycloalkanoic acids or their amidine analogs for the treatment of grey matter edema.
The compounds of the invention have the added advantage of being devoid of the pharmacodynamic, toxic or various side effects characteristic of the diuretics, steroids and barbiturates.
DESCRIPTION OF THE INVENTION
The compounds of the instant invention are best characterized by reference to the following structural Formula (I): ##STR1## wherein:
R is ##STR2##
R 1 is hydrogen, C 1 -C 6 alkyl, C 1 -C 6 carboxyalkyl;
R 2 is NH 2 , NHR 4 or NR 4 R 5 ;
R 3 is NH 5 or NR 5 ;
R 4 and R 5 are each independently lower alkyl, branched or unbranched, containing from 1 to 5 carbon atoms, or amino, provided that R 4 and R 5 are not both amino;
wherein R 2 and R 3 may be joined together via R 4 to form a heterocyclic ring of 5 or 6 atoms containing 2 nitrogen atoms and 3 or 4 carbon atoms, such as ##STR3## or wherein R 4 and R 5 may be joined together to form a 5- or 6-membered ring containing one nitrogen atom and 4 or 5 carbon atoms, such as: ##STR4##
R 6 is lower alkyl, branched or unbranched, containing from 1 to 5 carbon atoms such as methyl, ethyl, n-propyl, isopropyl and the like, aryl such as phenyl, halo substituted aryl such as p-fluorophenyl, o-fluorophenyl, p-chlorophenyl and the like, aralkyl such as benzyl, cycloalkyl containing from 3 to 6 nuclear carbon atoms such as cyclopropyl, cyclobutyl, cyclopenyl and the like, or cycloalkyl-lower alkyl containing from 4 to 7 total carbon atoms such as cyclopentylmethyl.
X and Y are halo or lower alkyl, such as methyl; and x is 1 to 4.
Since the 5a-carbon atom in the molecule is asymmetric, the compounds of the invention are racemic. However, these compounds or their precursors can be resolved so that the pure enantiomers can be prepared, thus the invention includes the pure enantiomers. This is an important point since some of the racemates consist of one enantiomer which is much more active than the other one. Furthermore, the less active enantiomer generally possesses the same intrinsic toxicity as the more active enantiomer. In addition, it can be demonstrated that the less active enantiomer depresses the inhibitory action of the active enantiomer at the tissue level. Thus, for three reasons it is advantageous to use the pure, more active enantiomer rather than the racemate.
Since the ethaneimidamide products of the invention are basic, the invention also includes the obvious pharmaceutically acceptable acid addition salts such as the hydrochloride, hydrobromide, sulfate, isethionate, acetate, methanesulfonate, maleate, succinate and the like salts.
Likewise, since the alkanoic acid products of the invention are acidic, the invention also includes the obvious pharmaceutically acceptable salts such as the sodium, potassium, ammonium, trimethylammonium, piperazinium, 1-methylpiperazinium, guanidinium, bis-(2-hydroxyethyl)ammonium, N-methyl-glucosammonium and the like salts.
It is also to be noted that the compounds of Formula I, as well as their salts, often form solvates with the solvents in which they are prepared or from which they are recrystallized. These solvates may be used per se or they may be desolvated by heating (e.g. at 70° C.) in vacuo.
Although the invention primarily involves novel (1,2-dichloro-8-oxo-5a-substituted-5a,6,7,8-tetrahydrodibenzofuran-3-yl)alkanoic acids and alkanimidamides, and their salts, it also includes their derivatives, such as oximes, hydrazones, esters and the like. Additionally, this invention includes pharmaceutical compositions in unit dosage form containing a pharmaceutical carrier and an effective amount of a compound of Formula I, its R or S enantiomer, or the pharmaceutically acceptable salts thereof, for treating brain injury. The method of treating a person with brain injury by administering said compounds or said pharmaceutical compositions is also a part of this invention.
PREFERRED EMBODIMENT OF THE INVENTION
The preferred embodiments of the instant invention are realized in structural Formula II ##STR5## wherein: R is carboxy, ##STR6##
R 7 is lower alkyl, branched or unbranched, containing from 1 to 5 carbon atoms.
A preferred compound is [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid.
Also preferred is 1-carboxy-1-methylethyl [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetate.
Also preferred is 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimidamide hydrochloride.
Especially preferred are the pure enantiomers since, in most instances, one enantiomer is more active biologically then its antipode.
Included within the scope of this invention are the pharmaceutically acceptable salts of (1,2-dichloro-8-oxo-5a-substituted-5a,6,7,8-tetrahydrodibenzofuran-3-yl) alkanoic acids and alkanimidamides since a major medical use of these compounds is solutions of their soluble salts which can be administered parenterally.
Thus, the acid addition salts can be prepared by the reaction of the (1,2-dichloro-8-oxo-5a-substituted-5a,6,7,8-tetrahydrodibenzofuran-3-yl)alkanoic acids of this invention with an appropriate alkali metal hydroxide, carbonate or bicarbonate such as sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and the like or an organic base, such as ammonium hydroxide, piperazine, 1-methylpiperazine, guanidine, bis-(2-hydroxyethyl)amine, N-methylglucosamine and the like salts of the alkanimidamides of this invention may be prepared by reaction with an appropriate pharmaceutically acceptable mineral acid or organic carboxylic acid, such as hydrochloric acid, sulfuric acid, hydrobromic acid, isethionic acid, methanesulfonic acid, maleic acid, succinic acid, acetic acid and the like. The salts selected are derived from among the non-toxic, pharmaceutically acceptable acids.
The synthesis of the compounds of this invention in which R═COOH and x=1 (Ia) is illustrated by the following nine-step series of reactions to produce IIa wherein R═COOH, X=1, and R 7 =propyl. ##STR7##
The phenol of Formula III is reacted with benzyl bromide in the presence of a base, such as potassium carbonate using a solvent, such as N,N-dimethylformamide. The reaction is completed by stirring and heating at 40°-80° C. for 1 to 6 hours. Methoxylation of the compound of Formula IV to the anisole of Formula V occurs by heating with sodium methoxide in a solvent like hexamethylphosphoramide. The reaction requires stirring and heating at 80° to 120° C. for 15-25 hours. Cleavage of the benzyl moiety of the compound of Formula V to give the compound of Formula VI results by reaction with hydrogen in the presence of a catalyst, such as 5% palladium on carbon.
The reaction requires shaking in a hydrogen atmosphere at 20 to 30 p.s.i at a temperature of 20-30° C. for 2-5 hours.
Treatment of the compound of Formula VI with ethyl 2-bromopentanoate in N,N-dimethylformamide at 50° to 75° C. for 30 minutes to 2 hours produces the ethyl ester corresponding to Formula VII. Hydrolysis of this ester in aqueous sodium hydroxide and N,N-dimethylformamide by heating and stirring at 80°-100° C. for 3 to 6 hours produces the compound of Formula VII upon acidification. Annulation of the compound VII to form compound VIII is accomplished by first converting the compound of Formula VII to the corresponding acid chloride. This is accomplished by reaction with thionyl chloride in benzene at reflux for about one hour. The annulation to compound VIII is then effected by treatment of the acid chloride with aluminum chloride under Friedel Crafts reaction conditions. The reaction is conducted in methylene chloride, adding the aluminum chloride at 0°-10° C. followed by stirring at 20°-30° C. for 15-20 hours and finally refluxing the mixture for 15 minutes to 2 hours.
Reaction of the compound of Formula VIII with methyl vinyl ketone in tetrahydrofuran occurs by heating at 50°-60° C. in the presence of a catalyst, such as 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) or 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) produces the 2-(3-oxobutyl) derivative (Formula IX). This compound is cyclized by heating in aqueous ethanol containing a catalytic quantity of a strong base such as sodium hydroxide or potassium hydroxide to produce the compound of Formula X.
Cleavage of the methyl ether moiety of the compound of Formula X to form the corresponding phenol of Formula XI is accomplished by heating with molten pyridine hydrochloride at 175° to 195° C. for 15 to 30 minutes. Alternatively, one may use sodium nitrite in N,N-dimethylformamide at 130°-150° C. for 18 to 30 hours.
Reaction of the compound of Formula XI with ethyl bromoacetate in N,N-dimethylformamide at 50°-75° C. for 1 to 3 hours in the presence of a base such as potassium or sodium carbonate produces the ethyl ester corresponding to the compound of Formula IIa. Saponification of this ester is accomplished by heating in aqueous methanolic base such as sodium or potassium hydroxide. The reaction occurs at a temperature of 15° to 50° C. for 15 minutes to 5 hours. The compound of Formula IIa is generated by acidification of the reaction mixture with an acid such as hydrochloric or sulfuric acid.
It is to be recognized that these compounds of Formula I possess an asymmetric carbon atom at position 5a and, therefore, consist of racemates composed of two enantiomers. The resolution of the two enantiomers where R═COOH (Ia) may be accomplished by forming a salt of the racemic mixture with an optically active base such as (+) or (-) amphetamine, (-) cinchonidine, dehydroabietylamine, (+) or (-)-α-methylbenzylamine, (+) or (-)-α-(1-naphthyl)ethylamine, (+) cinchonine, brucine or strychnine and the like in a suitable solvent such as methanol, ethanol, 2-propanol, benzene, acetonitrile, nitromethane, acetone and the like. There is formed in the solution two diastereomeric salts, one of which is usually less soluble in the solvent than the other. Repetitive recrystallization of the crystalline salt generally affords a pure diastereomeric salt from which is obtained the desired pure enantiomer. The optically pure enantiomer is obtained by acidification of the salt with a mineral acid, isolation by filtration and recrystallization of the optically pure antipode.
The other optically pure antipode may generally be obtained by using a different base to form the diastereomeric salt. It is of advantage to isolate the partially resolved acid from the filtrates of the purification of the first diastereomeric salt and to further purify this substance through the use of another optically active base. It is especially advantageous to use an optically active base for the isolation of the second enantiomer which is the antipode of the base used for the isolation of the first enantiomer. For example, if (+)-α-methylbenzylamine was used first, then (-)-α-methylbenzylamine is used for the isolation of the second (remaining) enantiomer.
Since the products of Formulas Ia and IIa of the invention are acidic, the invention also includes the obvious pharmaceutically acceptable salts, such as the sodium, potassium, ammonium, trimethylammonium, piperazinium, 1-methylpiperazinium, guanidinium, bis-(2-hydroxethyl)ammonium, N-methylglucosammonium and the like salts.
The synthesis of the alkanimidamides of Formula I can be illustrated by the synthesis of IIb wherein ##STR8## x=1, and R 6 =propyl which is prepared following two-step reaction ##STR9##
The phenol of Formula XI is reacted with chloroacetonitrile in a base, such as potassium or sodium carbonate and a solvent such as N,N-dimethylformamide. The reaction mixture is heated at 55°-75° C. for 1-5 hours. Treatment of the nitrile of Formula XII with methanol containing a catalytic amount of base, such as sodium or potassium methoxide produces the corresponding imido ester which upon reaction with ammonium chloride produces the compound of Formula IIb.
The pure enantiomers of Formula Ib are conveniently prepared from the pure enantiomer of Formula Ia which in turn are converted to the pure enantiomeric phenols (XI), nitriles (XII) and alkanimidamides (Ib). This is illustrated by the series of reactions to produce IIb-R and IIb-S from Ia-R and Ib-S: ##STR10##
The acid addition salts of Formula Ib or IIb are formed by at least one of two methods. (1) The salt of ammonia or amine used in the reaction of the imido ester generated from the compound of Formula XII determines the salt of Formula Ib or IIb. (2) The salt of Formula Ib or IIb can be converted to the free base by treatment with aqueous base, such as sodium or potassium hydroxide) and the free base treated with a pharmaceutically acceptable acid, for example mineral acids, carboxylic acids or other organic acids, such as hydrochloric acid, sulfuric acid, isethionic acid, methanesulfonic acid, tartaric acid, succinic acid, maleic acid, acetic acid and the like.
The reaction may be conducted in water but it is preferred to conduct the reaction in an organic solvent, such as ether, ethanol, N,N-dimethylformamide and the like.
The preferred salts are the pharmaceutically acceptable salts such as the hydrochloride salts and the like.
Inasmuch as there are a variety of symptoms and severity associated with grey matter edema, particularly when it is caused by head trauma, stroke, cerebral hemorrhage or embolism, post-operative brain surgery trauma, spinal cord injury, cerebral infections, various brain concussions and elevated intracranial pressure, the precise treatment is left to the practioner. Generally, candidates for treatment will be indicated by the results of the patient's initial general neurological status, findings on specific clinical brain stem functions and findings on computerized axial tomography (CAT), nuclear magnetic resonance (NMR) or position emission tomography (PET) scans of the brain. The sum of the neurological evaluation is presented in the Glascow Coma Score or similar scoring system. Such a scoring system is often valuable in selecting the patients who are candidates for therapy of this kind.
The compounds of this invention can be administered by a variety of established methods, including intravenously, intramuscularly, subcutaneously, or orally. The parenteral route, particularly the intravenous route of administration, is preferred, especially for the very ill and comatose patient. Another advantage of the intravenous route of administration is the speed with which therapeutic brain levels of the drug are achieved. It is of paramount importance in brain injury of the type described to initiate therapy as rapidly as possible and to maintain it through the critical time periods. For this purpose, the intravenous administration of drugs of the type of Formula I in the form of their salts is superior.
A recommended dosage range for treatment is expected to be from 0.05 mg/kg to 20 mg/kg of body weight as a single dose, preferably from 0.2 mg/kg to 10 mg/kg. An alternative to the single dose schedule is to administer a primary loading dose followed by a sustaining dose of half to equal the primary dose, every 4 to 24 hours. When this multiple dose schedule is used the dosage range may be higher than that of the single dose method. Another alternative is to administer an ascending dose sequence of an initial dose followed by a sustaining dose of 1.5 to 2 times the initial dose every 4 to 24 hours. For example, 3 intravenous doses of 4, 6 and 8 mg/kg of body weight can be given at 6 hour intervals. If necessary, 4 additional doses of 8 mg/kg of body weight can be given at 12 hour intervals. Another effective dose regimen consists of a continuous intravenous infusion of from 0.05 mg/kg/hr to 3.0 mg/kg/hr. Of course, other dosing schedules and amounts are possible.
One aspect of this invention is the treatment of persons with grey matter edema by concomitant administration of a compound of Formula I or its salts, and an antiinflammatory steroid. These steroids are of some, albeit limited, use in control of white matter edema associated with ischemic stroke and head injury. Steroid therapy is given according to established practice as a supplement to the compound of Formula I as taught elsewhere herein. Similarly, a barbiturate may be administered as a supplement to treatment with a compound of Formula I.
The compounds of Formula I are utilized by formulating them in a pharmaceutical composition such as tablet, capsule or elixir for oral administration. Sterile solutions or suspensions can be used for parenteral administration. A compound or mixture of compounds of Formula I, or its physiologically acceptable salt, is compounded with a physiologically acceptable vehicle, carrier, excipient, binder, preservative, stabilizer, flavor, etc. in a dosage form as called for by accepted pharmaceutical practice.
Illustrative of the adjuvants which may be incorporated in tablets, capsules and the like are 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; a sweetening agent such as sucrose, lactose, or saccharin; a flavoring agent such as peppermint, oil of wintergreen or cherry. 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 enhanc the pharmaceutical elegance of the preparation. For instance, tablets may be coated with shellac, sugar or the like. A syrup or elixir may contain the active compound, sucrose as a sweetening agent, methyl and propyl parabens as preservatives, a dye and a flavoring such as cherry or orange flavor.
Sterile compositions for injection or infusion can be formulated according to conventional pharmaceutical practice by dissolving the active substance in a conventional vehicle such as water, saline or dextrose solution by forming a soluble salt in water using an appropriate acid, such as a pharmaceutically acceptable carboxylic acids or mineral acids. Alternatively, a suspension of the active substance in a naturally occurring vegetable oil like sesame oil, coconut oil, peanut oil, cottonseed oil, etc., or a synthetic fatty vehicle like ethyl oleate or the like may be formulated for injection or infusion. Buffer, preservatives, antioxidants and the like can be incorporated as required.
The basic premise for the development of agents for the treatment of brain injury of the types described is based on the studies in experimental head injury by R. S. Bourke et. al. (R. S. Bourke, M. A. Daze and H. K. Kimelberg, Monograph of the International Glial Cell symposium, Leige, Bel. August 29-31, 1977 and references cited therein) and experimental stroke by J. H. Garcia et. al. (J. H. Garcia, H. Kalimo, Y. Kamijyo and B. F. Trump, Virchows Archiv. [Zellopath.], 25, 191 (1977).
These and other studies have shown that the primary site of traumatic brain injury is in the grey matter where the process follows a pattern of insult, edema, ischemia, hypoxia, neuronal death and necrosis followed, in many instances, by irreversible coma or death. The discovery of a drug that specifically prevents the edema would obviate the sequalae.
Experimental head injury has been shown to produce a pathophysiological response primarily involving swelling of astroglial as a secondary, inhibitable process. At the molecular level, the sequence appears to be: trauma, elevation of extracellular K + and/or release of neurotransmitters, edema, hypoxia and necrosis. Astroglial swelling results directly from a K + -dependent, cation-coupled, chloride transport from the extracellular into the intracellular compartment with a concommitant movement of an osmotic equivalent of water. Thus, an agent that specifically blocks chloride transport in the astroglia is expected to block the edema caused by trauma and other insults to the brain. It is also important that such chloride transport inhibitors be free or relatively free of side effects, particularly those characteristics of many chloride transport inhibitors, such as diuretic properties. Compounds of the type illustrated by Formula I exhibit the desired effects on brain edema and are relatively free of renal effects.
That this approach is valid has been demonstrated by the correlation of the in vitro astroglial edema inhibiting effects of chloride transport inhibitors with their ability to reduce the mortality of animals receiving experimental in vivo head injury. As a final proof, one compound (ethacrynic acid) which exhibited activity both in vitro and in vivo assays was effective in reducing mortality in clinical cases of head injury. These studies are described in the Journal of Medicinal Chemistry, Volume 25, page 567 (1982), which is hereby incorporated by reference.
Three major biological assays can be used to demonstrate biological activity of the compounds. The (1) in vitro cat cerebrocortical tissue slice assay, (2) the in vitro primary rat astrocyte culture assay and (3) the in vivo cat head injury assay. The first assay, the in vitro cat cerebrocortical tissue slice assay has been described by Marshall, L. F.; Shapiro, H. M.; Smith, R. W. In "Seminars in Neurological Surgery: Neural Trauma"; Popp, A. J.; Bourke, R. S.; Nelson, L. R. ; Kimelberg, H, K,. Eds.; Raven Press: New York, 1979; p. 347, by Bourke, R. S.; Kimelberg, H, K.; Daze, M. A. in Brain Res. 1978, 154, 196, and by Bourke, R. S.; Kimelberg, H. K,; Nelson, L. R. in Brain Res. 1976, 105, 309. This method constitutes a rapid and accurate method of determining the intrinsic chloride inhibitory properties of the compounds of the invention in the target tissue.
The second assay method involves the in vitro primary rat astrocyte assay. The method has been described by Kimelberg, H. K.; Biddlecome, S.; Bourke, R. S. in Brain Res. 1979, 173, 111, by Kimelberg, H. K.; Bowman, c.; Biddlecome, S.; Bourke, R. S., in Brain Res. 1979, 177, 533, and by Kimelberg, H. K.; Hirata, H. in Soc. Neurosci. Abstr. 1981, 7, 698. This method is used to confirm the chloride transport inhibiting properties of the compounds in the pure target cells, the astrocytes.
The third assay method, the in vivo cat head injury assay has been described by Nelson, L. R.; Bourke, R. S.; Popp, A. J.; Cragoe, E. J. Jr.; Signorelli, A.; Foster, V. V.; Creel, in Marshall, L. F.; Shapiro, H. M.; Smith, R. W. In "Seminars in Neurological Surgery: Neural Trauma"; Popp, A. J.; Bourke, R. S.; Nelson, L. R.; Kimelberg, H. K., Eds.; Raven Press: New York, 1979; p. 297.
This assay consists of a highly relevant brain injury in cats which is achieved by the delivery of rapid repetitive acceleration-deceleration impulses to the animal's head followed by exposure of the animals to a period of hypoxia. The experimental conditions of the assay can be adjusted so that the mortality of the control animals falls in the range of about 25 to 75%. Then, the effect of the administration of compounds of this invention in reducing the mortality over that of the control animals in concurrent experiments can be demonstrated.
Using the in vitro cat cerebrocortical tissue slice assay, described in Example 1, compounds of the present invention can be tested for activity. This test provides the principal in vitro evaluation and consists of a determination of concentration vs. response curve. The addition of HCO 3 - to isotonic, K + -rich saline-glucose incubation media is known to specifically stimulate the transport of Cl - coupled with Na + and an osmotic equivalent of water in incubating slices of mammalian cerebral cortex. Experiments have demonstrated that the tissue locus of swelling is an expanded astroglial compartment. Thus, the addition of HCO 3 - to incubation media stimulates statistically significant and comparable increases in cerebrocortical tissue swelling and ion levels. After addition of drug to the incubation media, detailed drug concentration-response curves are then obtained. The data are expressed as percent HCO 3 - -stimulated swelling vs. drug concentration, from which the concentration of drug providing 50% inhibition of HCO 3 - -stimulated swelling (I 50 in molarity) is interpolated.
The following examples are included to illustrate the in vitro cerebrocortical tissue slice assay, the preparation of representative compounds of Formula I and representative dosage forms of these compounds. It is intended that the specification and examples be considered as exemplary only, with the true scope and spirit of the invention being indicated by the following claims. All temperatures in the examples are in Centigrade unless otherwise indicated.
EXAMPLE 1
In Vitro Cerebrocortical Tissue Slice Assay
Adult cats of 2-3 kg body weight are employed in tissue slice studies. Prior to sacrifice, the animals are anesthetized with ketamine hydrochloride (Ketaset), 10 mg/kg intramuscularly. Eight (three control, five experimental) pial surface cerebrocortical tissue slices (0.5-mm thick; approximately 150 mg initial fresh weight) are cut successively with a calibrated Stadie-Riggs fresh tissue microtome without moistening and weighed successively on a torsion balance. During the slice preparation all operations except weighing are PG,24 confined to a humid chamber. Each slice is rapidly placed in an individual Warburg flask containing 2 ml of incubation medium at room temperature. The basic composition of the incubation media, in millimoles per liter, is as follows: glucose, 10; CaCl 2 , 1.3; MgSO 4 , 1.2; KHSO 4 , 1.2; Hepes (N-2-hydroxyethylpiperazine-N'-2-ethanesulfonic acid, titrated with NaOH to pH 7.4), 20. Except when adding HCO 3 - , the osmolarity of the media is maintained isosmotic (approximately 285 mOsm/L) by reciprocal changes of Na + or K + to achieve a concentration of K + of 27 mM. The basic medium was saturated with oxygen by bubbling pure oxygen through the solution for 30 minutes before use. When added, NaHCO 3 or triethylammonium bicarbonate (TEAB) is initially present in the sidearm of each flask at an initial concentration of 50 mM in 0.5 ml of complete medium. Nonbicarbonate control slices are incubated at 37° C. in 2.5 ml of basic medium for 60 minutes. Bicarbonate control slices are similarly incubated for an initial 20 minutes at 37° C. in 2.0 ml of basic medium to which is added from the sidearm an additional 0.5 ml of incubation medium containing 50 mM HCO 3 - , which, after mixing, results in a HCO 3 - concentration of 10 mM and a total volume of 2.5 ml. The incubation is continued for an additional 40 minutes. The various compounds to be tested are dissolved by forming the hydrochloride salts in water. When only the free bases are available, the hydrochloride salts are formed by treating the free base with a molar equivalent of hydrochloric acid and diluting to the appropriate concentrations. Just prior to incubation, all flasks containing HCO 3 - are gassed for 5 minutes with 2.5% CO 2 /97.5% O 2 instead of 100% O 2 .
Following the 60-minute incubation period, tissue slices are separated from incubation medium by filtration, reweighed, and homogenized in 1N HClO 4 (10% w/v) for electrolyte analysis. The tissue content of ion is expressed in micromoles per gram initial preswelling fresh weight. Control slice swelling is expressed as microliters per gram initial preswelling fresh weight. The effectiveness of an inhibitor at a given concentration is measured by the amount of HCO 3 - -stimulated swelling that occurred in its presence, computed as a percent of the maximum possible. Tissue and media Na + and K + levels are determined by emission flame photometry with Li + internal standard; Cl - levels are determined by amperometric titration. Tissue viability during incubation is monitored by manometry.
EXAMPLE 2
[(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid
Step A: 3,4,5-Trichlorophenol, benzyl ether
A mixture of 3,4,5-trichlorophenol (8.0 g, 0.04 mole) benzyl bromide (7.5 g, 0.044 mole) and potassium carbonate (6.1 g, 0.044 mole) in N,N-dimethylformamide (DMF) (50 mL) was heated at 60° C. with stirring for 3 hours then poured into ice water. The 3,4,5-trichlorophenol benzyl ether was filtered rinsed with water, dried and used in Step B without further purification.
Step B: 2,3-Dichloro-5-benzyloxyanisole
A mixture of 3,4,5-trichlorophenol benzyl ether (7.5 g, 0.026 mole) and sodium methoxide (1.7 g, 0.032 mole) in hexamethylphosphoramide (60 ml) was heated with stirring on a steam bath for 20 hours. The reaction mixture was poured into ice water, extracted into ether, washed with water, brine, and dried over magnesium sulfate. The solvent was evaporated at reduced pressure and the residual oil chromatographed on silica gel (320 g) eluting with ethyl acetate-hexane; 1:4 to obtain 1.1 g of 2,3-dichloro-5-benzyloxyanisole which melted at 79°-81° C.
Analysis for C 14 H 12 Cl 2 O 2 : Calc: C, 59.38, H, 4.27; Found: C, 59.94; H, 4.25.
Step C: 3,4-Dichloro-5-methoxyphenol
To a solution of 2,3-dichloro-5-benzyloxyanisole (3.4 g, 0.02 mole) in acetic acid (60 ml) was added 5% palladium on carbon (2.0 g) and the mixture hydrogenated using a Parr apparatus at 20 p.s.i. of hydrogen for 3 hours. The catalyst was removed by filtration and the acetic acid evaporated at reduced pressure. The residue was dissolved in ether, extracted with 2N sodium hydroxide acidified, extracted into ether, washed with water, brine, dried over magnesium sulfate and the solvent removed by evaporation in vacuo to give 1.0 g of 3,4-dichlor-5-methoxyphenol which melted at 119°-120° C.
Analysis for C 7 H 6 Cl 2 O 2 : Calc: C, 43.55; H, 3.13; Found: C, 43.88; H, 3.12.
Step D: 2-(3,4-Dichloro-5-methoxy)phenoxypentanoic acid
A mixture of 3,4-dichloro-5-methoxyphenol (1.1 g, 0.0062 mole) potassium carbonate (0.95 g, 0.0068 mole) and ethyl 2-bromopentanoate (1.35 g, 0.0065 mole) in N,N-dimethylformamide (10 ml) was heated at 65° C. with stirring for 1 hour. To the reaction mixture was added water (10 ml) and 10N sodium hydroxide solution (2 ml) and heating was continued on a steam bath for 3 hours. The reaction mixture was poured into ice water, acidified with hydrochloric acid, extracted with ether, washed with water, brine, dried over MgSO 4 and evaporated at reduced pressure to give 1.7 g of 2-(3,4-dichloro-5-methoxy)phenoxypentanoic acid which melted at 141° C. after recrystallization from butyl chloride.
Analysis for C 12 H 13 Cl 2 O 4 : Calc: C, 49.33; H, 4.49; Found: C, 49.33; H, 4.87.
Step E: 4,5-Dichloro-6-methoxy-3-oxo-2-propylbenzo-furan
A solution of 2-(3,4-dichloro-5-methoxy)phenoxypentanoic acid (7.5 g, 0.027 mole) and thionyl chloride (12 g, 0.10 mole) in benzene (30 ml) was heated at reflux for 1 hour. The benzene and excess thionyl chloride were evaporated at reduced pressure and the residual acid chloride was dissolved in methylene chloride (60 ml), cooled to 5° C. and treated over 1/2 hour with aluminum chloride (3.5 g, 0.027 mole). The reaction mixture was stirred at 25° C. for 18 hours then heated at reflux for 1/2 hour. The methylene chloride was evaporated at reduced pressure, the residue treated with ice water, extracted with ether, washed with water, brine, dried over MgSO 4 and the solvent evaporated at reduced pressure. Chromatography on silica gel (175 g) with ethyl acetate-hexane; 1:4 gave 3.5 g of 4,5-dichloro-6-methoxy-3-oxo-2-propylbenzofuran which melted at 90°-92° C.
Analysis for C 12 H 12 Cl 2 O 3 : Calc: C, 52.38; H, 4.40; Found: C, 52.45, H, 4.45.
Step F: 1,2-Dichloro-3-methoxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran
A solution of 4,5-dichloro-6-methoxy-3-oxo-2-propylbenzofuran (0.785 g, 0.0029 mole) in tetrahydrofuran (THF) (8 ml) was warmed to 40° C. and treated with 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) (10 μl) and then with methyl vinyl ketone (2 ml) over a 10 minute period. The reaction mixture was heated at 55° C. for 1/2 hour during which time DBN (2 x 10 μl) was added. The THF was evaporated in vacuo, the residual oil dissolved in ether and ethyl acetate, washed with water, dried over MgSO 4 and evaporated in vacuo. The residual oil consisting of 4,5-dichloro-6-methoxy-3-oxo-2-(3-oxobutyl)-2-propylbenzofuran (0.81 g) was dissolved in ethanol (10 ml) and water (5 ml), treated with 5% NaOH (1 ml) and stirred at 25° C. for 72 hours. Treatment of the reaction mixture with water (5 ml) caused precipitation of 1,2-dichloro-3-methoxy-8-oxo-5a-propyl-5a,6,7,8,-tetrahydrodibenzofuran (0.6 g) which melted at 172°-173° C.
Analysis for C 16 H 16 Cl 2 O 3 : Calc: C, 58.73, H, 4.93; Found: C, 58.81; H, 5.07.
Step G: 1,2-Dichloro-3-hydroxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran
A mixture of 1,2-dichloro-3-methoxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran (0.6 g) and pyridine hydrochloride (7 g) was heated with stirring at 190° for 1/2 hour then poured into ice water. The solid which separated was filtered, rinsed with water, dried and used in Step H without further purification.
Step H: [(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid
A stirred mixture of 1,2-dichloro-3-hydroxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran (0.4 g) potassium carbonate (0.2 g) and ethyl bromoacetate (200 μl) in N,N-dimethylformamide (7 ml) was heated at 65° C. for 1 1/4 hours. The reaction mixture was poured into ice water and the solid ester which precipitated was removed by filtration then dissolved in methanol (15 ml) containing water (1 ml) and 10N sodium hydroxide (1 ml). After 1/2 hour the methanol solution was poured into dilute aqueous hydrochloric acid, extracted with ether which was washed with water, brine, dried over MgSO 4 and evaporated in vacuo. Trituration of the residue with methylene chloride gave 0.35 g of (1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)acetic acid which melted at 248°-250° C.
Analysis for C 17 H 16 Cl 2 O 5 : Calc: C, 55.00; H, 4.34; Found: C, 55.14; H, 4.48.
EXAMPLE 3
Resolution of [(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid
Racemic [(1,2-dichloro-8-oxo-5a-propyl5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid (3.71 g, 10 mmole) in acetonitrile (270 ml) is heated to boiling and cinchonine (2.95 g, 10 mmole) is added. The solution is stirred at 5° C. for 48 hours and the solid (I) that separates removed by filtration, washed with acetonitrile and dried. The filtrate (II) is saved. The solid (I) is recrystallized from acetonitrile and the product removed by filtration, washed with acetonitrile, dried, treated with 1 normal hydrochloric acid (50 ml) and extracted with a solution of 20% tetrahydrofuran in ether. The extract is washed with brine dried over magnesium sulfate, the solvent evaporated in vacuo and the residue recrystallized from toluene to give the pure R-enantiomer of [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid.
Filtrate II is evaporated in vacuo, treated with 2N hydrochloric acid (45 ml), extracted with 20% tetrahydrofuran in ether, washed with brine and dried over magnesium sulfate. The solvent is evaporated in vacuo and the residue dissolved in acetonitrile (250 ml), heated to boiling and cinchonidine (2.95 g, 10 mMole) is added. The solution is cooled to 5° and stirred for 48 hours. The solid that separates is treated as described for I to obtain the pure S-enantiomer of [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid.
EXAMPLE 4
2-[(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethaneimidamide hyd
Step A: 2-[(1,2-DiChloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetonitri
A stirred mixture of 1,2-dichloro-3-hydroxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran (0.4 g), potassium carbonate (0.2 g) and chloroacetonitrile (160 μl) in N,N-dimethylformamide (7 ml) is heated at 65° C. for 2 hours, poured into ice water, extracted with ether, washed with water, brine, dried over MgSO 4 and evaporated in vacuo. Trituration of the residual oil with butyl chloride gives 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzouran-3-yl)oxy]acetonitrile which is filtered and dried.
Step B: 2-[(1,2-Dichloro-5a,6,7,8-tetrahydro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-2-yl)oxy]ethaneimidamide hydrochloride
To a solution of 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetonitrile (200 mg) in methanol (3 ml) is added sodium methoxide (10 mg). After stirring for 1 hour ammonium chloride (80 mg) is added and stirring is continued for 2 hours. The reaction mixture is poured into ice water containing 0.5 ml of 10N sodium hydroxide extracted with ether, washed with water dried over potassium carbonate, filtered and acidified with 10N ethanolic hydrochloric acid to precipitate 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuranyl)oxy]ethaneimidamide hydrochloride.
EXAMPLE 5
Preparation of the two enantiomers of 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofura ethanimidamide hydrochloride
Step A: R-1,2-Dichloro-3-hydroxy-8-oxo5a-propyl-5a,6,7,8,-tetrahydrodibenzofuran
R-[(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid (Example 3) (1.86 g, 5 mmole) and pyridine hydrochloride (18.6 g, 160 mMole) is heated with stirring for 15 minutes at 185° C. and then poured into crushed ice. The solid R-1,2-dichloro-3-hydroxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran that separates is separated by filtration, washed with water, dried and used in the next step without purification.
Step B: R-[(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8 -tetrahydrodibenzofuran-3-yl)oxy]acetonitrile
By carrying out the reaction as described in Example 4, Step A, except that the racemic 1,2-dichloro-3-hydroxy-8-oxO-5a-propyl-5a,6,7,8-tetrahydro is replaced by R-1,2-dichloro-3-hydroxy-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran there is obtained R-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetonitrile.
Step C: R-2-[(1,2-Dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimid
By carrying out the reaction as described in Example 4, Step B except that the racemic 2-[(1,2 --dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodib acetonitrile is replaced by R-2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetonitrile there is obtained R-2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimidamide hydrochloride.
By replacing the R-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid used in Example 5, Step A with the corresponding S-enantiomer and using the product of that reaction in Step B and the product of Step B in Step C there is obtained S-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimidamide hy
EXAMPLE 6
1-Carboxy-1-methylethyl [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-
[(1,2-Dichloro-8-oxo-5a-propyl-5a-propyl-5a,6,7,8,tetrahydrodibenzofuran-3-yl)oxy]acetic acid (3.71 g, 10 mmole) is dissolved in tetrahydrofuran (20 ml). 1,1'-Carbonyldiimidazole (3.2 g, 10 mmole) is added and the mixture stirred at 20° C. for one hour. 2-Hydroxy-2-methylpropionic acid (1.05 g, 10 mmole) is added and the mixture stirred for 18 hours at 25° C. The solvent is removed by evaporation in vacuo and the residue dissolved in methylene chloride, washed with water and dried over magnesium sulfate. The solvent is removed by evaporation in vacuo and the residue purified by column chromatography over silica (250 g) using a methylene chloride/tetrahydrofuran/acetic acid 100/2/1 (v.v.v.) mixture as the eluant. Selecting the appropriate fractions gave 1-carboxy-1-methylethyl [(1,2-dichloro-8-oxo-5a -propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetate upon evaporation of the solvent.
By using a pure enantiomer (R- or S-) of [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid instead of the racemate, there is obtained the pure 1-carboxy-1-methylethyl R-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetate or 1-carboxy-1-methylethyl S-[(1,2-dichloro-8-oxo-5a -propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetate.
EXAMPLE 7
Parenteral solution of the Sodium Salt of R-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran acetic acid
The R-[(1,2-dichloro-8-oxo-5a-propyl5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid (Example 3) (500 mg) is dissolved by stirring and warming with a solution of 0.25N sodium bicarbonate (5.6 ml). The solution is diluted to 10 ml with water and sterilized by filtration. All the water that is used in the preparation is pyrogen-free. The concentration of the active ingredient (calculated as free acid) in the final solution is 5%.
Similar parenteral solutions can be prepared by replacing the active ingredient of this Example by any of the other carboxylic acids of this invention.
EXAMPLE 8
Parenteral solution of R-2-[(1,2-Dichloro-8-oxo-5a-propyl-5a,5,7,8-tetrahydrodibenzofuran-3-yl) hydrochloride
The R-2-[(1,2-dichloro-8-oxo-5a-propyl5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimidamide hydrochloride (Example 5) (549 mg) is dissolved by warming with sufficient water to give a total volume of 10 ml and the solution is sterilized by filtration. All the water used in the preparation is pyrogen-free. The concentration of the active ingredient (calculated as free base) is 5%.
Similar parenteral solutions can be prepared by replacing the active ingredient of this Example by any of the other imidamide salts of this invention.
EXAMPLE 9
Dry-Filled Capsules Containing 100 mg of Active Ingredient (free acid) Per Capsule
______________________________________ Per Capsule______________________________________[(1,2-Dichloro-8-oxo-5a- 100 mgpropyl-5a,6,7,8-tetrahydro-dibenzofuran-7-yl)oxy]-acetic acidLactose 99 mgMagnesium Stearate 1 mgCapsule (Size No. 1) 200 mg______________________________________
The [(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]acetic acid (Example 2, Step H) is reduced to a No. 60 powder and then the lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 1 dry gelatin capsule.
EXAMPLE 10
Dry-Filled Capsules Containing 100 mg of Active Ingredient (free and) Per Capsule
______________________________________ Per Capsule______________________________________2-[(1,2-Dichloro-8-oxo-5a- 110 mgpropyl-5a,6,7,8-tetrahydro-furan-3-yl)oxy]ethanimidamidehydrochlorideLactose 89 mgMagnesium Stearate 1 mgCapsule (Size No. 1) 200 mg______________________________________
The 2-[(1,2-dichloro-8-oxo-5a-propyl-5a,6,7,8-tetrahydrodibenzofuran-3-yl)oxy]ethanimidamide hydrochloride (Example 4, Step B) is reduced to a No. 60 powder and then the lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 1 dry gelatin capsule.
EXAMPLE 11
Dry-Filled Capsules Containing 100 mg of Active Ingredient (ester) Per Capsule
______________________________________ Per Capsule______________________________________1-Carboxy-1-methylethyl [(1,2- 100 mgdichloro-8-oxo-5a,6,7,8,tetra-hydrodibenzofuran-3-yl)oxy]-acetateLactose 99 mgMagnesium Stearate 1 mgCapsule (Size No. 1) 200 mg______________________________________
The 1-carboxy-1-methylethyl [(1,2-dichloro8-oxo-5a-propyl-5a,6,7,8,tetrahydrodibenzofuran-3-yl)oxy]acetate (Example 6) is reduced to a No. 60 powder and then the lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 1 dry gelatin capsule.
Similar dry-filled capsules can be prepared by replacing the active ingredient of this Example by any of the other compounds of this invention. | The invention relates to novel (1,2-dichloro-8-oxo-5a-substituted-5a,6,7,8-tetrahydrodibenzofuran-3-yl)alkanoic acids and alkanimidamides, their derivatives and their salts. The compounds are useful for the treatment and prevention of injury to the brain and of edema due to head trauma, stroke (particularly ischemic), arrested breathing, cardiac arrest, Reye's syndrome, cerebral thrombosis, cerebral embolism, cerebral hemorrhage, cerebral tumors, encephalomyelitis, spinal cord injury, hydrocephalus, post-operative brain injury trauma, edema due to cerebral infections including that due to AIDS virus, various brain concussions and elevated intracranial pressure. | 2 |
This invention was made during the course of work supported at least in part by NIH grant #AI-18796-02 and U.S. Army Medical Research and Development Command grant DAMD 17-83-C-3239; the U.S. Government has rights in this invention.
This is a continuation of co-pending application Ser. No. 741,232 filed on June 4, 1985 now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to protecting against bacterial infection.
Traditional immunological models posit two classes of immune response: 1) the cellular immune responses mediated by lymphocytes designated as T cells which act directly against foreign matter or which activate macrophages to act against foreign matter; and 2) the humoral immune response initiated by a second class of lymphocytes designated as B cells. The cellular response involves direct attack by sensitized T cells on the invading antigen, e.g., attack on the surface of a foreign cell resulting in cell lysis. The humoral response involves secretion of antibodies by sensitized B cells. There are several other types of T cells in addition to the above-described cytotoxic T cells, including T cells that aid B-cell differentiation and proliferation (helper T cells), T cells that amplify cytotoxic T cells (T A cells), and T cells that suppress immune responses (suppressor T cells).
Much attention has been paid to antibody production by B cells, and it has become standard practice to generate antibodies to a selected antigen using hybrid cells made by fusing a sensitized B cell to a myeloma cell (B cell tumor line) that confers immortality on the hybrid.
It has also been known that an immune protection to pathologic bacteria or characteristic surface features of such bacteria can be transferred from one individual or species to another.
Ziegler et al. (1982) N.E. J. Med. 307:1225-1230 report treating human patients with human antiserum to bacterial endotoxin (lipopolysaccharide) prepared by vaccinating humans with heat killed Escherichia coli J5, a mutant having a core identical to most gram negative bacteria and lacking lipopolysaccharide oligosaccharide side chains.
An immune response to the capsular polysaccharide of Bacteroides fragilis protects against abscess formation caused by that organism. That immune response is reported to be cellular in nature, rather than humoral, and the cells that mediate the response are reportedly antigen-specific but non-H-2-restricted T cells belonging to the Ly-1 - 2 + subset, a subset which would not be expected to include helper T cells. Shapiro et al. (1982) J. Exper Med. 154:1188-1197. Thus, Shapiro et al. say (at pp. 1195) that
It is not known how the protective effect against B. fragilis abcesses is mediated, but antibody production does not appear to play a decisive role . . . One might speculate that the immune T cell population is composed of suppressor cells . . . [A]nother possible interpretation is that T cells prevent the bacteria from becoming established at all . . . [An effector] T cell could function by binding or inactivating the bacteria or (more likely) by releasing a lymphokine that activates or attracts macrophages.
The protection against B. fragilis can be passively transferred by nylon wool non-adherent spleen cells. Onderdonk et al. (1982) J. Clin. Invest. 69:9-16.
Suppressor T cells are known to produce soluble factors specific for molecular antigens, and those soluble factors interact with other cells to control an immune response. Asherton et al. (1982) Annals. N.Y. Acad. Sci. Vol. 392:71-89. Healy et al. (1983) J. Immunology 131:2843-2847 disclose a suppressor T-cell hybridoma. Lifshitz et al. disclose a helper T-cell factor (1983) Proc. Nat'l Acad. Sci. 80:5689-5693. Murphy et al. (1983) J. Immunol. 130:2876-2881 disclose a soluble factor produced by antigen-specific suppressor T cells.
SUMMARY OF THE INVENTION
We have discovered that suppressor T cells produce a water soluble protein factor in response to a challenge by a bacterium or characteristic antigenic surface components of that bacterium. The protein factor conveys specific protection against the challenging bacterium when transferred as a soluble suppressor T-cell lysate or purified fraction thereof.
In one aspect, the invention features a method of protecting a mammal against a pathogenic bacterium by administering a water-soluble suppressor T-cell factor derived from a mammal that has been immunized with the bacterium or an antigenic surface fragment of the bacterium.
In a second aspect, the invention features: a hybrid cell comprising a fusion of a suppressor T cell from such an immunized organism; soluble factors and methods of treatment using such hybrid cells; and methods of making such hybrid cells.
In a third aspect, the invention features a soluble protein factor that confers immunity against B. fragilis-induced abscesses, the factor being characterized by: a) a molecular weight below 12,000; b) elution from a P2 Biogel column in fractions intermediate between the bed volume and the void volume using 4° C. 5mM NH 4 CH 3 COO - at pH 7.1, 8 cc/hour; and c) heat lability.
In preferred embodiments of the first two aspects, the bacterium is a member of the species E. coli or B. fragilis. The B. fragilis protection is provided by organisms immunized with the capsular polysaccharide of that bacterium.
The immune mechanism at work here is distinct from humoral immune mechanisms in that the factors are distinct from antibodies in their source (T cells, not B cells), their size (much smaller), and their structure (the absence of the large constant region characteristic of antibodies). The factors are also distinct from relatively non-specific protective T-cell products such as lymphokines or interferons. Finally, the factors are present in a cell lysate and are derived from suppressor T cells, thus distinguishing them from cellular immune response by cytotoxic T cells.
Other features and advantages of the invention will be apparent from the following description of the preferred embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The anti-bacterial T-cell factor is illustrated by the following description of an anti-B. fragilis factor.
Bacteriodes fragilis, an extracellular gram negative anaerobe accounting for the majority of positive anaerobic blood cultures, is a common isolate from intraabdominal abscesses, particularly abscesses arising from a colonic source.
A cell-free factor (ITF) prepared from an immune splenic T-cell population protects from development of intraabdominal abscesses caused by B. fragilis. The active material is low in molecular weight, selectively binds to B. fragilis capsular polysaccharide, and induces antigen-specific immunity to abscesses. The material is heat-labile and loses efficacy after protease, but not nuclease, digestion.
Preparation of ITF
ITF is prepared by immunizing C57BL6 mice (Jackson Laboratory, Bar Harbor, Me.) at 6-10 weeks of age with capsular polysaccharide (CP) antigen of B. fragilis (ATCC accession number 23745, American Type Culture Collection, Rockville, Md.). CP antigen preparation is described in Kasper et al. (1983) J. Bacteriol. 153:991-997. Mice are immunized with 10 mg of antigen in 0.1 ml phosphate buffered saline (PBS) three times/week for three weeks.
At the fourth week, spleens from immunized mice are removed by blunt dissection, gently teased apart, and ground over a wire mesh screen. Cell suspensions in balanced salt solution (BSS) with 5% fetal calf serum (FCS) (M. A. Bioproducts, Walkersville, Md.) are counted by trypan blue dye exclusion after filtering through glass wool. Nylon wool columns are utilized to eliminate B cells and macrophages and to obtain T-cell-enriched spleen cell suspensions using the general method described in Onderdonk et al., cited above.
Lysates of T-cell-enriched fractions from immunized mice are prepared by serial freeze-thawing of known concentrations of cells. Suspensions containing 2.5×10 7 cells/ml are shell-frozen with dry ice and alcohol and then transferred to a boiling water bath sequentially four times. Debris is filtered out by passage over glass wool, and the volume returned to starting volume with BSS and 5% FCS. 1 ml aliquots are stored at -80° C. Microscopic examination of the solution should reveal no intact cells.
One ml of the lysate prepared from T cells from immunized mice (ITF) is placed into a 12,000 MW exclusion dialysis membrane (Arthur H. Thomas Co., Philadelphia, Pa.) and dialyzed at 4° C. against 10 ml of 5 mM ammonium acetate buffer, ph 7.1. Dialysis proceeds for 24 hours with two changes of the dialysate. The contents of the dialysis bag are removed and frozen immediately at -80° C. The dialysate is pooled (30 ml total volume) and frozen at -80° C.
One cc of ITF containing the equivalent of 5×10 7 cells/ml is fractionated on an S-200 column, .9×50 cm column (Pharmacia, Uppsala, Sweden). The buffer is phosphate buffered saline (PBS) pH 7.2 and the column is run at 4° C. at a speed of 8 cc/h. Fractions are read at 280, 260 and 210 nm in a spectrophotometer (Perkin-Elmer, Norwalk, Conn.) and pooled fraction peaks are collected. Three ml of active peaks are, in turn, loaded on a P2 Biogel (Bio-Rad, Richmond, Calif.) column, 1.6×90 cm (Amicon, Danvers, Mass.) and run at 4° C. in 5 mM ammonium acetate buffer pH 7.1 at a speed of 8 cc/h. The refractive index (RI) is monitored (Waters Assoc., Milford, Mass.), appropriate fractions are pooled, and testing is performed in mice.
Use of ITF
The factor's ability to protect selectively against B. fragilis-related abscesses is tested by injecting 0.1-0.2 cc of factor or column fractions into mice by the intracardiac (i.c.) route. After 24 hours, animals are challenged i.p. with B. fragilis or complex inocula containing B. fragilis at a concentration of 1×10 6 organisms. Organisms are mixed 50:50 v/v with sterile cecal contents from meat-fed rats as adjuvant. Animals are sacrificed six days later and examined for abscesses. Animals with one or more gross abscess containing polymorphonuclear leukocytes (PMN) by gram stain are scored as positive for abscesses. For the experiments with complex inocula, abscess contents are cultured and gram negative rods of differing colonial morphologies, usually 5-10 colonies per plate, are subcultured and identified using standard anaerobic identification procedures.
ITF at concentrations of 2.5-25×10 6 cell equivalents prevents the development of abcesses following challenge with viable B. fragilis to the same degree as 2.5×10 6 intact immune T cells. No protection is provided against organisms such as B. distasonis (ATCC 8503) or Fusobacterium varium (TVDL 37). Neither 2.5×10 6 nonimmune T cells or 25×10 6 cell equivalents of NITF, a factor prepared from such T cells, provide any protection. Even a dose of 0.25×10 6 cell equivalents of ITF provides a significant degree of protection compared to NITF. Crude factor prepared by lysing immune T cells leaving no cells intact by microscopic examination is as active as intact cells in preventing abscess formation in mice. Protective ITF is prepared from mouse splenic T cells at least 46 days following completion of the immunization protocol.
Specificity of ITF
ITF's specificity for B. fragilis can be demonstrated not only by its failure to confer protection against other bacteria but also by its selective binding to B. fragilis CP. To verify this characteristic of ITF, it is adsorbed with sheep red blood cells (SRBC) coupled with either B. fragilis capsular polysaccharide or an unrelated capsular polysaccharide.
The preferred capsular polysaccharide of either B. fragilis or type III group B Streptococcus (GBS) is extracted and purified and coupled to sheep red blood cells (SRBC) with chromium chloride by the general method of Baker et al. (1976) J. Exp. Med. 143:258-270. Purified capsular polysaccharides are added to 10% solutions of SRBC in the presence of 1% chromium chloride. After five minutes incubation at room temperature, cells are washed in saline. Coupling is confirmed by specific hemagglutination of sensitized RBC in microtiter plates by rabbit antisera raised to purified CP. ITF, prepared as above, is incubated with SRBC coupled to either CP or with SRBC alone at 4° C. for 30 minutes. SRBC concentrations are 5× 10 7 and 2.5×10 8 cells for 2.5×10 7 cell equivalents of ITF. After 30 minutes incubation, SRBC are removed by centrifugation. 25×10 6 cell equivalents of ITF in 0.2 cc are transferred i.c. to naive mice. Mice are challenged as usual with B. fragilis 24 hours later.
Mice receiving unadsorbed ITF and ITF adsorbed with SRBC alone or SRBC coupled to GBS CP are protected against abscesses caused by B. fragilis. Mice receiving ITF adsorbed with SRBC coupled to B. fragilis CP develop abscesses. Thus, absorption of ITF with SRBC coupled to B. fragilis, but not to the unrelated polysaccharide, elimates the protective effect of the factor indicating that ITF derived from immune splenic T cells is capable of specific binding to the B. fragilis CP.
Characterization of ITF
To assess an approximate molecular size of the component which confers protection, ITF is dialyzed in a 12,000 MW exclusion dialysis membrane for 24 hours at 4° C. against 5 mM ammonium acetate pH 7.1.
The active component of the lysate is smaller than 12,000 MW since the dialysis bag contents loses protective capacity, while the dialysate is protective despite a thirty-fold dilution from the initial volume of 1 ml.
The T-cell lysate is purified partially by molecular sieve chromatography. ITF is loaded initially on an S-200 column and pooled fractions tested for protective activity in mice. Protection is conferred by fractions near and at the bed volume of the column. A protective peak which elutes at 26 ml from the S-200 column (where 12 ml represented void volume and 43 ml bed volume) is placed on a P2 Biogel column. Two ml fractions from the P2 Biogel column are pooled as marked by an elution profile recorded by RI monitoring. The P2 Biogel column has an exclusion size of 1800 MW for proteins. Doses of 0.2 cc of these pooled fractions are transferred to mice which are challenged and examined for abscesses.
Mice given 0.2 ml of peaks intermediate between the bed volume and void volume are protected from abscess formation. The bed volume peak and void volume peak do not protect. Thus, on the P2 Biogel column, protective activity resides in column fractions intermediate between the void volume and bed volume.
Heating ITF to 37° C. or 56° C. for 30 minutes eliminates the protective effect. The extreme heat lability of column-purified ITF indicates that the active component was not antibody. DNase/RNase treatments do not alter protection, but both pronase and trypsin digestion, however, eliminate the protective effect of ITF against abscesses caused by B. fragilis (p. less than 0.001 compared to ITF), indicating that ITF is a protein or, alternatively, that activity depends on a protein co-factor.
T-Cell Hybridomas
As an alternative to producing ITF from suppressor T-cell lysate, a hybridoma is produced by fusing an immunized suppressor T cell with a transformed or malignant cell. For example, the T cell may be fused with a mouse thymoma cell (T cell tumor line BW ATCC No. 5147) according to techniques known in the art for making hybridomas to produce monoclonal antibodies. A suitable fusion technique that can be followed is reported in Taniguchi et al. (1980) Nature 283:227 et seq.
A hybridoma producing ITF is selected by first isolating a single cell using the limiting dilution technique described generally in Langhore et al. (1981) Immunological Methods 2:-221 et seq. and then screening. For example, an in vitro bacteriological assay can be used to screen cells; alternatively, an immunological screening technique using antibody directed to ITF can be used.
Such an ITF-producing hybridoma was deposited with American Type Culture Collection, 12301 Parklawn Drive, Rockville, Md. 20852, on May 14, 1985, and has the accession number HB 8004.
Other Embodiments
Other embodiments are within the following claims. For example, the invention can be used to provide protection against other pathogenic bacteria. For example, rats immunized with rough mutant J5 Escherichia coli are a source of suppressor T cells (splenic) that produce a soluble factor protecting against challenge by wild-type E. coli. The suppressor T cells producing ITF can be human cells, rat cells, or mouse cells. | A method of protecting a mammal against a pathogenic bacterium by administering a soluble suppressor T-cell factor derived from a mammal that has been immunized with the bacterium or an antigenic surface fragment of the bacterium. Also disclosed are a hybrid cell fusion of an immunized suppressor T cell, methods of making such cells, and method of producing soluble suppressor T-cell factors. | 2 |
BACKGROUND OF THE INVENTION
This invention relates to a bicyclo[3.3.0]octene derivative and a process for producing the same.
9(0)-methano-Δ 6 (9α) -PGI 1 has a potent platelet aggregation inhibiting action. For example, its action is comparable to chemically unstable PGI 2 , when human platelet is employed, and it is a compound which can be utilized as a therapeutic or preventive for various diseases of circulatory organs (see the test examples shown below).
In the prior art, as the process for producing 9(0)-methano-Δ 6 (9α) -PGI 1 , there have been known (a) the process in which it is produced through the 14 steps using PGE 2 as the starting material [Preliminary Text for Lectures in 103rd Annual Meeting in Pharmaceutical Society of Japan, p. 156, (1983)] and (b) the process in which it is produced from 1,3-cyclooctadiene through 19 steps [Preliminary Text for Lectures in 103rd Annual Meeting in Pharmaceutical Society of Japan, p. 157, (1983)]. The former process has the drawback that the starting material is expensive, while the latter process that the desired product is formed as a racemic mixture. Further, both processes (a) and (b) are also disadvantageously very low in the overall yield.
SUMMARY OF THE INVENTION
The present inventors have studied extensively to produce 9(0)-methano-Δ 6 (9α) -PGI 1 from a cheap starting material at good yield and with optical activity as well as steric configuration specificity, and consequently found that the compound of the present invention and the process for producing the same can be an important intermediate and a process for achieving the object to accomplish the present invention.
This invention concerns a compound of the formula: ##STR2## wherein R 1 : a straight, branched or cyclic alkyl group or alkenyl group each having 5 to 10 carbon atoms;
R 2 and R 3 : each represent a hydrogen atom or a protective group of a hydroxy group; and
R 4 : --CHO, --CH═CH--(CH 2 ) 2 --COOR 5 or --CH 2 R 6 ; where
R 5 : a hydrogen atom or an alkyl group; and
R 6 : a hydroxy group, an acetyloxy group or a butenyl group,
and a process for producing the same.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The bicyclo[3.3.0]octene derivative represented by the above formula [I] of this invention can be led to 9(0)- methano-Δ 6 (9α) -PGI 1 and derivatives thereof as follows: Namely, among the above bicyclo[3.3.0]octene derivatives, bicyclo[3.3.0]octenylaldehyde derivatives which are R 4 being --CHO can be led to 9(0)-methano-Δ 6 (9α) -PGI 1 by subjecting them to elongation reaction of α-chain by using Wittig reagent which is prepared by 3-carboxypropyltriphenylphosphonium bromide and a base, subjecting a hydroxy group to deprotection reaction, then subjecting a double bond selectively to reduction and thereafter subjecting an ester to hydrolysis; (4'-alkoxycarbonyl-1'-alkenyl)-cis-bicyclo[3.3.0]octene derivatives which are R 4 being --CH═CH--(CH 2 ) 2 --COOR 6 can be led the same by subjecting them to elongation reaction of α-chain, subjecting a hydroxy group to deprotection reaction and thereafter subjecting an ester to hydrolysis; and bicyclo[3.3.0]octene derivatives which have R 4 being --CH 2 R 5 can be led the same by subjecting them to hydration reaction, then subjecting a hydroxy group to deprotection reaction, and thereafter subjecting to oxdation reaction (see the following Reference examples).
The protective group of hydroxy group in this invention may include, for R 2 , a tetrahydropyranyl group, a methoxymethyl group, a 4-methoxytetrahydropyranyl group, a 1-ethoxyethyl group, a 1-methyl-1-methoxyethyl group, a t-butyldimethylsilyl group, a diphenyl-t-butylsilyl group, a benzoyl group, an acetyl group, etc. and, for R 3 , a t-butyldimethylsilyl group, a benzoyl group, an acetyl group, a tetrahydropyranyl group, a methoxymethyl group, a 4-methoxytetrahydropyranyl group, a 1-ethoxyethyl group, a 1-methyl-1-methoxyethyl group, a diphenyl-t-butylsilyl group, etc.
The bicyclo[3.3.0]octene derivative represented by the above formula [I] can be produced according to the reaction schemes as shown below.
In the compounds of the present invention, (4'-alkoxycarbonyl-1'-alkenyl)-cis-bicyclo[3.3.0]octene derivatives [I-c] can be prepared following the reaction schemes shown below: ##STR3## wherein R 1 , R 2 , R 3 and R 5 are the same as defined above.
[The first step]
This step produces an allyl cyclopentylidene derivative represented by the formula [III] by methylenation of an allyl cyclopentanone derivative represented by the above formula [II].
The allyl cyclopentanone derivative which is employed as the starting material of this step is produced by reacting a cyclopentenone represented by the formula [V]: ##STR4## wherein R 2 represents a protective group of a hydroxy group, with an organic copper compound represented by the formula [VI]: ##STR5## wherein R 1 is the same meaning as defined above; R 3 represents a protective group of a hydroxy group; and Y represents a group of ##STR6## phenylthio group or a 1-pentynyl group (see Japanese Provisional Patent Publication No. 171965/1982).
Examples of the thus obtained compounds may be {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-1'-transoctenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-4'-methyl-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-4'-methyl-1'-trans-octenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-(1'-ethoxyethyloxy)-1'-trans-octenyl]-4(R)-(1'-ethyoxyethyloxy)-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-(1'-ethoxyethyloxy)-3'-cyclopentyl-1'-trans-propenyl]-4(R)-(1'-ethoxyethyloxy)-1-cyclopentanone}, {2(R)-allyl-3(R)-[3'(S)-(1'-ethoxyethyloxy)-4'-methyl-1'-trans-octenyl]-4(R)-(1'-ethoxyethyloxy)-1-cyclo-pentanone} and the like.
The methylenation in this step may be carried out by use of a mixed reagent of methylene bromide-titanium tetrachloride-zinc [L. Lombardo, Tetrahedron Lett., 23, 4293 (1982)] or Johnson reagent [C. R. Johnson, J. R. Shanklin, R. A. Kirchoff, J. Am. Chem. Soc., 95, 6462 (1973)].
The reaction should desirably be carried out in a solvent, for example, a solvent mixture such as a halogenic solvent (e.g. methylene chloride)--an ether solvent (e.g. tetrahydrofuran) in the case of using the former reagent, while an ether solvent in the case of the latter reagent.
The reaction can proceed smoothly at -80° C. to 60° C., but room temperature is preferred because the reaction can be carried out without heating or cooling.
[The second step]
This step produces a hydroxymethyl cyclopentane derivative represented by the above formula [IV] by hydration of an allyl cyclopentylidene derivative represented by the above formula [III].
The hydration reaction in this step is conducted out by hydroboration and oxidation. In carrying out hydroboration, there may be employed a hydroborating reagent such as 9-BBN (9-borabicyclo[3.3.1]nonane), disiamylborane, thexylborane, etc. The amount of the hydroborating agent used may be generally 1 to 3 equivalent.
The reaction is desired to be carried out in a solvent, preferably an ether type solvent such as tetrahydrofuran, diglyme, diethylether, etc.
The reaction proceeds smoothly at -25° C. to room temperature.
Further, this step carries out oxidation of the product subsequent to the hydroboration without isolation thereof. The oxidation may be carried out by use of an oxidizing agent such as an alkaline hydrogen peroxide, an amine oxide, oxygen, peracid, etc. The amount of the oxidizing agent employed may be 5 to 15 equivalents.
The reaction proceeds smoothly at room temperature to 60° C.
In this step, the compound formed by hydroboration with the use of, for example, 9-BBN may be estimated to have a formula as shown below: ##STR7##
[The third step]
This step produces a bicyclo[3.3.0]octenylaldehyde derivative represented by the above formula [I-b] by oxidation and dehydration of the hydroxymethyl cyclopentane derivative represented by the above formula [IV] obtained by the above second step.
In carrying out oxidation, it is possible to use a dimethylsulfoxide-oxalyl chloride, dimethylsulfoxidepyridine complex of sulfur trioxide, etc. The amount of the oxidizing agent employed may be generally 1 to 5 equivalents.
The reaction is desired to be carried out in a solvent, for example, a halogenated hydrocarbon such as methylene chloride.
The reaction can proceed smoothly at a temperature, which may differ depending on the oxidizing agent employed, but generally at -70° C. to room temperature.
For obtaining the oxidized product in this step, a tertiary amine such as triethylamine, diisopropylethylamine, etc. is added into the reaction product and treatment is carried out at -70° C. to room temperature.
Further, this step carries out dehydration of the obtained product subsequent to the oxidation without isolation thereof.
Dehydration is required to be carried out in the presence of an acidic catalyst. As the acidic catalyst, an acid-ammonium salt is available. An acid-ammonium salt can be formed from an acid and an amine. The acid available may be exemplified by trifluoroacetic acid, toluenesulfonic acid, camphorsulonic acid, acetic acid, etc. The amine available may be exemplified by dibenzylamine, diethylamine, dimethylamine, diisopropylamine, piperidine, pyrrolidine, piperazine, etc. These acids and amines may appropriately be selected and combined to be provided for use. Above all, the catalyst comprising a combination of trifluoroacetic acid and dibenzylamine is preferred on account of good yield of the desired product. The amount of the catalyst employed may be about 0.2 equivalent, but it is preferred to employ about one equivalent in order to proceed rapidly the reaction.
The reaction is desired to be carried out in a solvent, for example, an aromatic hydrocarbon such as benzene, toluene, xylene, etc.
The reaction temperature may be selected within the range from room temperature to 100° C., but preferably within the range from 50° C. to 70° C. in order to carry out the reaction smoothly.
[The fourth step]
This step produces a (4'-alkoxycarbonyl-1'-alkenyl)-cis-bicyclo[3.3.0]octene derivative represented by the above formula [I-c] by reacting the bicyclo[3.3.0]octenylaldehyde derivative represented by the above formula [I-b] obtained by the above third step with 3-carboxypropyl triphenyl phosphonium halide represented by the formula: ##STR8## wherein R 7 is an alkyl group or an aryl group, and X is a halogen atom, in the presence of a base.
This step is required to be carried out in the presence of a base. The base may include potassium t-butoxide, butyl lithium, sodium salt of dimethylsulfoxide, etc. For carrying out the reaction with good efficiency, it is preferred to employ potassium t-butoxide. The amount of the base employed may be generally 1 to 1.2 equivalent based on the above 3-carboxypropyl triphenyl phosphonium halide which is employed as one of the starting material. Preferable example of the 3-carboxypropyl triphenyl phosphonium halide is 3-carboxypropyl triphenyl phosphonium bromide.
The reaction may be carried out preferably in an ether solvent such as tetrahydrofuran, dimethoxyethane, diethyl ether, etc. The solvent is not particularly limited, provided that it does not interfere with the reaction.
The reaction temperature may be selected within the range from 0° C. to 50° C., at which the reaction can proceed smoothly.
The compound obtained in this step is formed generally as a free carboxylic acid, but it can be isolated as an ester by use of the condition of diazomethane or alkyl halide-diazabicycloundecene-acetonitrile for the reactions in the subsequent step et seq. Conversion to ester may be conducted according to the method easily done by those skilled in the art.
[The fifth step]
This step produces a bicyclo[3.3.0]octene derivative represented by the above formula [I-a] in which only the disubstituted olefin of α-chain is selectively reduced by catalytic reduction of the (4'-alkoxycarbonyl-1'-alkenyl)-cis-bicyclo[3.3.0]octene derivative represented by the formula [I-c] obtained in the above fourth step.
The available catalysts include palladium catalysts such as palladium-carbon, palladium black, etc., Wilkinson catalysts, platinum, nickel, etc. For carring out the reaction with good efficiency, it is preferred to employ Wilkinson catalyst. The catalyst may be sufficiently employed in the so-called catalytic amount.
In practicing this step, hydrogen may be allowed to react with the compound under normal pressure or under pressurization.
The reaction may be carried out preferably in a solvent, for example, an alcohol solvent such as methanol, ethanol, etc. or an ester solvent such as ethyl acetate, etc.
The reaction can proceed smoothly at a temperature selected within the range from -25° C. to 60° C.
The (4'-alkoxycarbonyl-1'-alkenyl)-cis-bicyclo[3.3.0]octene derivative of this invention has a asymmetric carbon atom in the molecule, and the present invention includes compounds of a R-configuration, S-configuration and a mixture of a volumtary ratio thereof with regard to the asymmetric carbon atom.
Further, in the above formula [I], the bicyclo[3.3.0]octene derivatives in which R 4 being --CH 2 R 6 represented by the formula [I-f] can be produced by subjecting bicyclo[3.3.0]octenyl aldehyde derivative represented by the above formula [I-b] to the reaction step as mentioned below: ##STR9##
[The first step]
This step produces a bicyclo[3.3.0]octenyl methyl alcohol derivatice represented by the above formula [I-d] by reduction of the bicyclo[3.3.0]octenylaldehyde derivative represented by the above formula [I-b].
In the bicyclo[3.3.0]octenylaldehyde derivatives, the compounds in which R 1 are straight or branched alkyl or alkenyl group are prepared according to the method as described in Preliminary text for lectures in 104th annual meeting in Pharmaceutical Society of Japan (1984), p. 282, and the compound in which R 1 are cylcic alkyl or alkenyl are prepared according to the same method as mentioned above.
Reduction is required to be carried out in the presence of a reducing agent. As the reducing agent, diisobutylaluminum hydride, sodium borohydride, lithium aluminumhydride and the like are available. The amount of the reducing agent employed may be about one equivalent or slightly excess amount based on the bicyclo[3.3.0]octenylaldehyde derivative represented by the above formula [I-b].
The reaction should desirably be conducted in a solvent, for example, an alcohol solvent such as methanol, ethanol, etc., an ether solvent such as diethyl ether, tetrahydrofuran, etc., an aromatic solvent such as benzene, toluene, etc., and a halogenic solvent such as methylene chloride, chloroform, etc. The solvent may optionally be selected due to the reducing agent to be used. The reaction can proceed smoothly at -100° to 50° C.
[The second step]
This step produces a bicyclo[3.3.0]octenylmethylacetate derivative represented by the above formula [I-e] by acetylation of the bicyclo[3.3.0]octenylmethyl alcohol derivative represented by the above formula [I-d] obtained in the above first step.
In carrying out acetylation, it is possible to use an acetic anhydride which is generally employed this type of reaction.
Further, in carrying out this step, it is possible to employ a catalyst such as pyridine, 4-dimethylaminopyridine, etc.
The reaction should desirably be conducted in a solvent, for example, an aromatic solvent such as benzene, toluene, etc., an ether solvent such as diethyl ether, tetrahydrofuran, etc., and a halogenic solvent such as methylene chloride, etc.
The reaction can proceed smoothly at -25° to 100° C.
[The third step]
This step produces a pentenylbicyclo[3.3.0]octene derivative represented by the above formula [I-f] by reacting the bicyclo[3.3.0]octenylmethyl acetate derivative represented by the above formula [I-e] obtained in the above second step with lithium dialkylcuprate.
The lithium dialkylcuprate is a compound which is easily prepared by reacting copper (I) iodide with 3-butenyl lithium (as for the preparative method thereof, see R. F. Cunico, Y. K. Han, J. Organomet. Chem., 174, 247 (1977)).
In carrying out this step, an ether solvent such as diethyl ether, tetrahydrofuran, dimethoxyethane, etc. may desirably be employed.
The reaction can proceed smoothly at -100° to 50° C.
The present invention is described in more detail by referring to the following Reference examples and Examples.
REFERENCE EXAMPLE 1
To a solution of {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentanone} (707 mg, 1.44 mmol) dissolved in methylene chloride (7 ml) was added zinc-titanium chloride-methylene bromide reagent (Zn-TiCl 4 -CH 2 Br 2 /THF, 7.48 ml, about 1.3 equivalents) at room temperature. The mixture was stirred at the same condition for 30 minutes so that the starting materials were all reacted. Subsequently, the mixture was poured into the two layer system solution comprising ether-saturated aqueous sodium hydrogencarbonate solution so as to stop the reation. Then, an ether layer was separated from the mixture, and an aqueous layer was extracted with ether. The combined ether layers were washed with a saturated aqueous ammonium chloride solution and saturated saline solution, and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentylidene} (652 mg, Yield: 88%) as substantially colorless oily products.
IR (neat): 3080, 2930, 2850, 1650, 1460, 1360, 1250 cm -1 .
NMR δ (CDCl 3 ): 5.70 (m, 1H), 5.41 (m, 2H), 4.75-5.10 (m, 4H), 4.02 (m, 1H), 3.76 (m, 1H), 2.00-2.70 (m, 6H), 1.40 (m, 8H), 0.88 (s, 21H), 0.02 (s, 12H).
Mass m/z (%): 435 (M + -57), 421, 393, 323, 303, 289, 229, 147, 75, 73.
REFERENCE EXAMPLE 2
To {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentylidene} (700 mg, 1.42 mmol) was added a THF solution (7.10 mmol, 14.2 ml) of 9-borabicyclo[3.3.1]nonane (9-BBN) at room temperature, and the mixture was stirred for 3 hours. Then, to the reaction system were gradually added dropwise a 6 N-NaOH aqueous solution (6.9 ml) and a 30% H 2 O 2 aqueous solution (5.8 ml) at room temperature, and the mixture was stirred at 60° C. for 2 hours. The mixture was extracted with ether, and the separated ether layer was washed with an aqueous sodium thiosulfate solution and water. After dryness with anhydrous magnesium sulfate, followed by evaporation of the solvent and purification through silica gel column chromatography to obtain {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxy-cyclopentane} (502 mg, Yield: 67%) as colorless oily products.
IR (neat): 3350, 2930, 2850, 1460, 1360, 1250 cm -1 .
NMR δ (CDCl 3 ): 5.38 (m, 2H), 3.96 (m, 2H), 3.59 (m, 4H), 2.83 (m, 1H), 2.16 (m, 3H), 1.10-1.80 (m, 15H), 0.87 (s, 21H), 0.04 (s, 12H).
Mass m/z (%): 471 (M + -57), 453, 396, 379, 339, 325, 321, 247, 229, 75, 73.
EXAMPLE 1
To a methylene chloride solution (5 ml) of oxalyl chloride (0.46 ml, 5.40 mmol) was added dropwise a methylene chloride solution (4 ml) of DMSO (0.83 ml, 11.7 mmol) at -78° C. for 5 minutes, and the mixture was stirred at the same condition for 15 minutes. To the thus prepared mixture was added dropwise a methylene chloride solution (3 ml) of {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-4(R)-t-butyldimethylsilyloxycyclopentane} (475 mg, 0.900 mmol), and the mixture was further stirred at -78° C. for 15 minutes. Under the same condition, triethylamine (2.50 ml, 18.0 mmol) was added thereto, then a cooling bath was removed and the mixture was stirred for 15 minutes. Methylene chloride was distilled out under reduced pressure and to the resultant residue were added benzene (8 ml) and trifluoroacetic acid salt of dibenzylamine (220 mg, 0.900 mmol) and the mixture was stirred at 70° C. for 4 hours. The mixture was diluted with ether, washed successively with an aqueous ammonium chloride solution, a saturated aqueous sodium hydrogencarbonate solution and a saturated saline solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purifired through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (441 mg, Yield: 97%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1680, 1460, 1360, 1250 cm -1 .
NMR δ (CDCl 3 ): 9.82 (s, 1H), 6.73 (bs, 1H), 5.48 (m, 2H), 4.08 (m, 1H), 3.76 (m, 1H), 3.24 (m, 1H), 1.10-2.80 (m, 14H), 0.87, 0.90 (2s, 21H), 0.03 (s, 12H).
Mass m/z (%): 449 (M + -57), 435, 359, 339, 317, 303, 202, 73.
EXAMPLE 2
{3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (18.9 mg, 0.0374 mmol) was mixed in a mixed solvent of acetic acid-water-tetrahydrofuran (3:1:1) (0.2 ml) and the mixture was stirred at 45° C. for 3 hours. After evaporation of the solvent under reduced pressure, to the residue was added a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (8.3 mg, Yield: 80%) as substantially colorless oily product.
IR (neat): 3400, 2950, 2850, 1680 cm -1 .
NMR δ (CDCl 3 ): 9.82 (s, 1H), 6.73 (bs, 1H), 5.45 (m, 2H), 4.10 (m, 1H), 3.80 (m, 1H), 3.24 (m, 1H).
Mass m/z (%): 278 (M + ), 260 (M + -H 2 O).
REFERENCE EXAMPLE 3
In the method as described in Reference examples 1 and 2, the same procedures were carried out as in Reference examples 1 and 2 except that {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone} (434 mg, 1 mmol) was employed as the starting material to obtain {1(S)-hydroxy-methyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-4(R)-tetrahydropyranyloxycyclopentane} (374 mg) at a yield of 80% as substantially colorless oily product.
IR (neat): 3350, 2930, 2850, 1450, 1365, 1200 cm -1 .
NMR δ (CDCl 3 ): 5.35 (m, 2H), 4.50 (m, 2H), 4.00 (m, 2H), 3.60 (m, 8H).
Mass m/z (%): 468 (M + ), 450.
EXAMPLE 3
In the method as described in Example 1, the same procedures were carried out in Example 1 except that {1(S)-hydroxymethyl-2(S)-(3'hydroxypropyl)-3(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-4(R)-tetrahydropyranyloxycyclopentane} (374 mg, 0.80 mmol) was employed as the starting material to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (232 mg) at a yield of 65% and as substantially colorless oily product.
IR (neat): 2950, 2850, 1680 cm -1 .
NMR δ (CDCl 3 ): 9.81 (s, 1H), 6.75 (bs, 1H), 5.44 (m, 2H), 4.50 (m, 2H), 3.20-4.10 (m, 7H).
Mass m/z (%): 446 (M + ), 361.
EXAMPLE 4
The reaction was carried out following the same procedures as in Reference examples 1 and 2 and Example 1 by using {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone} (868 mg, 2 mmol) to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (446 mg, Overall yield: 50%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1680 cm -1 .
NMR δ (CDCl 3 ): 9.81 (s, 1H), 6.75 (bs, 1H), 5.44 (m, 2H), 4.50 (m, 2H), 3.20-4.10 (m, 7H).
Mass m/z (%): 446 (M + ), 361.
EXAMPLE 5
{3-Formyl-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (7.8 mg, 0.1 mmol) was dissolved in anhydrous methylene chloride (1 ml), and to the solution was added subsequently dihydropyrane (84 mg, 1 mmol) and catalytic amount of anhydrous p-toluenesulfonic acid and stirred at room temperature for 5 minutes. After the reaction was stopped by adding a saturated aqueous sodium hydrogencarbonate solution, the mixture was extracted with ether. The separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (42.4 mg, Yield: 95%) as substantially colorless oily product. Spectrum data thereof are agreed with those of the sample obtained in Example 3.
REFERENCE EXAMPLE 4
To a methylene chloride (7 ml) solution of {2(R)-allyl-3(R)-[[3'(R)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentanone} (354 mg, 0.72 mmol) was added a zinc-titanium chloride-methylene bromide reagent (Zn-TiCl 4 -CH 2 Br 2 /THF, 3.74 ml, about 1.3 equivalents). The mixture was stirred at the same condition for 30 minutes so that the starting materials were all reacted. Subsequently, the mixture was poured into the two layer system solution comprising ether-saturated aqueous sodium hydrogencarbonate solution so as to stop the reation. Then, an ether layer was separated from the mixture, and an aqueous layer was extracted with ether. The combined ether layers were washed with a saturated aqueous ammonium chloride solution and saturated saline solution, and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentylidene} (326 mg, Yield: 88%) as substantially colorless oily products.
IR (neat): 3078, 2930, 2850, 1648, 1460, 1360, 1247 cm -1 .
NMR δ (CDCl 3 ): 5.70 (m, 1H), 5.40 (m, 2H), 4.70-5.05 (m, 4H), 4.02 (m, 1H), 3.76 (m, 1H), 2.00-2.60 (m, 6H), 1.38 (m, 9H), 0.88 (s, 18H), 0.02 (s, 12H).
Mass m/z (%): 433 (M + -57), 419, 391.
REFERENCE EXAMPLE 5
To {2(R)-allyl-3(R)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxy-1-cyclopentylidene} (698 mg, 1.42 mmol) was added THF solution of 9-borabicyclo[3.3.1]nonane (9-BBN) (7.10 mmol, 14.2 ml) at room temperature, and the mixture was stirred for 3 hours. Then, to the reaction system were gradually added dropwise an aqueous 6 N-NaOH solution (6.9 ml) and an aqueous 30% H 2 O 2 solution (5.8 ml) at room temperature, and the mixture was stirred at 60° C. for 2 hours. The reaction mixture was extracted with ether and the extracted ether layer was washed with an aqueous sodium thiosulfate solution and water. After dryness with anhydrous magnesium sulfate, followed by evaporation of the solvent and purification the residue through silica gel column chromatography to obtain {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxycyclopentane} (442 mg, Yield: 59%) as colorless oily product.
IR (neat): 3345, 2920, 2850, 1456, 1360, 1246 cm -1 .
NMR δ (CDCl 3 ): 5.35 (m, 2H), 3.95 (m, 2H), 3.59 (m, 4H), 2.16 (m, 4H), 1.10-1.80 (m, 16H), 0.87 (s, 18H), 0.04 (m, 12H).
Mass m/z (%): 469 (M + -57), 451, 394, 377.
EXAMPLE 6
To a methylene chloride solution (5 ml) of oxalyl chloride (0.46 ml, 5.40 mmol) was added dropwise methylene chloride solution (4 ml) of DMSO (0.83 ml, 11.7 mmol) at -78° C. for 5 minutes, and the mixture was stirred at the same condition for 15 minutes. To the thus prepared mixture was added dropwise a methylene chloride solution (3 ml) of {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-t-butyldimethylsilyloxycyclopentane} (473 mg, 0.900 mmol), and the mixture was further stirred at -78° C. for 15 minutes. Under the same condition, triethylamine (2.50 ml, 18.0 mmol) was added thereto, then a cooling bath was removed and the mixture was stirred for 15 minutes. Methylene chloride was distilled out under reduced pressure and to the resultant residue were added benzene (8 ml) and trifluoroacetic acid salt of dibenzylamine (220 mg, 0.900 mmol) and the mixture was stirred at 70° C. for 4 hours. The mixture was diluted with ether, washed successively with an aqueous ammonium chloride solution, a saturated aqueous sodium hydrogencarbonate solution and a saturated saline solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purifired through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (385 mg, Yield: 85%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1675, 1450, 1360, 1250 cm -1 .
NMR δ (CDCl 3 ): 9.82 (s, 1H), 6.72 (bs, 1H), 5.45 (m, 2H), 4.05 (m, 1H), 3.76 (m, 1H), 3.23 (m, 1H), 1.10-2.80 (m, 15H), 0.87, 0.90 (2s, 18H), 0.03 (s, 12H).
Mass m/z (%): 447 (M + -57), 433, 357, 337, 315, 301, 200, 71.
EXAMPLE 7
{3-Formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (18.9 mg, 0.0374 mmol) was mixed in a mixed solvent of acetic acid-H 2 O -tetrahydrofuran (3:1:1) (0.2 ml) and the mixture was stirred at 45° C. for 3 hours. After evaporation of the solvent under reduced pressure, to the residue was added a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (8.7 mg, Yield: 84%) as substantially colorless oily product.
IR (neat): 3400, 2950, 2850, 1684 cm -1 .
NMR δ (CDCl 3 ): 9.81 (s, 1H), 6.74 (bs, 1H), 5.45 (m, 2H), 4.10 (m, 1H), 3.80 (m, 1H), 3.23 (m, 1H).
Mass m/z (%): 276 (M + ), 258 (M + -H 2 O).
REFERENCE EXAMPLE 6
In the method as described in Reference examples 4 and 5, the same procedures were carried out as in Reference examples 4 and 5 except that {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone} (432 mg, 1 mmol) was employed as the starting material to obtain {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-tetrahydropyranyloxycyclopentane} (275 mg) at a yield of 74% as substantially colorless oily product.
IR (neat): 3350, 2930, 2850, 1450, 1365, 1200 cm -1 .
NMR δ (CDCl 3 ): 5.34 (m, 2H), 4.50 (m, 2H), 4.00 (m, 2H), 3.60 (m, 8H).
Mass m/z (%): 466 (M + ), 448.
EXAMPLE 8
In the method as described in Example 3, the same procedures were carried out as in Example 3 except that {1(S)-hydroxymethyl-2(S)-(3'-hydroxypropyl)-3(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1-trans-propenyl]-4(R)-tetrahydropyranyloxycyclopentane} (275 mg, 0.74 mmol) was employed as the starting material to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (223 mg) at a yield of 68% as substantially colorless oily product.
IR (neat): 2950, 2850, 1680 cm -1 .
NMR δ (CDCl 3 ): 9.81 (s, 1H), 6.74 (bs, 1H), 5.45 (m, 2H), 4.48 (m, 2H), 3.20-4.10 (m, 7H).
Mass m/z (%): 444 (M + ), 359.
EXAMPLE 9
The reaction was carried out following the same procedures as in Reference examples 4 and 5 and Example 8 by using {2(R)-allyl-3(R)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-4(R)-tetrahydropyranyloxy-1-cyclopentanone} (864 mg, 2 mmol) to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclo-pentyl-1'-transpropenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo-[3.3.0]oct-2-ene} (408 mg, Overall yield: 46%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1680 cm -1 .
NMR δ (CDCl 3 ): 9.81 (s, 1H), 6.74 (bs, 1H), 5.45 (m, 2H), 4.48 (m, 2H), 3.20-4.10 (m, 7H).
Mass m/z (%): 444 (M + ), 359.
EXAMPLE 10
{3-Formyl-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-transpropenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (27.6 mg, 0.1 mmol) was dissolved in anhydrous methylene chloride (1 ml), and to the solution was added subsequently dihydropyrane (84 mg, 1 mmol) and catalytic amount of anhydrous p-toluenesulfonic acid and stirred at room temperature for 5 minutes. After the reaction was stopped by adding a saturated aqueous sodium hydrogencarbonate solution, the mixture was extracted with ether. The separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (39.5 mg, Yield: 89%) as substantially colorless oily product. Various spectrum data thereof are agreed with those of the sample obtained in Example 8.
EXAMPLE 11
3-Carboxypropyltriphenylphosphonium bromide (321 mg, 0.748 mmol) was suspended in THF (3.0 ml), and to the suspension was added potassium t-butoxide (167 mg, 1.49 mmol) and the mixture was stirred at room temperature for 10 minutes. To the obtained yield compound having reddish orange color was added a THF (1.5 ml) solution of {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-transoctenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (189 mg, 0.374 mmol), and the mixture was stirred for 30 minutes. The mixture was diluted with ether, added a 10% aqueous HCl solution and after it was confirmed that the mixture was acidic (pH=4), an ether layer was separated therefrom. After the separated aqueous layer was extracted with ether, the ether layers were combined, washed with a saturated aqueous NaCl solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the resultant residue was dissolved in small amount of ether and added thereof an ether solution of diazomethane to obtain a methyl ester derivative. Evaporation of the solvent, followed by purification and separation through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (194 mg, Yield: 88%) as substantially colorless oily products.
IR (neat): 2950, 2850, 1750, 1460, 1360, 1250 cm -1 .
NMR δ (CDCl 3 ): 6.27 (d, J=16 Hz, 2/5H, trans), 6.02 (d, J=11 Hz, 3/5H, cis), 5.51 (m, 4H), 4.07 (m, 1H), 3.70 (m, 1H), 3.69 (s, 3H), 2.97 (m, 1H), 1.10-2.70 (m, 16H), 0.87, 0.90 (2s, 21H), 0.03 (s, 12H).
Mass m/z (%): 590 (M + ), 534, 533, 519, 458, 427, 401, 301, 75, 73.
[α] D 20 =-37° (c=0.614, CHCl 3 ).
EXAMPLE 12
To a THF (0.5 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (31 mg, 0.05 mmol) was added a solution of tetrabutylammonium fluoride dissolved in THF (0.16 ml, 1M solution), and the mixture was stirred at room temperature for 15 hours. After the reaction was stopped by adding a saturated aqueous ammonium chloride solution, THF was distilled out under reduced pressure. The resultant aqueous layer was extracted with ethyl acetate, and the separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (15 mg, Yield: 79%) as colorless caramel.
IR (neat): 3400, 2950, 1742 cm -1 .
NMR δ (CDCl 3 ): 6.30 (d, J=16 Hz, 1/3H, trans), 6.02 (d, J=11 Hz, 2/3H, cis), 5.60 (m, 3H), 5.40 (m, 1H), 4.10 (m, 1H), 3.80 (m, 1H), 3.70 (s, 3H), 3.02 (m, 1H).
Mass m/z (%): 362 (M + , 7), 344 (44), 326 (19), 300 (37), 220 (54), 178 (55), 168 (41), 43 (100). [α] D 20 =-35° (c=0.466, MeOH).
EXAMPLE 13
In the method as described in Example 11, the same procedures were carried out as in Example 11 except that {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (446 mg, 1 mmol) was employed as the starting material to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (477 mg, Yield: 90%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1745 cm -1 .
NMR δ (CDCl 3 ): 6.25 (d, J=16 Hz, 1/3H, trans), 6.02 (d, J=11 Hz, 2/3H, cis), 5.50 (m, 4H), 4.60 (m, 2H), 3.40-4.10 (m, 6H), 3.69 (s, 3H), 2.97 (m, 1H), 0.87 (t, J=7 Hz, 3H).
Mass m/z (%): 530 (M + ), 499, 445.
EXAMPLE 14
{3-(4'-Methoxycarbonyl-1'-butenyl)-6-(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (470 mg, 0.89 mmol) was dissolved in a mixed solvent of acetic acid (4.7 ml), water (1.6 ml) and THF (1.6 ml), and heated at atmospheric temperature of 45° C. for 6 hours. After evaporation of acetic acid under reduced pressure, to the residue was added a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with saturated saline solution, and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (261 mg, Yield: 81%) as colorless caramel. Spectrum data thereof are agreed with those of the sample obtained in Example 12.
EXAMPLE 15
{3-(4'-Methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (15 mg, 0.04 mmol) was dissolved in methanol (0.3 ml). To the solution was added a 10% aqueous sodium hydroxide solution (0.3 ml) at 0° C. After stirring at 0° C. for 16 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution under cooling. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. The extract was dried with anhydrous magnesium sulfate and distilled out the solvent to obtain {3-(4'-carboxy-1'-butenyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (14 mg, Yield: 100%) as colorless caramel.
IR (neat): 3350, 1720, 1090, 970 cm -1 .
NMR δ (CDCl 3 ): 6.34 (d, J=16 Hz, 1/3H), 6.06 (d, J=11 Hz, 2/3H), 5.65 (m, 3H), 5.45 (m, 1H), 3.10 (m, 1H).
EXAMPLE 16
3-Carboxypropyltriphenylphosphonium bromide (321 mg, 0.748 mmol) was suspended in THF (3.0 ml), and to the suspension was added potassium t-butoxide (167 mg, 1.49 mmol) and the mixture was stirred at room temperature for 10 minutes. To the obtained yield compound having reddish orange color was added THF (1.5 ml) solution of {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (189 mg, 0.374 mmol), and the mixture was stirred for 30 minutes. The mixture was diluted with ether, added a 10% aqueous HCl solution and after it was confirmed that the mixture was acidic (pH=4), an ether layer was separated therefrom. After the separated aqueous layer was extracted with ether, the ether layers were combined, washed with a saturated aqueous NaCl solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the resultant residue was dissolved in small amount of ether and added an ether solution of diazomethane to obtain a methyl ester derivative. Evaporation of the solvent, followed by purification and separation through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (175 mg, Yield: 80%) as substantially colorless oily products.
IR (neat): 2950, 2850, 1745, 1460, 1358, 1240 cm -1 .
NMR δ (CDCl 3 ): 6.25 (d, J=16 Hz, 2/5H, trans), 6.01 (d, J=11 Hz, 3/5H, cis), 5.50 (m, 4H), 4.07 (m, 1H), 3.69 (m, 1H), 3.68 (s, 3H), 2.98 (m, 1H), 1.10-2.70 (m, 17H), 0.87, 0.90 (2s, 18H), 0.03 (s, 12H).
Mass m/z (%): 588 (M + ), 532, 531, 517.
[α] D 20 =-37° (c=1.618, CHCl 3 ).
EXAMPLE 17
To a THF (1.5 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (81 mg, 0.14 mmol) was added a solution of tetrabutylammonium fluoride dissolved in THF (0.42 ml, 1M solution), and the mixture was stirred at room temperature for 16 hours. After the reaction was stopped by adding a saturated aqueous ammonium chloride solution, THF was distilled out under reduced pressure. The resultant aqueous layer was extracted with ethyl acetate, and the separated organic layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (49 mg, Yield: 100%) as colorless caramel.
IR (neat): 3400, 1740, 1430, 1160, 1090, 965 cm -1 .
NMR δ (CDCl 3 ): 6.22 (d, J=16 Hz, 1/3H, trans), 5.95 (d, J=11 Hz, 2/3H, cis), 5.13-5.74 (m, 4H, olefinic proton), 3.66 (s, 3H), 3.50-4.00 (m, 2H), 3.02 (m, 1H).
Mass m/z (%): 360 (M + ), 342 (M + -H 2 O), 324 (M + -2H 2 O), 298, 273.
[α] D 20 =-30° (c=1.16, MeOH).
EXAMPLE 18
In the method as described in Example 16, the same procedures were carried out as in Example 16 except that {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (408 mg, 0.92 mmol) was employed as the starting material to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (447 mg, Yield: 92%) as substantially colorless oily product.
IR (neat): 2950, 2850, 1744 cm -1 .
NMR δ (CDCl 3 ): 6.24 (d, J=16 Hz, 1/3H, trans), 6.01 (d, J=11 Hz, 2/3H, cis), 5.50 (m, 4H), 4.60 (m, 2H), 3.50-4.10 (m, 6H), 3.68 (s, 3H), 2.98 (m, 1H).
Mass m/z (%): 528 (M + ), 497, 443.
EXAMPLE 19
{3-(4'-Methoxycarbonyl-1'-butenyl)-6-(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (500 mg, 0.95 mmol) was dissolved in a mixed solvent of acetic aicd (4.7 ml), water (1.6 ml) and THF (1.6 ml), and heated at atmospheric temperature of 45° C. for 6 hours. After evaporation of acetic acid under reduced pressure, to the residue was added a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with saturated saline solution, and dried with anhydrous magnesium sulfate. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (308 mg, Yield: 90%) as colorless caramel. Spectrum data thereof are agreed with those of the sample obtained in Example 17.
EXAMPLE 20
{3-(4'-Methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (50 mg, 0.14 mmol) was dissolved in methanol (1.1 ml). To the solution was added a 10% aqueous sodium hydroxide solution (1.1 ml) at 0° C. After stirring at 0° C. for 16 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution under cooling. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. The extract was dried with anhydrous magnesium sulfate and distilled out the solvent to obtain {3-(4'-carboxy-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (43 mg, Yield: 89%) as colorless caramel.
IR (neat): 3350, 1715, 1085, 970 cm -1 .
NMR δ (CDCl 3 ): 6.32 (d, J=16 Hz, 1/3H), 6.04 (d, J=12 Hz, 2/3H), 5.64 (m, 3H), 5.44 (m, 1H), 3.10 (m, 1H).
REFERENCE EXAMPLE 7
To a benzene (0.9 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (48 mg, 0.081 mmol) was added RhCl(Ph 3 P) 3 (10 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by passing short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 45 mg of colorless oily product. To the product was added a THF solution (0.8 ml, 1M concentration) of tetrabutylammonium fluoride and the mixture was stirred at room temperature for 12 hours to remove silyl ether. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonylbutyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0] oct-2-ene} (20 mg, Yield: 69%).
IR (neat): 3400, 2970, 2930, 2870, 1742 cm -1 .
NMR δ (CDCl 3 ): 5.60 (m, 2H), 5.33 (bs, 1H), 4.12 (m, 1H), 3.80 (m, 1H), 3.69 (s, 3H), 3.00 (m, 1H).
Mass m/z (%): 346 (M + -H 2 O), 328, 315, 302, 275, 247, 232, 199, 193, 180, 179.
REFERENCE EXAMPLE 8
{3-(4'-Metoxycarbonylbutyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (10 mg, 0.027 mmol) was dissolved in methanol (0.3 ml). To the solution was added a 10% aqueous sodium hydroxide solution (0.2 ml) at 0° C. After stirring at 0° C. for 9 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution under cooling. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. After dryness with anhydrous magnesium sulfate, followed by evaporation of the solvent to obtain [9(0)-methano-Δ 6 (9α) -PGI 1 ] (10 mg, Yield: 100%).
IR (neat): 3350, 2910, 2850, 1700, 1450, 1250 cm -1 .
NMR δ (CDCl 3 ): 5.60 (m, 2H), 5.31 (bs, 1H), 4.11 (m, 1H), 3.80 (m, 1H), 3.00 (m, 1H), 0.90 (t, J=6 Hz, 3H).
Mass (CI, NH 3 ) m/z: 368 (M + +NH 4 ).
Melting point: 73° to 79° C.
[α] D 20 =+16° (c=0.25, MeOH).
REFERENCE EXAMPLE 9
To a benzene (0.5 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (15 mg, 0.041 mmol) was added RhCl(Ph 3 P) 3 (5 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by passing short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 9 mg of colorless oily product. The thus obtained product was dissolved in methanol (0.1 ml). To the solution was added a 10% aqueous sodium hydroxide solution (0.1 ml) at 0° C. After stirring at 0° C. for 9 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution at 0° C. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. After dryness with anhydrous magnesium sulfate followed by evaporation of the solvent to obtain {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (9 mg) as colorless solid. Spectrum data thereof are agreed with those of the sample obtained in Reference example 8.
REFERENCE EXAMPLE 10
To a benzene (0.5 ml) solution of {3-(4'-carboxy-1'-butenyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (14 mg, 0.041 mmol) was added RhCl(Ph 3 P) 3 (5 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 6 mg of {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} as colorless solid. Spectrum data thereof are agreed with those of the sample obtained in Reference example 8.
REFERENCE EXAMPLE 11
To a benzene (0.9 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (47 mg, 0.081 mmol) was added RhCl(Ph 3 P) 3 (10 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by passing short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 42 mg of colorless oily product. To the product was added a THF solution (0.8 ml, 1M concentration) of tetrabutylammonium fluoride and the mixture was stirred at room temperature for 12 hours to remove silyl ether. Evaporation of the solvent, followed by purification through silica gel column chromatography to obtain {3-(4'-methoxycarbonylbutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (17 mg, Yield: 60%).
IR (neat): 3400, 2960, 2880, 1740 cm -1 .
NMR δ (CDCl 3 ): 5.61 (m, 2H), 5.32 (bs, 1H), 3.85 (m, 2H), 3.67 (s, 3H), 3.00 (m, 1H), 1.10-2.60 (m, 26H).
Mass m/z (%): 344 (M + -18), 326 (M + -36), 300, 275, 243, 232, 225, 199, 193, 183, 181, 180, 179, 141, 119, 117, 105, 93, 91, 81, 79, 69, 67, 55, 41.
REFERENCE EXAMPLE 12
{3-(4'-Metoxycarbonylbutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (10 mg, 0.027 mmol) was dissolved in methanol (0.3 ml). To the solution was added a 10% aqueous sodium hydroxide solution (0.2 ml) at 0° C. After stirring at 0° C. for 9 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution under cooling. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. After the extract was dried with anhydrous magnesium sulfate, then distilled out the solvent to obtain {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (10 mg, Yield: 100%) as colorless solids. Recrystallization from ethyl acetate-hexane of the solids yielded colorless powders having melting point of 115° to 116° C.
IR (KBr): 3430 (OH), 2960, 1700, 1655 cm -1 .
NMR δ (CDCl 3 ): 5.60 (m, 2H), 5.32 (bs, 1H), 3.90 (m, 2H), 3.00 (m, 1H), 1.00-2.70 (m, 25H).
Mass (CI, NH 3 ) m/z: 366 (M + +NH 4 )
REFERENCE EXAMPLE 13
To a benzene (0.5 ml) solution of {3-(4'-methoxycarbonyl-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (15 mg, 0.041 mmol) was added RhCl(Ph 3 P) 3 (5 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by passing short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 8 mg of colorless viscous oil. The thus obtained oil was dissolved in methanol (0.1 ml). To the solution was added a 10% aqueous sodium hydroxide solution (0.1 ml) at 0° C. After stirring at 0° C. for 9 hours, the mixture was neutralized with a 10% aqueous hydrochloric acid solution under cooling. After evaporation of methanol under reduced pressure, the residue was adjusted to pH 3 to 4 and extracted with ethyl acetate. After dryness with anhydrous magnesium sulfate followed by evaporation of the solvent to obtain {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (8 mg) as colorless solid. Spectrum data thereof are agreed with those of the sample obtained in Reference example 12.
REFERENCE EXAMPLE 14
To a benzene (0.5 ml) solution of {3-(4'-carboxy-1'-butenyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (14 mg, 0.041 mmol) was added RhCl(Ph 3 P) 3 (5 mg), and the mixture was stirred, under hydrogen atmosphere (ordinary pressure), at room temperature for an hour and then at 45° C. for 1.5 hours. After the catalyst was removed by passing short length silica gel column, the resultant residue was purifired again through silica gel column chromatography to obtain 7 mg of {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} as colorless solid. Spectrum data thereof are agreed with those of the sample obtained in Reference example 12.
EXAMPLE 21
To a toluene (3.5 ml) solution of {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (420 mg, 0.83 mmol) was added diisobutylaluminum hydride (1.25 mmol, 0.71 ml, 1.76M hexane solution) at -78° C. and the mixture was stirred for 90 minutes. To the mixture was added dropwise methanol until the generation of hydrogen was stopped, and the mixture was diluted with ether. To the mixture was further added a saturated saline solution and stirring was continued until an organic layer became transparent. After an ether layer was separated from the mixture, extraction of an aqueous layer with ether was repeated. The separated ether layer and the extracts were combined and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purified through silica gel column chromatography to obtain {3-hydroxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy- 1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (373 mg, Yield: 88%) as substantially colorless oily product.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.47 (m, 3H), 4.13 (m, 3H), 3.73 (m, 1H), 2.97 (m, 1H).
Mass m/z: 451 (M + -57).
EXAMPLE 22
In the method as described in Example 21, the same procedures were carried out as in Example 21 except that {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo-[3.3.0]oct-2-ene} (370 mg, 0.83 mmol) was employed as the starting material to obtain {3-hydroxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (316 mg, Yield: 85%) as substantially colorless oily product.
IR (neat): 3345 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 3H), 4.55 (m, 2H), 4.10 (m, 3H), 3.50-4.00 (m, 5H), 2.98 (m, 1H).
Mass m/z: 364 (M + -84).
EXAMPLE 23
To a pyridine (1.5 ml) solution of {3-hydroxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (97 mg, 0.19 mmol) were added acetic anhydride (0.29 mmol, 27 μl) and catalytic amount of 4-dimethylaminopyridine at room temperature, and the mixture was stirred for 30 minutes under the same conditions. To the mixture was added a saturated aqueous copper sulfate solution and the mixture was extracted with ether. The separated ether layer was washed with water and then dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purified through silica gel column chromatography to obtain {3-acetoxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo-[3.3.0]oct-2-ene} (104 mg, Yield: 100%) as colorless oily product.
IR (neat): 1755 cm -1 .
NMR δ (CDCl 3 ): 5.47 (m, 3H), 4.55 (s, 2H), 4.01 (m, 1H), 3.68 (m, 1H), 2.93 (m, 1H), 2.05 (s, 3H).
Mass m/z: 493 (M + -57).
EXAMPLE 24
In the method as described in Example 23, the same procedures were carried out as in Example 23 except that {3-hydroxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cisbicyclo[3.3.0]oct-2-ene} (85 mg, 0.19 mmol) was employed as the starting material to obtain {3-acetoxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (93 mg, Yield: 100%) as substantially colorless oily product.
IR (neat): 1750 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 3H), 4.55 (m, 4H), 4.05 (m, 1H), 3.40-4.00 (m, 5H), 2.91 (m, 1H), 2.05 (s, 3H).
Mass m/z: 406 (M + -84).
EXAMPLE 25
To a suspension of cuprous iodide (163 mg, 0.85 mmol) in ethyl ether (1.5 ml) was added freshly prepared 3-butenyl lithium (1.70 mmol, 1,31 ml, 1.30M hexane solution) at -30° C., and the mixture was stirred for 30 minutes. After the mixture was cooled to -78° C., an ethyl ether (1 ml) solution of {3-acetoxymethyl-6(S)-[3'(S)-t-butyl-dimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (213 mg, 0.39 mmol) was added thereto and the mixture was stirred for an hour at the same conditions. After further continuation of stirring at room temperature for 0.5 hour, the reaction was stopped by adding a saturated aqueous ammonium chloride solution. The reaction mixture was extracted with ether, and the separated ether layer was washed with a saturated saline solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purified through silica gel column chromatography to obtain {3-(4'-pentenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1R,5R)-cis-bicyclo[3.3.0]oct-2-ene} (154 mg, Yield: 73%) as substantially colorless oily product. The thus obtained product contained about 10% of {2-(3'-butenyl)-3-methylidene-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-(1S,5S)-cis-bicyclo[3.3.0]octane}.
IR (neat): 1645 cm -1 .
NMR δ (CDCl 3 ): 5.40-6.05 (m, 1H), 5.35 (m, 2H), 5.20 (bs, about 1H), 4.90 (m, 2H), 4.00 (m, 1H), 3.60 (m, 1H), 2.90 (m, about 1H).
Mass m/z: 489 (M + -57).
EXAMPLE 26
In the method as described in Example 25, the same procedures were carried out as in Example 25 except that {3-acetoxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cisbicyclo[3.3.0]oct-2-ene} (191 mg, 0.39 mmol) was employed as the starting material to obtain {3-(4'-pentenyl)-6(S)-[ 3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (133 mg, Yield: 70%) as substantially colorless oily product. The thus obtained product contained about 10% of {2-(3'-butenyl)-3-methylidene-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-(1S,5S)-cis-bicyclo[3.3.0]octane}.
IR (neat): 1645 cm -1 .
NMR δ (CDCl 3 ): 5.40-6.05 (m, 1H), 5.35 (m, 2H), 5.20 (bs, about 1H), 4.90 (m, 2H), 4.55 (m, 2H), 4.00 (m, 1H), 3.40-3.70 (m, 5H), 2.90 (m, about 1H).
Mass m/z: 402 (M + -84).
EXAMPLE 27
In the method as described in Example 21, the same procedures were carried out as in Example 21 except that {3-formyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (418 mg, 0.83 mmol) was employed as the starting material to obtain {3-hydroxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (372 mg, Yield: 86%) as substantially colorless oily product.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 3H), 4.13 (m, 3H), 3.70 (m, 1H), 2.98 (m, 1H).
Mass m/z: 449 (M + -57).
EXAMPLE 28
In the method as described in Example 21, the same procedures were carried out as in Example 21 except that {3-formyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[ 3.3.0]oct-2-ene} (368 mg, 0.83 mmol) was employed as the starting material to obtain {3-hydroxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (306 mg, Yield: 83%) as substantially colorless oily product.
IR (neat): 3345 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 3H), 4.55 (m, 2H), 4.10 (m, 3H), 3.50-4.00 (m, 5H), 2.98 (m, 1H).
Mass m/z: 362 (M + -84).
EXAMPLE 29
In the method as described in Example 23, the same procedures were carried out as in Example 23 except that {(3-hydroxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (96 mg, 0.19 mmol) was employed as the starting material to obtain {3-acetoxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (103 mg, Yield: 100%) as colorless oily product.
IR (neat): 1755 cm -1 .
NMR δ (CDCl 3 ): 5.47 (m, 3H), 4.54 (s, 2H), 4.00 (m, 1H), 3.68 (m, 1H), 2.92 (m, 1H), 2.05 (s, 3H).
Mass m/z: 492 (M + -57).
EXAMPLE 30
In the method as described in Example 23, the same procedures were carried out as in Example 23 except that {3-hydroxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (84 mg, 0.19 mmol) was employed as the starting material to obtain {3-acetoxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (91 mg, Yield: 100%) as substantially colorless oily product.
IR (neat): 1750 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 3H), 4.55 (m, 4H), 4.05 (m, 1H), 3.40-4.00 (m, 5H), 2.91 (m, 1H), 2.05 (s, 3H).
Mass m/z: 404 (M + -84).
EXAMPLE 31
In the method as described in Example 25, the same procedures were carried out as in Example 25 except that {3-acetoxymethyl-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (211 mg, 0.39 mmol) was employed as the starting material to obtain {3-(4'-pentenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (149 mg, Yield: 70%) as substantially colorless oily product. This product also contained about 10% of a substance formed by a reaction of γ-attack.
IR (neat): 1645 cm -1 .
NMR δ (CDCl 3 ): 5.40-6.05 (m, 1H), 5.35 (m, 2H), 5.20 (bs, about 1H), 4.90 (m, 2H), 4.00 (m, 1H), 3.60 (m, 1H), 2.90 (m, about 1H).
Mass m/z: 487 (M + -57).
EXAMPLE 32
In the method as described in Example 25, the same procedures were carried out as in Example 25 except that {3-acetoxymethyl-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl- 1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (211 mg, 0.39 mmol) was employed as the starting material to obtain {3-(4'-pentenyl)-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (131 mg, Yield: 70%) as substantially colorless oily product. This product also contained about 10% of a substance formed by a reaction of γ-attack.
IR (neat): 1645 cm -1 .
NMR δ (CDCl 3 ): 5.40-6.05 (m, 1H), 5.35 (m, 2H), 5.20 (bs, about 1H), 4.90 (m, 2H), 4.55 (m, 2H), 4.00 (m, 1H), 3.40-3.70 (m, 5H), 2.90 (m, about 1H).
Mass m/z: 400 (M + -84).
REFERENCE EXAMPLE 15
To a THF (1.2 ml) solution of {3-(4'-pentenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (175 mg, 0.32 mmol) (Purity: about 90%) was added 9-BBN (0.42 mmol, 0.83 ml, 0.5M THF solution) at 0° C., and the mixture was stirred for 5 hours at the same conditions. After continuation of stirring at the room temperature for 0.5 hour, to the mixture were added a 6N NaOH aqueous solution (0.21 ml) and a 30% hydrogen peroxide aqueous solution (0.18 ml). After stirring at 60° C. for an hour, the mixture was diluted with water and extracted with ether. The separated ether layer was washed with a saturated aqueous sodium thiosulfate solution and a saturated saline solution and dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purified through silica gel column chromatography to obtain {3-(5' -hydroxypentyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (145 mg, Yield: 81%) as substantially colorless oily product.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.47 (m, 2H), 5.24 (m, 1H), 4.05 (m, 1H), 3.64 (m, 3H), 2.91 (m, 1H).
Mass m/z: 507 (M + -57).
REFERENCE EXAMPLE 16
In the method as described in Reference example 15, the same procedures were carried out as in Reference example 15 except that {3-(4'-pentenyl)-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene}(156 mg, 0.32 mmol) was employed as the starting material to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (121 mg, Yield: 75%) as substantially colorless oily product.
IR (neat): 3400 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 2H), 5.24 (m, 1H), 4.60 (m, 2H), 4.05 (m, 1H), 3.40-3.70 (m, 7H), 2.91 (m, 1H).
Mass m/z: 420 (M + -84).
REFERENCE EXAMPLE 17
To {3-(5'-hydroxypentyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-1'-trans-octenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (22 mg, 0.039 mmol) was added a tetra-n-butylammonium fluoride solution (0.3 mmol, 0.3 ml, 1M THF solution), and the mixture was stirred at room temperature for 12 hours. The mixture was diluted with a saturated saline solution and then extracted with ethyl acetate. The separated organic layer was dried with anhydrous magnesium sulfate and the solvent was distilled out therefrom. The residue was separated and purified through silica gel column chromatography (ethyl acetate:acetone =95:5) to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (13 mg, Yield: 100%) as substantially colorless viscous liquid.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.52 (m, 2H), 5.28 (bs, 1H), 4.07 (m, 1H), 3.65 (m, 3H), 2.97 (m, 1H).
Mass m/z: 318 (M + -18).
REFERENCE EXAMPLE 18 {3-(5'-hydroxypentyl)-6(S)-[3'(S)-tetrahydropyranyloxy-1'-trans-octenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (20 mg, 0.040 mmol) was dissolved in a mixed solvent (1 ml) of acetic acid-water-THF (3:1:1), and the mixture was heated at 60° C. for 3 hours. After the solvent was removed by distillation, to the residue was added small amount of a saturated aqueous sodium hydrogencarbonate solution and the mixture was extracted with ethyl acetate. The separated organic layer was dried with anhydrous magnesium sulfate. After evaporation of the solvent, the residue was purified through silica gel column chromatography to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (13 mg, Yield: 100%) as substantially colorless viscous liquid. Each of the spectrum data thereof are completely agreed with those of the sample obtained in Reference example 17.
REFERENCE EXAMPLE 19
{3-(5'-Hydroxypentyl)-6(S)-[3'(S)-hydroxy-1'-trans-octenyl]- 7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (12 mg, 0.036 mmol) was dissolved in a mixed solvent of acetone-H 2 O (1:4, 1.5 ml), and to the solution were added Pt, as a catalyst, which was obtained by reducing PtO 2 and sodium hydrogencarbonate (3.2 mg, 0.038 mmol), and the mixture was stirred at 60° C. for 24 hours under oxygen gas stream. After the catalyst was removed by filtration and the mixture was neutralized with a 10% HCl aqueous solution, acetone was removed by distillation. The residue was made acidic solution again with the addition of a 10% HCl aqueous solution, the mixture was sufficiently extracted with ethyl acetate. The extract was dried with anhydrous magnesium sulfate and distilled out the solvent to obtain (+)-9(0)-methano-Δ 6 (9α) -PGI 1 (8 mg, Yield: 61%) as substantially colorless viscous oily product.
IR (neat): 3350, 1700, 1450, 1250 cm -1 .
NMR δ (CDCl 3 ): 5.60 (m, 2H), 5.31 (bs, 1H), 4.11 (m, 1H), 3.80 (m, 1H), 3.00 (m, 1H), 0.90 (t, J=6 Hz, 3H).
Mass (CI, NH 3 ) m/z: 368 (M + +NH 4 ).
[α] D 20 =+16° (c=0.25, MeOH).
REFERENCE EXAMPLE 20
In the method as described in Reference example 15, the same procedures were carried out as in Reference example 15 except that {3-(4'-pentenyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (173 mg, 0.32 mmol) was employed as the starting material to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (140 mg, Yield: 80%) as substantially colorless oily product.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.47 (m, 2H), 5.24 (m, 1H), 4.05 (m, 1H), 3.64 (m, 3H), 2.91 (m, 1H).
Mass m/z: 505 (M + -57).
REFERENCE EXAMPLE 21
In the method as described in Reference example 16, the same procedures were carried out as in Reference example 16 except that {3-(4'-pentenyl)-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (154 mg, 0.32 mmol) (purity: about 90%) was employed as the starting material to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (115 mg, Yield: 72%) as substantially colorless oily product.
IR (neat): 3400 cm -1 .
NMR δ (CDCl 3 ): 5.45 (m, 2H), 5.24 (m, 1H), 4.60 (m, 2H), 4.05 (m, 1H), 3.40-3.70 (m, 7H), 2.91 (m, 1H).
Mass m/z: 418 (M + -84).
REFERENCE EXAMPLE 22
In the method as described in Reference example 17, the same procedures were carried out as in Reference example 17 except that {3-(5'-hydroxypentyl)-6(S)-[3'(S)-t-butyldimethylsilyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-t-butyldimethylsilyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (21 mg, 0.039 mmol) was employed as the starting material to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (12 mg, Yield: 100%) as substantially colorless viscous liquid.
IR (neat): 3350 cm -1 .
NMR δ (CDCl 3 ): 5.52 (m, 2H), 5.28 (bs, 1H), 4.07 (m, 1H), 3.65 (m, 3H), 2.97 (m, 1H).
Mass m/z: 316 (M + -18).
REFERENCE EXAMPLE 23
In the method as described in Reference example 18, the same procedures were carried out as in Reference example 18 except that {3-(5'-hydroxypentyl)-6(S)-[3'(S)-tetrahydropyranyloxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-tetrahydropyranyloxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (19 mg, 0.040 mmol) was employed as the starting material to obtain {3-(5'-hydroxypentyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (12 mg, Yield: 100%) as substantially colorless viscous liquid. Each of the spectrum data thereof are completely agreed with those of the sample obtained in Reference example 22.
REFERENCE EXAMPLE 24
In the method as described in Reference example 19, the same procedures were carried out as in Reference example 19 except that {3-(5'-hydroxypentyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (11 mg, 0.036 mmol) was employed as the starting material to obtain {3-(4'-carboxybutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene} (7 mg, Yield: 60%) as colorless white solid.
Melting point: 115° to 116° C. (recrystallized from ethyl acetate-n-hexane)
IR (neat): 3430, 2960, 1700, 1655 cm -1 .
NMR δ (CDCl 3 ): 5.62 (m, 2H), 5.32 (bs, 1H), 3.90 (m, 2H), 3.00 (m, 1H).
Mass (CI, NH 3 ) m/z: 366 (M + +NH 4 ).
TEST EXAMPLE 1
In the compounds synthesized by the method as described above, 9(0)-methano-Δ 6 (9α) -PGI 1 , for example, has a biological activity as mentioned below. When the rabbit serum was employed, it depressd a cohesion of platelets to be induced by adenosine diphosphate (ADP) at a potency of 1/10 to that of PGI 2 , and it showed a potency of 1/2 to that of PGI 2 when the human blood was employed. As for the effects to the blood pressure, when rat was examined, it showed the same effect as that of PGI 2 and showed blood pressure depressing action at a dosage of 0.1 μg/kg. An effect to the heart stroke frequencies thereof are almost the same as that of PGI 2 , and increasing of the heart stroke frequencies were observed at a dosage of 1 μg/kg thereof in an experiment by using rats. As for an anti-fester action, it showed an activity at a low concentration of 10 -6 M in an experiment by using rabbit stomach, and it was the same strength as that of PGE.sub. 2. Cytotoxicity thereof are extremely weak and IC 50 =5 μg/ml.
TEST EXAMPLE 2
(+)-3-(4'-Carboxybutyl)-6(S)-[3'(S)-hydroxy-3'-cyclopentyl-1'-trans-propenyl]-7(R)-hydroxy-(1S,5S)-cis-bicyclo[3.3.0]oct-2-ene has biological activities as shown below. By using rabbit stomach epithelial cells, an experiment according to the method of Murota et. al. [K. Matsuoka, Y. Mitsui, and S. Murota, J. Pharm. Dyn., 5, 991 (1982)] was carried out to obtain the result that it showed a remarkable anti-fester action at a low concentration of 0.5×10 -6 M. This effect is the same as that of PGE 2 which is representative prostaglandin having anti-fester action. The above carbacyclin derivatives has no diarrhea inductive effect whereas the PGE 2 induces heavy diarrhea. | There are disclosed bicyclo[3.3.0]octene derivatives having the following formula: ##STR1## wherein R 1 is a straight, branched or cyclic alkyl group or alkenyl group each having 5 to 10 carbon atoms; and
R 2 and R 3 are each separately a hydrogen atom or a protective group of a hydroxy group,
and process for producing the same. These compounds and the process for producing them are available for producing a 9(0)-methano-Δ6(9α)-PGI 1 . | 2 |
BACKGROUND OF THE INVENTION
This invention relates generally to weatherstrips for automotive vehicles and specifically to weatherstrips having a core metallic layer and a dissimilar outer appearance metallic layer, separated by a barrier layer.
The worldwide automotive market has become increasing competitive and consumers have become more quality conscious. In particular, Galvanic corrosion has become a significant problem for automotive weatherstrips, and specifically beltline weatherstrips. Within a beltline weatherstrip an aluminum core material is often in contact with an outer aesthetic cap made of stainless steel. Galvanic corrosion can occur since these two metals have a different solution potential wherein the stainless steel acts as a cathode and the aluminum acts as an anode. The electrically conductive solution comes from salt water caused by acid rain, road salt spray and ocean salt spray that seeps between the two metals. This type of galvanic corrosion causes staining, bleeding and often bubbling of rust beneath the synthetic rubber or cap material.
Galvanic corrosion has become more intensified due to the use of EPDM synthetic rubber, rather than the prior SBR type of synthetic rubber previously used. Currently, one method which circumvents the corrosion problem is to use similar materials for the core and for the cap members. However, this usually necessitates that stainless steel be used for both members, thus, the beltline weatherstrip becomes very expensive.
Fender or quarter panel bright strips such as those shown by reference in U.S. Pat. No. 4,709,525, entitled "Molding For Automobile Body Panels, Such As Doors", issued on Dec. 1, 1987 to Adell, and U.S. Pat. No. 4,682,442, entitled "Door Edge Guard And Method", issued on Jul. 28, 1987 to Adell, have used an insulating layer between an inner section of the metal bright strip and the steel body panel. However, these products have not suggested the use of a barrier layer between two inner dissimilar metal parts. Furthermore, these bright strips were not encapsulated within a highly conductive EPDM elastomer. Moreover, the insulating layer used for these parts consists of a polyvinyl chloride (PVC) plastic layer which cannot withstand the high vulcanizing temperatures required for weatherstrips.
SUMMARY OF THE INVENTION
In accordance with the present invention, a weatherstrip, containing two dissimilar metals, is electrically isolated by a barrier layer, thereby preventing galvanic corrosion. By isolating the cap material from the core material the galvanic reaction is reduced. The term "weatherstrip" includes beltline weatherstrips, door top moldings, back window moldings and the like. A further aspect of the present invention relates to a process by which a weatherstrip, with two dissimilar materials, separated by a barrier layer, can be manufactured. This innovative process allows a barrier film to be fed into a set of roll form dies with the core material. The barrier film may be adhesively bonded to, or separate from, the core material. This method allows for a low cost barrier material to be used in the conventional weatherstrip tools and equipment.
In an alternate embodiment of the present invention, a process to manufacture the weatherstrip comprises a system wherein the barrier film is fed into the roll form dies separately or adhesively bonded to the cap material. This method allows for better alignment of the barrier film to the cap material and for off line bonding of the barrier film to the cap material. Thus, the present invention has many advantages over the prior art and reduces the current galvanic corrosion process.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of an automobile showing the relative location of the present invention beltline weatherstrip;
FIG. 2 is a sectional view of the embodiment of the present invention beltline weatherstrip in relation to the door panels and side window glass, taken from FIG. 1;
FIG. 3 depicts the processing steps for the embodiment of the present invention beltline weatherstrip, shown in FIG. 2, wherein the barrier film material is fed into the roll form dies with the core material; and
FIG. 4 depicts the processing steps for the embodiment of the present invention beltline weatherstrip, shown in FIG. 2, wherein the barrier film material is fed into the roll form dies with the cap material.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, the beltline weatherstrip 71 of the present invention is shown at a substantially horizontal position where the movable side window glass 72 meets the door outer sheet metal panel 73; this area is known as the beltline of the vehicle. The beltline weatherstrip 71 primarily performs two functions. First, it serves as a water, ice and wind seal against the side window glass 72. Second, the beltline weatherstrip 71 serves as an aesthetic part by hiding the raw end flanges 12 of the door outer sheet metal panel 73 and the door inner sheet metal panel 74. This can best be seen in FIG. 2. The outer sheet metal panel 73 is configured as part of the outer body shape of the vehicle and includes an outer show surface which is the finished exterior of the vehicle. The inner sheet metal panel 74 faces inward toward the side window glass panel 72. The beltline weatherstrip of the present invention consists of a core which is partially encapsulated within an elastomer, an appearance cap, both of which are separated by a film barrier layer.
An elongated metallic core 75 acts as a structural support for the beltline weatherstrip 71 and the core material 75 is preferably made from a malleable aluminum material. The elongated core 75 includes a flange portion 36, a show surface attachment portion 38 and an intermediate portion 39. The flange portion 36 is configured for placement adjacent to the inner surface of the door sheet metal end flanges 12 and the intermediate portion 39 connects the show surface portion 38 with the flange portion 36. The core member 75 also contains an S-shaped compression attachment portion 37 which acts coextensively with the flange portion 36 so as to retain the beltline weatherstrip 71 onto the door metal end flanges 12.
An elastomeric synthetic rubber material 79 partially encapsulates the core material 75. A synthetic rubber finger 77 is also integrated into the beltline weatherstrip 71 thereby providing an effective weather seal against the side window glass 72. The synthetic rubber material preferably used is an ethylene-propylenediene terpolymer (EPDM) elastomer although a styrene-butadiene (SBR) material may be used. The back side of the rubber finger 77 and various hidden portions of the rubber 79 may contain adhesively bonded fibers, known as flocking 78, which allow the side window glass 72 to move freely over the rubber surfaces.
In many cases the core member 75 has an appearance cap 76 crimped onto it. This cap member 76 is made from stainless steel type 51434 and primarily serves an aesthetic function. A barrier film 80 is mounted between the core member 75 and the stainless steel cap 76. This barrier film 80 serves to prevent the stainless steel cap member 76 from contacting the aluminum core 75, thereby preventing galvanic corrosion. Although an adhesive layer may be required for the barrier film 80 to be retained in this location, the forming of the C-shaped stainless steel cap 76 upon the aluminum core 75 should be sufficient to retain the barrier film 80 in its proper location. The barrier film 80 is preferably a 0.002 inch thick strip of polyester film which may contain a pressure sensitive adhesive backing.
FIG. 3 depicts the preferred steps required to process the beltline weatherstrip 71. The barrier film 80 is held in close registry with the aluminum core 75 as they are distributed from their respective roll, 42 and 41, and are then fed through a first set of roll form dies 43. The barrier film 80 may need to be adhesively bonded to the aluminum core 75 by using a pressure sensitive adhesive. The roll form dies 43 form the aluminum core to the desired cross sectional shape. As is traditionally done, the stainless steel cap 76 is then distributed from a roll 44 and is fed into a second set of roll form dies 60 coextensively with the preformed aluminum core 75 and film 80. At this point, the roll form dies 60 crimp the cap 76 onto the aluminum core 75, whereas the barrier film 80 is trapped therebetween.
An EPDM elastomer 79 is then extruded onto the aluminum core 75, barrier 80 and cap 76, in a cross headed die 46. This, and the following steps would be known to one skilled in the art. The assembly is then placed in a curing oven 47 for vulcanization. Next, selective areas of the weatherstrip finger portion 77 and flange portion 36 are adhesively coated at step 48 and thereafter electrostatically flocked 49 with fibers. The adhesive bonded flocking 78 is cured in an oven 50 and is then cleaned and cooled in a washing station 51. At the next stage, the beltline weatherstrip 71 is cut to size at station 52. The barrier film 80 is comprised of polyester material due to the high vulcanizing temperatures required. These temperatures range between 400° and 500° Fahrenheit. Thus, corrosion insulating materials like PVC used for other applications, such as for exterior bright strips, could not withstand the normal weatherstrip manufacturing temperatures. Furthermore, the polyester film material 80 should be thick enough to withstand the pressures from the roll form dies, 43 and 60, and a thickness of at least 0.002 inches thick has been found suitable.
FIG. 4 shows an alternate process for the present invention. The aluminum core 75 is fed from a roll 41 into a first set of roll form dies 43. These roll form dies 43 create the desired cross sectional shape. Simultaneously, off line, a wide sheet of barrier film 80 is adhesively bonded to a wide sheet of stainless steel cap material 64 thereby forming an assembly 62. This assembly 62 is then sliced to the proper width at step 63 and is then fed into a second set of roll form dies 60 on the main processing line. This series of roll form dies 60 crimp the stainless steel cap 76 bonded with the barrier film 80 onto the preformed aluminum core section 75. At step 45 the EPDM elastomer is then extruded onto the core 75, barrier 80 and cap 76 assembly. Although the barrier material 80 does not cover the longitudinal ends of the stainless steel cap 76 in this alternate process, the barrier film 80 will ooze from under the cap 76 within the vulcanizing ovens 47, such that the aluminum core 75 and the ends of the stainless steel cap 76 are effectively isolated. The remaining processing steps are the same as the preferred embodiment, and are known to one skilled in the art.
It will be appreciated that the beltline weatherstrip of the present invention represents a significant quality improvement such that galvanic corrosion is reduced. Since the film barrier material effectively isolates the cap member from the core member, the galvanic reaction is thereby minimized. Furthermore, the processes by which the barrier material may be inserted between the core and cap layers is very cost effective, accurate and can be manufactured within the current tools.
While a number of specific embodiments of this weatherstrip and the processes to make such have been disclosed, it will be appreciated that various modifications may be made to this weatherstrip without departing from the present invention. For example, the beltline weatherstrip may have different cross sectional shapes such that the aesthetic cap is mounted along the intermediate portion of the core, substantially perpendicular to the door end flanges. While the construction and processes to manufacture a beltline weatherstrip have been described, a similar barrier layer and method to insert the barrier layer between two dissimilar metal members may be applied to other non-beltline synthetic rubber weatherstrips, such as to door top moldings 82, and back window moldings 84, without departing from this invention. Furthermore, while various materials have been disclosed in exemplary fashion, various other materials may of course be employed. For example, SBR, Neoprene, TPE or PVC could be used in place of EPDM. The barrier layer may also be used to separate other metals such as copper from steel or stainless steel from magnesium. It is intended by the following claims to cover these and any other departures from these disclosed embodiments which fall within the true spirit of this invention. | An automotive beltline weatherstrip engaging an end flange of a vehicle for operative sealing between a glass window and a vehicle surface. The beltline weatherstrip having a core metallic layer and a dissimilar outer appearance metallic layer, separated by a film barrier layer, thereby preventing galvanic corrosion. A further aspect of the present invention relates to processes by which the weatherstrip with two dissimilar materials, separated by a barrier layer, can be manufactured. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is directed to an improved marine drilling riser of the type which utilizes means for providing buoyant support.
2. Description of the Prior Art
A substantial amount of exploratory drilling for deposits of crude oil and natural gas situated offshore is conducted from floating vessels. Such operations normally employ a marine riser which extends between the vessel and the subsea well. The riser is formed of a number of sections of pipe connected together end to end and serves to guide the drill string into the well and conduct drilling returns back to the vessel.
The riser must be supported to prevent its buckling due to its own weight, pressure differential caused by heavy drilling fluid, and forces acting on it as a result of waves, currents and the like. Generally, such support is provided by tensioning devices positioned on the vessel which apply an axial tensile force to the riser. Because the array of tensioning devices required for very deep water would be very cumbersome, tensioning has been supplemented with external buoyancy means affixed to the riser along the length thereof, permitting use of fewer tensioners aboard the vessel.
One method of providing external buoyancy is to affix cylindrical cans to the riser pipe. The cans are closed at the top and open at the bottom, allowing compressed air to be introduced into each can to expel the water therefrom and transform it into a buoyant member. The upper ends of the cans are rigidly affixed to the riser to support the can.
Failure from overstressing or metal fatigue is a severe problem in marine risers. Stress-inducing forces are exerted on the riser by heavy drilling fluid as well as by wind, waves and currents. Buoyancy can failures experienced with drilling risers employing buoyancy cans have led to the discovery that such cans have compounded the riser stress problem by substantially increasing stress in the riser.
SUMMARY OF THE INVENTION
The present invention relates to an improved marine drilling riser of the type which utilizes external means for providing buoyant support and alleviates the problems outlined above. In accordance with the invention, a marine riser is provided which includes a plurality of pipe sections connected together in end to end relation and extending between a subsea well and a drilling vessel situated at the water surface. A plurality of buoyancy cans are positioned concentrically about the riser and are situated at selected locations spaced along the length thereof. The cans are open at the bottom and are sealably connected to the riser at their upper end by a means for substantially eliminating the transfer of bending moments between the can and the riser.
In a preferred embodiment of the invention, a can is mounted over each of a plurality of selected riser pipe sections for receiving and retaining air or other compressed gas in the annular space between the riser pipe and the wall of the can. A connector is mounted on the upper end of the can for attaching the can to the riser at the connection between two riser joints. The connector includes means for flexibly attaching the can to the riser so as to form a seal therewith. A radial restraint guide is affixed to the riser pipe inwardly of the wall of the can to prevent excessive lateral movement of the can with respect to the riser pipe.
The riser of the present invention has the advantage of reducing the stiffness a riser provided with rigidly connected buoyancy cans would otherwise have and of eliminating localized stress concentrations at the point where each can is affixed to the riser. The riser of the present invention therefore has significant advantages over systems existing heretofore.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic elevation of the riser system of the present invention extending between a floating drilling vessel and a subsea well.
FIG. 2 is a side view partly in section of a section of riser pipe having a buoyancy can affixed thereto in accordance with the preferred embodiment of this invention.
FIG. 3 is a sectional view of the flexible connection of the buoyancy can to the riser joint.
FIG. 4 is a sectional view of the lower end of the buoyant can depicting the lower lateral restraint guide.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, the letter R generally designates the riser system of the preferred embodiment of this invention with its flexibly connected buoyancy cans. The riser extends from a floating drilling vessel V downwardly to subsea well W located on the bottom 10 of a body of water 11. The vessel includes a derrick D for supporting the drill string 13, which extends downwardly through an opening 12 extending through the vessel. The riser column guides the drill string into the subsea well and provides a conduit for the drilling fluid to return to the vessel.
The upper end portion 14a of the riser is connected to a slip joint assembly 15. The slip joint assembly 15 is connected by cables 15a to the vessel and compensates for relative vertical movement between the vessel and riser. Tensioning devices, designated by numerals 16 and 17, are positioned on the vessel and are attached to a clamp 18 affixed to the lower barrel of slip joint 15. Tensioners 16 and 17 function to exert a vertical tensile load on the riser. At its lower end 14b, the riser is pivotally connected to a blowout preventer stack 20 by means of a ball joint designated by the number 19. The blowout preventer stack is in turn connected to wellhead 21 at the bottom of the body of water.
The riser is comprised of a plurality of riser sections 25 connected end to end. One of the plurality of sections 25 of riser pipe having a buoyancy can 35 attached to it is illustrated in detail in FIG. 2. The illustrated riser section includes a cylindrical conduit or pipe which has affixed to the ends thereof an upper riser connector 29 and a lower riser connector 30. Pipe section 25 is a hollow, cylindrical member having an inside diameter sufficiently large to allow the passage of the drill string 13 including a drill bit mounted on the lower end thereof.
Upper riser connector 29 includes a hub portion 29a which is welded or otherwise connected to the upper end of pipe section 25. A flange portion 29b extends radially outwardly from the hub and forms an integral part thereof. It will be appreciated, however, that it could also be welded or otherwise attached to hub 29a. The lower riser connector 30 also includes a corresponding hub portion 30a and flange portion 30b.
Conduits 31 and 32, FIG. 2, extend through flange portions 29b and 30b of the upper and lower riser pipe connectors and along the length of riser pipe section 25. Conduits 31 and 32 are aligned in parallel with the longitudinal axis of riser section and are sealed about their periphery where they extend through the upper riser connector flange portion 29b. Such sealable connection may be provided by any suitable means. The conduits may be utilized to conduct various fluids, for example, as a source of compressed air to displace water from the buoyancy cans. In addition, they may be utilized to convey hydraulic fluid to power hydraulic valve elements or operators located at the subsea well or as choke and kill lines for controlling surges in well pressure.
A cylindrical can 35 is positioned concentrically about riser pipe section 25. Connector means, designated generally as 36 (FIG. 3), interconnect buoyancy can 35 and upper riser connector 29 for sealing the upper end of buoyancy can 35 against loss of fluid and for limiting the transfer of bending moments between the buoyancy can and the riser pipe 25. Buoyancy can 35 is normally a hollow cylindrical member and is generally made of metal. It is to be noted, however, that other shapes of buoyancy cans could also be employed. For example, the can may be swagged and have more than one diameter. The internal diameter of the can 35 is sized to provide an annular space S between the riser section 25 and the wall of the buoyancy can to provide the desired amount of buoyancy. The connector means 36 provides an essentially moment free, sealed connection between upper riser connector 29, and in particular the flanged portion 29b thereof, and buoyancy can 35 so that compressed air or other buoyancy inducing fluid can be received and retained within annular space S. Since the air or other compressed gas is not introduced into the buoyancy cans until they are submerged, the pressure of the fluid piped into the annular space must be sufficient to overcome the hydrostatic head of the water at the particular depth of each buoyancy can 35.
Connector means 36 includes an annular, flexible gasket mounted on the top rim 35d of buoyancy can 35. Preferably, as shown in FIG. 3, a laminated gasket 37 is employed which includes alternate layers 37a of rubber or other suitable resilient, sealing material positioned between annular rings 37b of steel or other rigid material. The alternate layers of rubber or other flexible sealing material provide a sealed connection between flange portion 29b of the upper riser connector and top rim 35d of the buoyancy can. In addition, the layers of flexible material permit movement of the cylindrical can with respect to riser pipe section 25. In this manner, connector means substantially eliminate the transfer of bending moments between the riser and the buoyancy can. This in turn serves to reduce the stress level in the riser pipe and thus increase its service life.
The upper end 35a of the buoyancy can 35 includes a series of circumferentially spaced, threaded bolt holes 35b extending therein. Flange 29b of the upper riser connector and the annular gasket 37 include a group of circumferentially spaced openings 38 and 39 that align with the threaded holes 35b in the upper end 35a of the buoyancy can. Apertures 38, 39 and 35b are adapted to receive connector bolts 40 which extend through the openings 38 and 39 into threaded engagement with the opening 35b. The diameter of the opening 38 through the flange is larger than that of the bolt to allow for limited movement of the bolt shaft in response to movement of buoyancy can 35. Thus, limited movement of the buoyancy can 35 can be tolerated without imposing significant bending stresses on the bolt shaft, thereby increasing the life of bolts 40.
The annular, elastic connecting gasket 37 substantially prevents the transfer of bending moments between the riser and the buoyancy can 35 by permitting limited pivotal movement or flexure of the cylindrical can 35 with respect to the upper riser connector flange 29b. For example, in response to a force applied in the direction of arrow 41 to the right-hand side of can 35, the buoyancy can 35 will tilt in the direction 41 of the force. The annular, resilient gasket 37 is thus compressed on the left-hand side thereof, permitting the flexing of the buoyancy can. The compression of the resilient gasket 37 prevents the transfer of any substantial bending moment to the riser.
Situated just below upper riser connector 29 is a radially extending, lateral restraint guide 29c. It may be welded or otherwise attached to hub portion 29a of the upper riser connector or be directly connected to the riser pipe. The lateral restraining guide 29c provides an outer restraining surface 29d which is positioned a predetermined distance away from an inner surface 35d of the upper end of the buoyancy can. The distance between inner surface 35d of the can and the outer surface of the lateral restraint guide 29c is sufficient to allow only limited lateral movement of the buoyancy can, thereby protecting the integrity of the annular gasket 37 and preventing failure of connector bolt 40. Similarly, flange portion 30b of the lower riser connector 30 includes an outer, restraining surface 30c which is positioned a predesignated distance away from the inner surface 35e of the buoyancy can in order to limit lateral movement of the lower end of the buoyancy can.
The upper riser connector 29 further includes a downwardly facing, annular shoulder or offset 50 which is adapted to receive a spider or other gripping device for supporting the entire riser.
The foregoing disclosure and description of the invention are illustrative and explanatory thereof, and various changes in the size, shape and materials as well as in the details of the illustrated construction may be made without departing from the spirit of the invention. | An improved marine riser is described which is comprised of a plurality of conduit sections joined together end to end. Buoyancy cans for retaining a compressed gas are flexibly connected to the riser at selected locations along its length and form a fluid tight seal therewith. | 4 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of and priority to U.S. Provisional Application Ser. No. 61/445,700, filed on Feb. 23, 2011, the entire contents of which are incorporated herein by reference.
BACKGROUND
[0002] 1. Technical Field
[0003] The present disclosure relates generally to medical devices. More specifically, the present disclosure relates generally to systems and methods for controlled tissue compression.
[0004] 2. Background of the Related Art
[0005] Some surgical procedures require the compression, e.g., clamping, of a patient's tissue. Such procedures may include, e.g., anastomosing, stapling, and resecting of tissue. For example, where cancerous tissue is identified in a patient's gastrointestinal tract, the cancerous tissue may need to be surgically removed. Where, for example, the cancerous tissue is located on the colon and is accessible by surgical instrumentation, the surgeon may make an incision in the patient's abdomen to allow access to the bowel. The surgeon may then use a linear cutting and stapling device, such as that described in U.S. patent application Ser. No. 12/235,362, filed Sep. 22, 2008 (U.S. Patent Publication No. 2009/0101692), which is expressly incorporated herein in its entirety by reference thereto, to cut and staple the colon tissue on opposite sides of the cancerous portion to be removed. In this procedure, the colon is externally clamped (e.g., between opposed jaws) to compress the tissue. While the tissue is compressed, a cutter and a stapler are activated to make a linear cut and apply typically two linear rows of staples in the areas adjacent the cut. The stapling thus closes both open ends of the portion of the bowel to be removed, as well as providing a temporary closure of the two cut ends of the bowel. This closure limits exposure of the surrounding tissue to the interior of the bowel, thus limiting the risk of infection. After the cutting and stapling procedure, the cancerous portion of tissue may be removed from the patient's body.
[0006] After the resection of the cancerous tissue, the surgeon may employ an anastomosing and stapling device, e.g., a circular stapler/cutter, such as that described in U.S. patent application Ser. No. 10/785,682, filed Feb. 24, 2004 (U.S. Pat. No. 7,342,983), which is expressly incorporated herein in its entirety by reference thereto. During this procedure a head portion is positioned within the colon adjacent one of the cut ends and a base or shaft portion is positioned within the colon adjacent the other cut end. The head portion and the base portion may be coupled via a shaft and/or cable that extends out of one cut end and into the other. Via this coupling, the surgeon is able to actuate the anastomosing and stapling device to draw the head portion and the base portion together. After the two cut ends of the colon contact each other, the actuation continues such that the two portions of the colon are clamped together at an annular area of contact. While clamped, the anastomosing and stapling device may be further actuated to apply an annular ring of staples into the compressed tissue. The device may also cut excess tissue disposed within the colon. The head portion and the base portion are then moved apart and the anastomosing and stapling device removed from the patient.
[0007] To achieve effective stapling in the above procedures, the tissue must be compressed to the extent that there is an adequately small tissue gap, e.g., one millimeter, between the faces of the tool. If the clamping structures of the instrument are exposed to excessive force, maintaining a uniform target tissue gap across the length of tissue to be stapled may be difficult or even impossible.
[0008] Moreover, when performing the compression, a constant closing rate (e.g., the closing rate between jaws of a linear stapler or between the head and base portion of a circular stapler/cutter) may exert a high level of pressure on the clamped tissue. This high level of pressure may result in excess tissue trauma. It is thus desirable to limit this trauma, e.g., by effectively controlling the pressure applied to the tissue.
[0009] Further, it is desirable to determine how the tissue to be clamped is responding to compression and process this information to determine clamping pressure. U.S. patent application Ser. No. 09/510,927, filed Feb. 22, 2000 (now U.S. Pat. No. 6,716,233), which is expressly incorporated herein in its entirety by reference hereto, describes apparatus and methods of using a tissue sensor to control operation of a surgical stapler.
SUMMARY
[0010] In an embodiment of the present disclosure, a surgical device is provided. The surgical device includes an end effector configured to clamp, staple or cut tissue, a motor configured to drive the end effector and a control system. The control system receives information about at least one tissue property and selects a tissue management mode based on the at least one tissue property. The control system controls the motor based on the selected tissue management mode.
[0011] The surgical device may also include an indicator that provides a clinician with a status of a tissue gap range of the end effector and a sensor array configured to detect at least one tissue property. The sensor array may detect at least one tissue property by measuring the current draw on the motor or the dwell effect at the end effector. The sensor array may also assess tissue properties by taking measurements such as pulse oximetry, tissue oxygen saturation or tissue impedance. The dwell effect occurs as the jaws remain at a static pressure for a period and fluids escape from the tissue cells, allowing the tissue to relax.
[0012] The tissue management modes that can be selected by the surgical device include a constant torque profile, a modulated torque profile, a maximum torque profile or a manual override mode. The control system applies a constant signal to the motor in the constant torque profile or a periodic signal to the motor in the modulated torque profile. In the maximum torque profile, the powered surgical instrument fires at a speed that is faster than the speed of firing in the constant torque profile, the modulated torque profile or the manual override mode. In the manual override mode, the user manually controls the motor. Typically, pressure during tissue clamping will be a function of the motor torque.
[0013] In another embodiment of the present disclosure, a method for applying a staple by a powered surgical instrument is provided. The method includes the steps of providing a surgical instrument having an end effector that is powered by a motor, inputting a tissue type and/or disease type to determine an initial clamping or tissue management mode, clamping tissue using the end effector driven by the motor, detecting at least one tissue property of the clamped tissue, determining if a desired tissue gap range is achieved by the end effecter, if necessary, selecting an additional clamp mode to iteratively adjust clamping to achieve the desired tissue gap, and firing the powered surgical instrument to apply staples to the clamped tissue once the desired tissue gap has been achieved.
[0014] The method may also include the step of providing an indication of a status of a tissue gap range. The tissue property may be detected by measuring the current draw on the motor or measuring a dwell effect at the end effector.
[0015] Selecting the clamping or tissue management mode may be based on the tissue property of the clamped tissue detected or be performed by a clinician. The tissue management modes that can be selected by the surgical device include a constant torque profile, modulated torque profile or maximum torque profile. A manual override mode may allow the user to select a tissue management mode.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The above and other aspects, features, and advantages of the present disclosure will become more apparent in light of the following detailed description when taken in conjunction with the accompanying drawings in which:
[0017] FIG. 1 is a perspective view of a powered surgical instrument according to an embodiment of the present disclosure;
[0018] FIG. 2 is a system block diagram of the powered surgical instrument according to an embodiment of the present disclosure;
[0019] FIG. 3 is a flow chart depicting operation of the powered surgical instrument according to an embodiment of the present disclosure; and
[0020] FIG. 4 is a flow chart depicting an indicator system according to an embodiment of the present disclosure.
DETAILED DESCRIPTION
[0021] Particular embodiments of the present disclosure are described hereinbelow with reference to the accompanying drawings; however, it is to be understood that the disclosed embodiments are merely exemplary of the disclosure and may be embodied in various forms. Well-known functions or constructions are not described in detail to avoid obscuring the present disclosure in unnecessary detail. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present disclosure in virtually any appropriately detailed structure.
[0022] Like reference numerals may refer to similar or identical elements throughout the description of the figures. As shown in the drawings and described throughout the following description, as is traditional when referring to relative positioning on a surgical instrument, the term “proximal” refers to the end of the apparatus which is closer to the user and the term “distal” refers to the end of the apparatus which is farther away from the user. The term “clinician” refers to any medical professional (i.e., doctor, surgeon, nurse, or the like) performing a medical procedure involving the use of embodiments described herein.
[0023] A powered surgical instrument, e.g., a surgical stapler, in accordance with the present disclosure is referred to in the figures as reference numeral 100 . Powered surgical instrument 100 is merely an example of a surgical instrument that utilizes the embodiments of the present disclosure described herein and therefore, is not intended to limit the present disclosure to this one particular embodiment of a surgical instrument.
[0024] Referring initially to FIG. 1 , powered surgical instrument 100 includes a housing or handle 110 , an endoscopic portion 140 defining a longitudinal axis A-A extending therethrough, and an end effector 160 , defining a longitudinal axis B-B (illustrated substantially aligned with axis A-A in FIG. 1 ) extending therethrough. Endoscopic portion 140 extends distally from housing 110 , and clamping mechanism or end effector 160 is disposed adjacent a distal portion 142 of endoscopic portion 140 . End effector 160 is used to clamp, staple and/or cut tissue disposed therebetween.
[0025] Powered surgical instrument 100 may include a control system designated generally as 200 in FIG. 2 . Control system 200 may be integrated in housing 110 of powered surgical instrument 100 or some of the components may be provide in a stand-alone unit. Control system 200 includes a processor 202 , an input device 204 , a display 206 , a memory 208 , an indicator 210 , a motor 212 and a sensor array 214 .
[0026] Processor 202 may be an integrated circuit or may include analog and/or logic circuitry that may be used to: execute instructions according to inputs provided by the input device 204 or sensor array 214 ; execute instructions according to a program provided in memory 208 ; and/or control motor 212 thereby controlling the end effector 160 to clamp, staple and/or cut tissue therebetween.
[0027] Input device 204 may include a keyboard, a touchscreen input device, switches and/or buttons to control operation of the powered surgical instrument 100 . Input device 204 may be used to: select between tissue management modes; control end effector 160 ; apply a staple or clamp; and input tissue properties such as tissue type and/or disease.
[0028] Display 206 may include a liquid crystal display, a light emitting diode display or the like. Display 206 may output a status of the powered surgical instrument, the measured tissue properties, the number of staples/clips applied, etc.
[0029] Control system 200 may also include an indicator 210 that may include at least one light emitting diode (LED) to indicate whether a tissue gap range, between the jaws of end effector 160 , has been met. Indicator 210 may include a single multi-color LED or separate LEDs for red, yellow and green. The red LED may indicate a malfunction, a yellow LED may indicate that a tissue gap range has not been met and a green LED may indicate that the tissue gap range has been met. Additionally, an LED may be pulsed to indicate additional information. For instance, a pulsing yellow LED can indicate that an additional clamping cycle is being performed.
[0030] Sensor array 214 determines tissue properties by detecting the current draw on motor 212 or a dwell effect at end effector 160 . The detected tissue properties are used to determine a clamping or tissue management mode, a tissue gap range, firing parameters, a speed of the motor, a modulation/pulse of the motor, deployment of the staples, etc. The tissue properties are used as an input to the iterative adjustment of the clamping pressure and duration for a tissue management mode.
[0031] Memory 208 may be a volatile type memory (e.g., RAM) and/or non-volatile type memory (e.g., flash media, disk media, etc.) that stores programs or sets of instructions for the operation of the powered surgical instrument 100 .
[0032] Such programs include a number of tissue management modes that may be used to clamp tissue in order to apply a staple or clip to the tissue grasped by end effector 160 . The tissue management modes are selected to apply an atraumatic stress or strain to the tissue by varying the compression of the tissue. The tissue management modes include a constant torque profile, a modulated torque profile, a maximum torque profile and a manual override mode. The tissue management modes may be automatically selected based on detected tissue parameters and/or tissue type and disease type inputted by a clinician or the tissue management mode may be selected by a clinician.
[0033] When a constant torque profile is selected, the powered surgical instrument 100 uses controlled tissue compression to apply constant rate if strain to tissue during the clamp, dwell and firing stages to optimize tissue gap and staple formation by applying a constant signal to motor 212 from processor 202 . The parameters used to control the motor 212 and/or end effector 160 in the constant torque profile may be based on a desired speed of firing of the surgical instrument 100 or the type of tissue grasped by end effector 160 .
[0034] The modulated torque profile applies pulsating or periodic strain energy to tissue by applying a periodic signal to motor 212 . More specifically, processor 202 applies a pulse width modulated signal (PWM) or any other periodic signal to the motor to achieve an optimized compression profile, i.e., minimum tissue gap (maximum strain) with minimum tissue trauma (minimum stress). The optimized compression profile may vary for different tissue types and/or disease types. The signal from processor 202 may be predetermined and stored in a memory. Alternatively, the signal outputted by processor 202 may be determined by performing a current slope analysis on the current detected from the motor, initial tissue thickness T 0 , initial clamped tissue thickness T 1 and total strain/energy.
[0035] When the tissue management mode is set for operation in the maximum torque profile, the surgical instrument 100 fires relatively faster than the other modes of operation. While in the maximum torque profile, surgical instrument 100 fires relatively faster at the beginning and at the end of the stroke where device stresses are relatively lower. When the tissue management mode is set to operate in the manual override mode, the clinician can manually control the motor of surgical instrument 100 to achieve the desired tissue gap of end effector 100 and to manually fire the surgical instrument 100 .
[0036] Memory 208 may also store correlation tables to correlate tissue type and disease type to the requisite tissue gap range and firing parameters that need to be achieved to successfully apply a staple or clip to tissue.
[0037] FIG. 3 depicts a flow chart describing an operation of the control system 200 of powered surgical instrument 100 . As shown in FIG. 3 , a clinician starts, “powers-up” or “turns on” the powered surgical instrument 100 in step 300 . A clinician enters the tissue type and/or disease type in step 305 using input device 204 . The clinician then positions end effector 160 onto the desired tissue and an initial clamping (tissue management) mode is determined. Then, in step 315 , end effector 160 clamps the desired tissue and determines tissue properties such as initial thickness, density, initial clamped thickness, etc. in step 320 . Processor 202 , then, in step 325 , determines if the tissue gap range is met for the particular tissue type. If the gap range is met, the control system 200 proceeds to step 370 .
[0038] In step 325 , if the gap range is not met, the tissue gap and tissue properties are evaluated by processor 202 to determine if additional clamping is beneficial. If it is, the gap range and tissue properties are used to determine a new clamping mode in step 327 . The iterative clamping and evaluation process then returns to step 315 and is continued until an optimum gap range is met or it is determined that the tissue is unsuitable for the selected range in which instance the powered surgical instrument 100 prompts the clinician with a suggestion if a different reload or end effector (loaded with a different sized staple) should be used. If the clinician selects a different reload or end effector, then the powered surgical instrument 100 is reloaded in step 340 and proceeds to step 315 to clamp tissue.
[0039] If the clinician does not select a different reload or end effector, the clinician may select a manual override mode in step 345 . If the user selects the manual override mode, the powered surgical instrument 100 is placed in the manual override mode in step 350 .
[0040] Alternatively, the process proceeds to step 355 to select a tissue management mode. The tissue management mode may be automatically selected by processor 202 based on the inputted tissue type, disease type, and/or tissue properties or selected by the clinician. Based on the selection of the tissue management mode, the powered surgical instrument 100 may enter the constant torque profile of step 362 , modulated torque profile of step 364 or the maximum torque profile of step 366 . Then the control system 200 proceeds to step 370 where a determination is made as to whether a staple should be applied. This determination may be made by processor 202 or by the clinician. If the staple should be applied, then in step 375 , the control system 200 controls the powered surgical instrument 100 to apply the staple. If the staple is not applied, the control system 200 ends the procedure (step 380 ) or restarts to apply a subsequent staple (step 300 ).
[0041] FIG. 4 depicts a flow chart describing an operation of the indicator system of the powered surgical instrument 100 . The powered surgical instrument 100 is started in step 400 and the tissue type and/or disease is entered in step 405 . Processor 202 then uses one of the correlating tables stored in memory 208 to determine the tissue gap range for the red-yellow-green indicator 210 . The tissue gap range is measured in step 415 . If an error is determined or the tissue gap range exceeds an upper limit, the process proceeds to step 430 and the red indictor is illuminated. If there is no error or the tissue gap range does not exceed an upper limit, the process proceeds to step 435 . If the tissue gap range is not in the acceptable range but it does not exceed the upper limit, the yellow indicator is illuminated in step 440 . If the tissue gap range is met, the process proceeds to step 445 and the green indicator is illuminated.
[0042] It should be understood that the foregoing description is only illustrative of the present disclosure. Various alternatives and modifications can be devised by those skilled in the art without departing from the disclosure. Accordingly, the present disclosure is intended to embrace all such alternatives, modifications and variances. The embodiments described with reference to the attached drawing figs. are presented only to demonstrate certain examples of the disclosure. Other elements, steps, methods and techniques that are insubstantially different from those described above and/or in the appended claims are also intended to be within the scope of the disclosure. | A surgical instrument is provided including an end effector configured to clamp, staple or cut tissue tissue, a motor configured to drive the end effector and a control system. The control system is configured to receive information about at least one tissue property and select a tissue management mode based on the at least one tissue property. The control system controls the motor based on the selected tissue management mode. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of (1) U.S. Provisional Patent Application Ser. No. 61/689,468, filed Jun. 6, 2012, and entitled “Physical Design Criteria for Active Blast Countermeasure System” and (2) U.S. Provisional Patent Application Ser. No. 61/689,471, filed Jun. 6, 2012, and entitled “Active Blast Countermeasure System,” the entire contents of both of which applications are incorporated herein by this reference.
FIELD OF THE INVENTION
[0002] This invention relates to systems and methods for actively countering forces experienced by an object or person and more particularly, although not exclusively, to systems and methods for actively countering forces experienced by a manned (or unmanned) vehicle upon encountering blast waves of a mine or other explosive device or other undesired forces.
BACKGROUND OF THE INVENTION
[0003] U.S. Patent Application Publication No. 2012/0239247 of Eridon, whose contents also are incorporated herein by this reference, purports to disclose “systems and methods for mitigating the effects of sudden accelerative forces on vehicles due to, for example, land mines and improvised explosive devices (IEDs).” See Eridon Application, p. 1, ¶0002. Described generally in the Eridon Application is such a system having sensors, a control system, countermeasures, and a human interface. According to the Eridon Application, the control system,
which is communicatively coupled to the plurality of sensors and countermeasures, is configured to determine the dynamic response of [a] vehicle based on the set of acceleration signals, then determine whether mitigation is required based on the dynamic response of the vehicle—e.g. whether the dynamic response of the vehicle is likely to cause harm to occupants of the vehicle. If it is determined that mitigation is required, [the] control system produces one or more countermeasure signals selected to at least partially counteract the dynamic response . . . . Countermeasures then activate in response to the one or more countermeasure signals, thereby at least partially counteracting the dynamic response of [the] vehicle.
See id., pp. 1-2, ¶0017 (numerals omitted).
[0005] Absent from the skeletal Eridon Application is, among other things, any discussion of numerous components of a satisfactory countermeasures system. No comprehensive trigger and activation system (TAS) is described, for example, and the sole identifications of a “human interface” in the Eridon Application are a block in the diagram of its FIG. 1 and the statement that it may include “any combination of processors, memory, storage, displays, [and] input devices.” See id., p. 3, ¶0029. Further, the only sensor detail provided in the Eridon Application relates to a particular piezoresistive accelerometer sold by a company called Measurement Specialties, and the countermeasures identification is limited to, generically, “an explosive or a propellant” possibly provided by DuPont. See id., ¶¶0027-28.
SUMMARY OF THE INVENTION
[0006] The present invention seeks to supply multiple novel components and techniques for creating active countermeasures systems deployable under a wide variety of hostile and other conditions. An exemplary TAS may, for example, comprise any or all of a first responder unit (FRU), a control display assembly (CDA), processors, sensors, and an electronic safe and arm device (ESAD). Each component assembly may be incorporated into a line replaceable unit (LRU) if desired, although such incorporation is not necessary.
[0007] Together with appropriate countermeasures, the TAS may be used to protect crew members of a vehicle from injury or death caused by, for example, IED or mine blasts or vehicle collisions or rollovers. Systems of the invention additionally may record event or damage information (for maintenance, evaluation, or otherwise) or transmit it remotely to alert other vehicles or headquarters operations of impending danger. The Global Positioning System (GPS) or any other suitable locator system may be used in connection with the invention.
[0008] The FRU is configured to allow personnel outside a vehicle to disable the countermeasures of the vehicle when appropriate to do so. Should personnel within the vehicle be injured or trapped, for example, first responders may need to breach the vehicle hull or otherwise attempt to enter the vehicle for rescue purposes. Because in some cases these actions could risk activation of any undeployed countermeasures, to avoid further risk to life and property first responders desirably may disable the countermeasures before acting. Preferably (although not necessarily) at least one FRU is mounted near the front or rear of the vehicle so as to be accessed externally thereof; a locking cover or other structure may be provided to reduce the possibility of inadvertent or improper disabling of the countermeasures.
[0009] The CDA is intended to allow crew of a vehicle to monitor and control status of the countermeasures systems. It preferably provides visual indication of system status, although aural, tactile, or other status indications may be provided alternatively or additionally. Equally preferably, the CDA comprises multiple switches necessarily operated in certain sequences and at certain time intervals to reduce risk of unintended arming or disarming of the countermeasures by the vehicle crew. The switches, further, beneficially may have differing actuating mechanisms, although such differing mechanisms are not required.
[0010] One or more processors may be utilized as part of each countermeasures system of the present invention. Preferably the processors are dual-core, allowing for parallel processing to occur. Data buses may transfer signals to and from the processors, which also may communicate electrically with a system interface chip (integrated circuit). Processors may control, provide information to, or receive information from, any or all of the FRU, CDA, and ESAD, vehicle sensors, and vehicle safety equipment such as airbags, active seat controls, intelligent clothing, seatbelt pretensioners, etc.
[0011] Sensors associated with the present invention may sense any or all of pressure, angular movement rate, acceleration, strain (deformation), force, displacement, velocity, or electric or magnetic field strength. Because the sensors may be deployed in electrically-noisy environments, signals from the sensors may be encoded using, for example, Manchester coding principles. Preferably, multiple sensors are used on each vehicle, with at least some not co-located with others. If desired, countermeasures deployment may be conditioned on certain signal types and durations being received from multiple non-co-located sensors.
[0012] The ESAD functions to arm and initiate countermeasures upon command of a processor. Like various other aspects of the inventive systems, the ESAD preferably “fails safe”—i.e. if it is non-functional, it enters or reverts to a mode in which countermeasures cannot activate. Fuze cord or any other suitable material may connect the ESAD to the countermeasures.
[0013] Countermeasures themselves may be of varying types yet remain consistent with the present invention. Advantageously, however, countermeasures may include cartridges into which ejectable masses and charges are loaded. Currently preferred ejectable masses are predominantly solids (as opposed to liquids or gases), with preferred solids either being disintegrable or comprising multiplicities of disintegrated particles. If so, the likelihood of serious injury to a bystander impacted by a portion of the ejected mass may be reduced.
[0014] Cartridge countermeasures may be placed in barrels mounted to or otherwise connected or attached to vehicles. The barrels may be constructed in sets or individually as desired and configured to receive cartridges in any manner allowing initiation of the propellant. In some versions of the invention, banks of barrels are mounted at the four corners of the roof of a vehicle. Alternatively or additionally, barrels may be mounted on vehicle sides, fronts, or rears. Presently preferred in some versions is that barrels not be placed on the vehicle undercarriage, although such placement could occur in other versions. Because the cartridges are separate from the barrels, the cartridges may be transported apart from the barrels and loaded only when needed, further reducing risk of undesired countermeasure deployment.
[0015] It thus is an optional, non-exclusive object of the present invention to provide systems and methods for countering at least certain undesired forces acting on a vehicle.
[0016] It is another optional, non-exclusive object of the present invention to provide systems and methods for devising countermeasures systems deployable under a wide variety of conditions.
[0017] It is also an optional, non-exclusive object of the present invention to provide systems and methods incorporating some or all of an FRU, a CDA, processors, sensors, and an ESAD, any of which may be incorporated into an LRU.
[0018] Numerous other objects, feature, and advantages of the present invention will be apparent to those skilled in relevant fields with reference to the remaining text and the drawings of this application.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 is a block diagram of aspects of a TAS consistent with the present invention.
[0020] FIG. 2 is a front elevational view of an exemplary CDA consistent with the present invention.
[0021] FIG. 3 is a partially-schematicized, cross-sectional view of portions of a countermeasure consistent with the present invention.
[0022] FIG. 4 is a partially-schematicized view of fuze or detonation cord connecting a countermeasure of the type shown in FIG. 3 to an ESAD consistent with the present invention.
[0023] FIGS. 5A-F are various views of possible configurations of countermeasures of the type shown in FIG. 3 .
[0024] FIG. 6 illustrates an exemplary algorithm for deploying one or more countermeasures of the type shown in FIG. 3 .
[0025] FIG. 7 is a perspective view of a vehicle including countermeasures of the type shown in FIG. 3 .
DETAILED DESCRIPTION
[0026] Depicted in FIG. 1 is a block diagram of an exemplary TAS 10 of the present invention. TAS 10 may include FRU 14 , CDA 18 , processor 22 , one or more sensors 26 , ESAD 30 , and one or more countermeasures 34 . Although conceivably useful wherever force-related countermeasures are desirably deployed—as to prevent vehicle rollover, for example, TAS 10 is especially designed for use in connection with a vehicle (labeled “V” in FIG. 7 ) operating in a theatre in which IEDs, mines, or other explosive devices may be present.
[0027] As illustrated in FIG. 1 , FRU 14 includes at least switch 38 . Switch 38 preferably is interposed in the main power supply line 42 of the vehicle between power supply 46 (e.g. a battery or electrical generator) and ESAD 30 to which countermeasures 34 are connected. If switch 38 is open, electricity is not available for ESAD 30 to arm the countermeasures 34 for deployment.
[0028] FRU 14 beneficially may include a box housing switch 38 and be either attached to or integrated into a hull of a vehicle so as to be accessible externally thereof. Alternatively, FRU 14 may comprise a cover for switch 38 or any other object or assembly configured to restrict access to the switch 38 . In at least some embodiments of the invention, FRU 14 will be locked, limiting access to switch 38 to those possessing an appropriate unlocking key or tool or knowing a suitable combination of symbols.
[0029] In particular, first responders to an accident or catastrophe involving the vehicle may need to breach its hull or otherwise enter its interior so as to rescue personnel or equipment contained therein. Entry activities of these first responders, or other actions impacting the vehicle, could risk activation of as-yet undeployed countermeasures 34 . Accordingly, the first responders may desire to access and open switch 38 upon arrival at the vehicle so as to reduce the possibility of countermeasures 34 deployed undesirably. Of course, persons skilled in appropriate fields of endeavor will recognize that FRU 14 is optional and in certain circumstances either may be omitted from TAS 10 or configured otherwise as described herein.
[0030] CDA 18 appears in FIGS. 1-2 . As noted in FIG. 1 , CDA 18 beneficially may—but need not necessarily—include (a) at least two safety arming features, (b) at least two manual actions, and (c) an indicator of whether countermeasures 34 are armed. CDA 18 additionally advantageously may be powered by power supply 46 (albeit perhaps after the power undergoes conditioning by power conditioner 50 ), although other sources of electricity possibly may be used instead. Outputs of CDA 18 may be connected electrically to (at least) processor 22 . Although wired connections among various components of TAS 10 typically are preferred, wireless communication among some or all of the components alternatively may occur.
[0031] CDA 18 functions to, among other things, allow crew of a vehicle to control and monitor status of TAS 10 . CDA 18 preferably is positioned in a dashboard of a vehicle with its face 54 visible to the crew and may, for example, include power switch 58 and an associated visual indicator 62 . Also depicted in FIG. 2 are arm power switch 66 and its associated visual indicator 70 , arm enable switch 74 and its associated visual indicator 78 , and plural bit status indicators 82 . Arm enable switch 74 may be covered by a pivotable or otherwise movable (or removable) cover 86 that must be moved physically in order to access the arm enable switch 74 .
[0032] In at least some versions of the invention, and assuming switch 38 is closed, TAS 10 may be initialized by closing power switch 58 (shown in FIG. 2 as a two-position toggle switch). In normal operating circumstances, closing power switch 58 illuminates associated indicator 62 , indicating to a crewmember that power switch 58 is closed so as to supply power to CDA 18 . Closing power switch 58 also causes processor 22 to initiate a power-on self-test (POST), with arm power switch 58 and arm enable switch 74 preferably remaining inactive at least until the POST is complete.
[0033] During the POST, bit status indicators 82 preferably flash in an orange hue. Successful completion of the POST causes bit status indicators 82 to remain illuminated for a brief period (e.g. one second) and then darken if all LRUs are deemed to be operating normally. By contrast, if an LRU fails the POST, its corresponding bit status indicator 82 will remain illuminated. Further, if any failure constitutes a safety-critical system fault, TAS 10 will enter a “fail safe” mode, and any attempt to recover from such a mode will, at minimum, require power switch 58 to be toggled off and then back on.
[0034] Following successful completion of the POST, respective arm power and arm enable switches 58 and 74 may become active. Arm power switch 58 preferably is a momentary switch; to initiate arming of countermeasures 34 , an operator toggles the switch 58 and releases it. Under normal operation and proper sequencing, indicator 70 illuminates in a yellow hue.
[0035] One proper sequencing technique requires crew manipulation of arm enable switch 74 to occur within a defined time period following toggling and release of arm power switch 58 . Such a defined time period may, for example, be between approximately 0.5-6.0 seconds. If switch 74 is not manipulated within the period, indicator 70 will de-illuminate and arm power switch 58 will deactivate, necessitating re-toggling and release of switch 58 to re-start the sequence. By contrast, if cover 86 is moved and switch 74 is manipulated within the period, indicator 78 illuminates and TAS 10 enters an “arm enable” mode.
[0036] With TAS 10 in this “arm enable” mode, processor 22 controls deployment of countermeasures 34 (unless switch 38 or 58 is opened). Processor 22 directly or indirectly receives signals from sensors 26 and determines if deployment of any countermeasure 34 is appropriate. If deployment is appropriate, processor 22 signals ESAD 30 . In some versions of the invention, processor 22 may be housed in an enclosure having deformable brackets so as to allow dampening of shocks otherwise likely experienced by the processor 22 .
[0037] FIGS. 3-4 and 5 A illustrate a sample countermeasure 34 . Countermeasure 34 may be assembled as a cartridge to facilitate shipping and storage, for example. It may include housing 90 containing at least mass 94 and charge 98 . Countermeasure 34 may connect to ESAD 30 and initiator 102 using conventional detonation cord 106 .
[0038] Presently-preferred masses 94 are predominantly solids (rather than liquids or gases). Such preferred solids either are disintegrable upon ejection from the vehicle or comprise multiplicities of disintegrated particles. Disintegration of mass 94 upon deployment of countermeasures 34 is preferred so as to reduce likelihood of serious injury to at least some bystanders possibly impacted by mass 94 .
[0039] Charge 98 may be or include any propellant or other substance capable of causing a countermeasure 34 to eject from a vehicle. Upon receipt of a suitable signal from processor 22 , ESAD 30 activates initiator 102 , which in turn ignites detonation cord 106 connected to a countermeasure 34 . Detonation of cord 106 causes deflagration (if pyrotechnic) or other activation of charge 98 so as to eject mass 94 from the vehicle. A single initiator 102 may be employed to launch any number of countermeasures 34 ; alternatively, each countermeasure 34 may be associated with a separate initiator 102 . To expedite initiation, capacitors associated with initiator 102 may be pre-charged under certain conditions.
[0040] FIGS. 5B-F depict various examples of banks 110 of barrels 114 into which countermeasure 34 may be loaded. Banks 110 may be mounted to vehicles at any suitable time either before or after the vehicles enter a hostile environment. Although cartridges of countermeasures 34 likewise may be loaded into barrels 114 at any time, preferably they remain unloaded until a vehicle is slated to approach or enter an environment in which deployment of countermeasures 34 may be considered reasonably likely. Barrels 114 may be made of metal, composites, or other suitable material and may be attached to or formed within banks 110 .
[0041] FIG. 5B schematically illustrates a bank 110 containing five barrels 114 , one of which is loaded with a countermeasure 34 . Bank 110 may be mounted onto a vehicle (see, e.g., FIG. 7 ) in any desired location. In some embodiments of the invention, a bank 110 is mounted onto a vehicle at or adjacent each of its four corners (front left, front right, rear left, rear right).
[0042] Depending on the locations and types of forces encountered by sensors 26 , any one or more banks 110 may launch countermeasures 34 . Moreover, if a bank 110 includes more than one barrel 114 , less than all countermeasures 34 loaded in the barrels 114 may be launched at any particular time. Launching of countermeasures 34 further may be staggered or sequenced in time (either within a particular bank 110 or between particular banks 110 ).
[0043] Presently preferred is that barrels 114 be vertical (or substantially so) with their openings 118 positioned upward when mounted to a vehicle. In this manner, a countermeasure 34 will be ejected upward from the vehicle upon deployment, producing a downward force vector upon ejection. Such downward force vector is intended to counteract (in whole or in part) an upward force impacting a vehicle because of, e.g., explosion of a mine or IED, collision of the vehicle with an object, or departure of the vehicle from a roadway or other normal travel surface.
[0044] Alternatively, one or more barrels 114 could be tilted or otherwise repositionable relative to a (nominal) vertical orientation. If so, deployment of materials loaded therein could be used to establish different force vectors acting on a vehicle, or the barrels 114 (regardless of orientation) could be used to deploy flares, missiles, projectiles, or other objects for various purposes. Because banks 110 themselves may have substantial mass, they may function as armor for a vehicle. Reactive armor plates or tiles may be deployed, as may any mass associated with a vehicle (e.g. engine, engine cover, battery, water supply, passive armor, etc.).
[0045] TAS 10 may be modular, scalable, and configured to be adapted for use with a variety of vehicles or other objects. Sensors 26 may sense such things as changes in acceleration, pressure, strain (deformation), force, displacement, infrared (IR) signals, radio frequency (RF) signals, acoustic signals, electric or magnetic field strength, or RADAR or LIDAR signals. Those skilled in the art will recognize that other signals, events, or changes may be sensed alternatively or additionally. However, presently preferred as sensors 26 are accelerometers augmented by either or both of strain and force sensors. At least some sensors 26 preferably are housed in enclosures mounted to or integrated into areas of a vehicle such as its A/B/C/D pillars or drivetrain tunnel or in other stiff (rigid) structural locations.
[0046] Data from sensors 26 may be filtered or encoded (or both) to reduce noise or other incorrect information being received by processor 22 . Some versions of TAS 10 further contemplate comparing information from at least two non-co-located sensors 26 as part of an assessment of the validity and location of a blast or other event. FIG. 6 identifies an example of certain logical conditions in which firing countermeasures 34 may be deemed appropriate. Computational logic assesses information from sensors 22 relating to “Effective G” (as discussed in S. Arepally, et al., “Application of Mathematical Modeling in Potentially Survivable Blast Threats in Military Vehicles,” 26th Army Science Conference, Dec. 1-4, 2008, the contents of which are incorporated herein in their entirety by this reference) and changes in vehicle velocity (dV) as a function of time length (L). In the exemplary case of FIG. 6 (as simplified for ease of explanation):
If G is less than a threshold value X or all countermeasures 34 have already fired, TAS 10 remains in a “safe” or “idle” mode. If G is greater than or equal to X and at least one countermeasure 34 remains unfired, TAS 10 is armed; however, if G subsequently becomes less than X, dV is less than a threshold Y 1 and L is less than a threshold Z, TAS 10 returns to the safe or idle mode. Once armed, TAS 10 remains so if G is greater than or equal to X or if dV is greater than Y 1 or L is greater than Z. If dV of one sensor set (S 1 ) exceeds Y 2 (where Y 2 >Y 1 ), dV of a different sensor set (S 2 ) exceeds Y 1 , and L exceeds Z, any unfired countermeasures 34 associated with set S 1 fire. By contrast, if no dV measurement exceeds Y 2 or L is less than Z, then TAS 10 remains armed but does not fire.
[0052] The foregoing is provided for purposes of illustrating, explaining, and describing embodiments of the present invention. Modifications and adaptations to these embodiments will be apparent to those skilled in the art and may be made without departing from the scope or spirit of the invention. | Described are systems and methods for actively countering certain forces experienced by, for example, a person within a vehicle. Adverse effects of blast waves of a mine or other explosive device (including improvised explosive devices [IEDs]) may be mitigated by the countermeasures systems, which may include any or all of a first responder unit (FRU), a control display assembly (CDA), processors, sensors, and an electronic safe and arm device (ESAD). Each component assembly may be incorporated into a line replaceable unit (LRU) if desired, although such incorporation is not necessary. | 5 |
FIELD OF THE INVENTION
The invention relates to a paver and a method of paving for casting multiple paving layers.
BACKGROUND OF THE INVENTION
A known paver for casting several layers of concrete comprises at least two high compaction concrete paving screeds which are located behind each other, are towed floatingly and are linked by separate towing bars to the chassis. Both paving screeds are situated in operation travelling direction behind the undercarriage. Two hoppers each for one sort of a concrete paving material are provided at the chassis from which hoppers separate longitudinal conveyors extend to the lateral distribution assemblies arranged in front of the respective paving screed. The undercarriage travels on the plane. The first paving screed casts and compacts the lower layer before an upper layer is immediately subsequently cast and compaction thereon. The structure of the paver is relatively complicated. The paver has a large working height. It thus is necessary to install upper paver components such that they can be removed for transport purposes. The weight of the paver is high, in particular in the rear region of the chassis such that in some cases rear cantilevering supporting outriggers equipped with running wheels are needed.
Furthermore, a paver for casting two asphalt layers on top of each other is known from the BAUMA 2004 exhibition (compact asphalt paver) which comprises two high compaction asphalt paving screeds which are linked by separate towing bars to the chassis and operate behind each other and behind the undercarriage. A second removable hopper is provided on top of a hopper which is integrated into the chassis. Separate longitudinal conveyers extend from both hoppers to lateral distribution assemblies in front of the respective paving screeds. The known paver is of complicated construction, very heavy, and has an enormous height. The rear chassis end is additionally supported on the plane by rear cantilevering outriggers equipped with ground wheels.
When casting a fixed trackway, e.g. a railway embankment, with one paver having two floatingly towed high compaction paving screeds of certain working widths e.g. two concrete layers are cast on top of each other each of which may have a thickness up to about 30 cm. This is done e.g. because a single layer of about 60 cm of concrete may be cast but could not be compacted sufficiently in the lower region. The undercarriage travels on the plane. Among other things, the paver is structurally complicated and heavy, because all of the paving material has to be fed longitudinally through the paver and has to be transferred to the towed paving screeds.
BRIEF DESCRIPTION OF THE INVENTION
Of further interest are: DE 295 10 058 U, DE 199 35 598 A.
It is an object of the invention to provide a paver of the kind as disclosed which is structurally simple, compact and lightweight, and to provide a method which allows to simultaneously cast several layers in a simpler fashion.
Feeding the one paving screed which casts a lower layer in front of the undercarriage only needs low apparatus efforts and is simpler in terms of the method than feeding is in the known pavers. With the help of the simplified feeding a simple and fair cost structure of the paver is achieved, offering the advantage of lower height and lower weight. The existing prejudice against a paver travelling on a freshly cast layer surprisingly has proven to be a false estimation, because modern paving screeds allow to generate in most of the usual paving material sorts a degree of compaction which withstands the mechanical load of the travelling undercarriage without any problems. The paving screed placed in the front improves the weight distribution of the paver and does not significantly hinder the conventional feeding by a dump truck or a feeder travelling ahead. The paving screed supported behind the undercarriage at the chassis then casts a respective upper layer. The paver can not only be used for concrete paving material but also for asphalt paving material or even for combinations of these paving materials. Even other paving materials can be processed with the paver provided that the respective paving material allows to be compacted sufficiently. Expediently the same sort of paving material is processed by the front and rear paving screeds because then the feeding is simpler. Alternatively, however, differing paving materials could be cast by the front and rear paving screeds.
In terms of the method it is expedient when the lower layer is cast and compacted with the help of direct feeding to the paving screed placed in front of the undercarriage while each upper layer first is cast and compacted behind the undercarriage on top of the compacted lowest layer.
Expediently the compacted devices of the paving screeds are high compaction devices which allow to generate at least a degree of compaction which can tolerate the undercarriage running thereon without problems, or which in some cases even is higher than would be needed for paver travelling with the total weight on the freshly compacted layer. In connection therewith the contents of DE C 31 14 049 and DE C 32 09 989 are incorporated here.
In a preferred embodiment the front paving screed is directly fixedly supported at the chassis in a selectively adjusted height and/or with a selectively adjusted blade angle. In this case a significant part of the total weight of the paver resting on the chassis can be used to easily reach a high degree of compaction. The thickness of the layer is determined by the adjustments of the paving screed in relation to the chassis.
In another embodiment it may be expedient to support the front paving screed at the chassis such that it is floatingly towed or pushed. In this case the total paver weight resting on the chassis cannot be used for the compaction, however, modern high compaction devices (DE C 31 14 049; DE C 32 09 989) produce without extra load sufficiently high degrees of compaction by means of the frequency and the strength of the compacting pulses.
In order not to complicate feeding into the hopper it is expedient when the front paving screed is placed in front of the chassis front end but at least partly below the filling area of the hopper.
The front paving screed should comprise at least one high compaction bar and compaction bar drives, e.g. of hydraulic nature, and at least one tamper bar and, preferably hydraulic, tamper bar drives. These two component groups allow in conjunction to produce sufficiently high degrees of compaction and a well-defined evenness of the cast and compacted lower layer.
Particularly expediently the front paving screed is comprised of a screed body of a base screed part of a standardised paving screed or of a standardised extendable paving screed (i.e. of a base screed part without extension parts). The screed body has small height and is not very deep in travelling direction such that the feeding conditions for the hopper are hardly negatively affected. The screed body used as the front paving screed corresponds in this case e.g. to a downsized base screed part of a standard paving screed or of a standard extendable paving screed, i.e. it does not need to be a specially manufactured new paving screed. Although the front paving screed could uniformly cast the lower layer on the plane out of a sufficiently large paving material heap, thanks to the strong pushing force of the undercarriage, it could be expedient to provide at least one lateral distribution assembly in front of the front paving screed, e.g. a lateral auger arrangement or a lateral distribution blade assembly. A lateral distribution blade or several lateral distribution blades save weight, only need a simple drive, and result in a small depth in working direction.
When the front paving screed is directly supported at the chassis it expediently can be pivotally adjusted about a lateral axis and can be fixed in selective pivotal positions, preferably by means of at least one adjustment drive arranged between the paving screed and the chassis. Furthermore, the paving screed should be adjustable and fixable in height relative to the lateral axis and relative to the chassis. The reaction forces resulting from casting the paving material on the plane directly are taken-up from the heavy chassis on which the total weight of the paver is resting.
Expediently, the front paving screed has a working width larger than the track width of the undercarriage, and corresponding to the working width of the paving screeds provided behind the undercarriage. In the case that e.g. the working width of a screed body of a base screed part should be too small compared to the desired working width, as usual, broadening parts can be mounted on the sides of the screed body.
Alternatively, the front paving screed could be an extendable paving screed having extension parts. This embodiment is expedient for casting layers of asphalt paving material. Structural equipment can be simple when the compaction bar drives and/or the tamper bar drives are directly connected to the power supply of compaction bar drives and/or tamper bar drives for one of the paving screeds provided behind the undercarriage. This does not exclude providing the front paving screed with its own power supply and power control. Although the front paving screed does not necessarily need vibrators, even vibrators for the smoothing plate could be installed, if desirable.
Feeding the respective paving material can be simplified if a saddleback roof-shaped pouring surface arrangement is provided above the front paving screed which arrangement both extends forwards in front of the front paving screed and rearwards to the filling area of the hopper. The paving material transferred from a dump truck or a feeder can be lead by the pouring surface arrangement into the hopper and at the same time to the plane region in front of the front paving screed to build a heap of paving material there. Preferably, the pouring surface arrangement is provided with a gathering snout which extends downwardly in front of the front paving screed and at which the lateral distribution assembly could be mounted. The gathering snout enhances the lateral distribution of the paving material and prevents too strong a contamination of the front paving screed. The pouring surfaces could be sheet metal parts and/or rubber plates. In a simple embodiment a rubber hood is used which is carried by the chassis.
In a preferred embodiment having a front paving screed supported fixedly at the chassis lateral tubes of a tube frame defining the lateral axis of the front paving screed are hung into outriggers provided at the chassis or at a lateral beam of the chassis, respectively. The height adjustment device is provided between the lateral tubes and the outriggers in order to allow to adjust and fix the blade angle of the paving screed. Furthermore, the adjustment drives for adjusting the height position of the lateral axis or of the paving screed, respectively, are arranged between the paving screed and the chassis lateral beam. The arrangement results in a well defined transfer of reaction forces into the chassis.
Expediently the front paving screed and accessory components define a sub-structure group which is removable from the paver. A paver designed for casting a single layer can be retrofitted with only small modifications in the front end region of the chassis without problems and with the sub-structure group to a paver for then casting several layers. For example, only the dump truck wheels pushing rollers need to be dismantled before the front paving screed is mounted instead.
In an expedient embodiment the paver is equipped with a caterpillar undercarriage, the front high compaction paving screed being located in front of the caterpillar undercarriage, with a further floatingly towed high compaction paving screed towed behind the caterpillar undercarriage, all for casting a firm trackway, e.g. a railway embankment, with a width up to about 3.0 m. Both paving screeds have the respectively needed working widths, which even may be equal among each other. Both paving screeds are aligned with one another in longitudinal direction of the paver. Expediently, both paving screeds even are base screed parts of standardised paving screeds or standardised extendable paving screeds, respectively.
Expediently, the method is carried out such that a firm trackway, e.g. a railway embankment, is cast of two concrete layers cast one above each other at a width of about 3.0 m.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will be explained with the help of the drawings. In the drawings is:
FIG. 1 a schematic side view of a paver prepared for casting several layers, and
FIG. 2 an enlarged illustration of a front chassis end region of the paver of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
A paver F in FIG. 1 serves to cast at the same time several paving material layers L 1 , L 2 which lie on top of each other, particularly from concrete and/or asphalt, on a plane P which has been subjected to a preparatory treatment. The paver F has a chassis 1 on an undercarriage 2 , in this case e.g. a caterpillar undercarriage, which is driven from a primary drive source 3 in operation running direction R. An operator's stand 4 is provided behind the primary driving source 3 . A paving material hopper 5 of paving material is placed in front of the primary driving source 3 at or within the chassis 1 . A longitudinal conveyor 6 indicated by dotted lines extends from the paving material hopper 5 to the rear end of the chassis 1 and to a lateral distribution assembly 7 which is provided on the chassis 1 , e.g. a lateral auger assembly. A paving screed B 2 which is placed behind the lateral distribution device 7 is floatingly towed by towing bars 8 which are linked to the sides of the chassis 1 .
The rear paving screed B 2 has a base screed part 9 with a lower screed body 11 , and, in some cases, even sidewardly extendable extension screed parts 10 . At least the base screed part 9 is equipped with at least one tamper bar 13 which e.g. is driven by not shown hydraulic motors and with one or several compacting bars 12 having, e.g. hydraulic, swelling force drives (not shown) and rotary valves, altogether constituting a compaction device of the paving screed B 2 , e.g. corresponding to DE C 31 14 049 or DE C 32 09 989.
At a frontal end section of the chassis 1 seen in the operation running direction a front paving screed B 1 is provided such that it can cast and compact the lower layer L 1 in front of the undercarriage 2 from a paving material heap V 1 . The paving screed B 1 as well is equipped with a compaction device, e.g. with at least one tamper bar 13 with e.g. a hydraulic drive and at least one compaction bar 14 with e.g. hydraulic drives. Furthermore, a frontally placed lateral distribution assembly 15 , 16 is associated to the front paving screed B 1 , e.g. a lateral hydraulic cylinder 16 driving at least one distribution blade 15 back and forth laterally to the operation running direction R, in order to uniformly distribute the paving material from the paving material heap V 1 . Not shown side plates can be, as conventional, provided at the paving screed B 1 .
The blade angle of the paving screed B 1 can be adjusted about a lateral axis 17 , in particular by adjustment drives indicated by a double arrow 19 . Furthermore, the paving screed B 1 is adjustable in height direction (double arrow 18 ) by a not shown height adjustment device. The front paving screed B 1 can be fixed in the respective selected pivotal position (blade angle) or height position in relation to the chassis 1 and is then directly fixedly supported at the chassis 1 .
In the embodiment shown, e.g. the hydraulic drives of the compaction bar 14 or the tamper bar 13 in the front paving screed B 1 are connected by supply strands 21 with a power supply of the tamper bar 13 and the compaction bar 14 of the rear paving screed B 2 placed behind the undercarriage 2 , such that the front paving screed B 1 does do not need its own power control assemblies like rotary valves or flow regulating valves. Alternatively, such power control devices as well could be contained in the one front paving screed B 1 and then could be connected with the hydraulic supply of the paver.
The compaction assembly of each paving screed B 1 , B 2 expediently is a high compaction assembly such that the lower layer L 1 can also be cast by the paving screed B 1 in front of the undercarriage 2 with a degree of compaction which then immediately can carry the undercarriage 2 with the total weight of the paver F, or which degree of compaction even is higher than needed for that.
The paving material for the rear paving screed B 2 is filled e.g. by a dump truck or a feeder into the hopper 5 . The paving material for the front paving screed B 1 e.g. is thrown by the same truck or feeder on the plane P in front of the paving screed B 1 to form the heap V 1 . The longitudinal conveyor 6 forms a paving material heap V 2 in front of the lateral distribution assembly 7 of the rear paving screed B 2 such that the rear paving screed B 2 is capable of casting the upper layer L 2 out of the heap V 2 and compacting the upper layer during the casting process.
During operation of the paver F in FIG. 1 the lower layer L 1 is cast by the front paving screed B 1 and is compacted so far that the undercarriage 2 can run without problems on the compacted lowest layer L 1 before the upper layer L 2 is cast and compacted behind the undercarriage by the rear paving screed B 2 .
Both paving screeds B 1 , B 2 have the same working width which e.g. is broader than the track width of the undercarriage 2 . The same paving material sort can be processed by both paving screeds B 1 , B 2 . Alternatively, different paving material sorts can be processed, however, then care has to be taken that the feeding processes to the front paving screed B 1 and to the hopper 5 are carried out separately. The thicknesses of the layers L 1 , L 2 may be equal or may differ from each other.
Expediently the front paving screed B 1 is a screed body 11 of the base screed part 9 of a standard paving screed. The extendable screed parts indicated in FIG. 1 at the rear paving screed B 2 may be present or may be omitted at the front paving screed B 1 . When the extendable screed parts are present at the rear paving screed, they will remain retracted to have a certain working width corresponding to the working width of the front paving screed B 1 .
Alternatively, both the front paving screed B 1 and the rear paving screed B 2 could be designed as extendable paving screeds having sidewardly extendable screed parts.
In FIG. 1 the front paving screed B 1 is fixedly supported at the chassis 1 such that the total weight of the paver F resting on the chassis 1 assists the compaction of the lower layer L 1 .
Alternatively (not shown), however, the front paving screed B 1 even could be towed or pushed floatingly, and in particular with pushing bars similar to the tow bars 6 . In this case the blade angle of the front paving screed B 1 fixed to the pushing bars could be adjusted by height adjustments of the linking points of the pushing bars at the chassis 1 .
FIG. 2 schematically indicates a part of a paver F which can be used as a not limiting embodiment in order to produce a firm trackway, e.g. a railway embankment, of two concrete layers, e.g. with a width up to 3.0 m. For this work the (not shown) rear paving screed B 2 of the paver in FIG. 2 may be a base screed part essentially like the base screed part 9 , 11 in FIG. 1 (without extendable screed parts) with a working width of 3.0 m or with a base width of 2.5 m and two sidewardly placed broadening parts of 25 cm each, and with a compaction assembly (high compaction assembly). The front paving screed B 1 may be a screed body 11 of a base screed part 9 only.
The side outriggers 24 are fixed at a conventional chassis lateral beam 25 and protrude forwards. The outriggers 24 contain in pockets lateral tubes of a tube frame of the paving screed B 1 . The lateral tubes define the pivot axis 17 . The height adjustment device 18 engages at each side at the lateral tubes. The adjustment drives 19 are placed between the paving screed B 1 and the chassis lateral beam 23 , e.g. in the form of hydraulic cylinders or turnbuckles or the like, in order to allow to adjust and fix the blade angle. Reference numeral 28 indicates e.g. hydraulic drives for the tamper bar 13 ; reference numeral 29 indicates e.g. hydraulic drives for both compaction bars 14 . Those drives are connected via supply strands 21 indicated in FIG. 1 either to the power control of the corresponding components in the rear paving screed B 1 (flow regulation valve, rotary valve), or (not shown) are equipped with their own power control devices which then are connected to the hydraulic system of the paver, respectively. Additionally, a vibrator 22 for the lower smoothing plate of the screed part 11 is indicated which may be provided optionally.
A pouring surface assembly with the shape of a saddleback roof having pouring sheet metal surfaces and/or rubber plates 25 , 26 is shown above the front paving screed B 1 . The assembly forms a downwardly sloped ramp into the filling region of the hopper 5 (for the paving material for the rear paving screed B 2 ) and a ramp (for the paving material for the front paving screed B 1 ) inclined forwardly in operating running direction R. A downwardly extending gathering snout 27 (made of sheet metal or rubber) continues the frontmost pouring sheet metal surface. The snout 27 covers the tamper bar 14 at the front side. The lateral distribution assembly indicated in FIG. 1 , e.g. consisting of the hydraulic cylinder 16 with the distributing blades 15 , is not shown in FIG. 2 . However, such an assembly could be provided in front of the snout 27 in order to sidewardly distribute the heap V 1 such that the front paving screed B 1 receives sufficient paving material forecasting the lowest layer L 1 over the full working width. The pouring surface assembly 25 , 26 could be a hood of semi-rigid rubber material including the gathering snout 27 and could cover the paving screed B 1 , could control the feeding flow of the paving material, and could be removably fixed at suitable locations of the chassis 1 .
During operation of the respective paving screed B 1 , B 2 the tamper bar 13 pre-compacts and evens before the at least one compaction bar 14 produces the final degree of compaction high enough to prevent damage in the lowest layer L 1 when the undercarriage 2 travels on the compacted lowest layer L 1 . The compacting bars 14 are actuated by swelling force pulses in order to uniformly compact the lower layer L 1 down to the plane P without a significant beating action. Incidentally, the plane P is pre-treated in order to be substantially even and free of larger objects.
Prior to the start of the casting operation the undercarriage 2 is moved on laid down planks or on ramps which slope upwardly in operation travelling direction R. Then the blade angle and the height position of the front paving screed B 1 are adjusted corresponding to the thickness of the lower layer L 1 . The rear paving screed B 2 is adjusted in analogous fashion.
The following alternatives could be provided:
In case that more than two layers are to be cast more than one paving screed B 2 , each expediently having its own towing bars 6 , could be provided behind the undercarriage 2 . In case that differing paving material sorts are to be processed more than the one hopper 5 could be provided. In this case the hopper for the front paving screed does not need a longitudinal conveyor but e.g. pours the paving material directly in front of the paving screed on the plane by gravity and through controlled dosing flaps or the like. In some cases heap touching feelers could be used to regulate a sufficiently large heap in front of the paving screed. Finally, the front paving screed B 1 could be a special one adapted to the particular casting conditions and feeding relationships in front of the paver.
The front paving screed B 1 with its accessory components expediently is a removable sub-structure of the paver F. The paver is slightly modified in comparison to a standard paver e.g. having truck wheels pushing rollers at the front The paver is retrofitted from a condition for casting a single layer behind the undercarriage or for casting several layers behind the undercarriage only into a condition for now casting several layers in front of and behind the undercarriage 2 .
The pouring surface assembly 25 , 26 in FIG. 2 expediently is provided for feeding one paving material sort from a dump truck or from a feeder to both paving screeds B 1 , B 2 . The dump truck or the feeder then does not only feed into the hopper 5 but also forms the heap V 1 . In case that differing paving material sorts are processed then e.g. two feeders which are offset sidewardly in relation to each other could feed into the hopper 5 and in front of the front paving screed B 1 . A further possibility is to load the hopper 5 from the side and to form the heap V 1 from the front side.
The core of the invention is to provide at a feeder F at the chassis in front of the undercarriage 2 (caterpillar undercarriage or wheeled undercarriage) a paving screed B 1 having a compaction device for casting a lower layer and for compacting the lower layer so strongly that the undercarriage can travel on the cast lower layer without damaging it before in some cases a further upper layer is cast behind the undercarriage. | At least two paving screeds B 1 , B 2 which are distant in operation running direction R are supported at a chassis 1 of a paver F. The paver F is designed for simultaneously casting several paving material layers L 1 , L 2 on top of each other on a plane P. Each paving screed B 1 , B 2 is provided with a compaction assembly. One paving screed B 1 for casting a lower layer L 1 is provided at a front end section of the chassis 1 and has the compaction assembly 13, 14 for generating a degree of compaction in the lower layer L 1 which suffices to withstand the direct contact of the undercarriage 2 . At least one further paving screed B 2 for casting an upper layer L 2 is arranged behind the undercarriage 2 . According to the method to be carried out with the paver F the lower layer which is cast and compacted in front of the undercarriage allows to run the undercarriage 2 on the lower layer while the upper layer L 2 is cast and compacted behind the undercarriage 2. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This nonprovisional utility application is a divisional application of and claims the benefit under 35 U.S.C.§120 to co-pending U.S. application Ser. No. 13/382,907 filed Mar. 8, 2012, all of which are incorporated, in their entirety, by this reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to extraction techniques and more particularly to a method of making longan seed extract.
[0004] 2. Description of the Related Art
[0005] (1) Inflammation is part of the complex biological response of vascular tissues to harmful stimuli, such as pathogens, damaged cells, or irritants. Inflammation is a protective attempt by the organism to remove the injurious stimuli and to initiate the healing process. Inflammation is not a synonym for infection, even in cases where inflammation is caused by infection. Although infection is caused by a microorganism, inflammation is one of the responses of the organism to the pathogen. However, inflammation is a stereotyped response, and therefore it is considered as a mechanism of innate immunity. Contents of inflammation comprise nitric oxide (NO), tumor necrosis factor (TNF), interleukin (IL), granulocyte colony stimulating factor (G-CSF), monocyte colony stimulating factor (M-CSF), granulocyte-monocyte colony stimulating factor (GM-CSF), and lymphotoxini (LT) such as TNF-α and TNF-β.
[0006] Without inflammation, wounds and infections would never heal. Similarly, progressive destruction of the tissue would compromise the survival of the organism. However, chronic inflammation can also lead to a host of diseases, such as hay fever, periodontitis, atherosclerosis, and rheumatoid arthritis. It is for that reason that inflammation is normally closely regulated by the body.
[0007] Typically, antibiotics, non-steroidal anti-inflammation drugs (NSAIDs), and anti-histamine drugs are used to treat inflammation and they improve symptoms. However, side effects are also reported.
[0008] (2) Gout is a medical condition usually characterized by recurrent attacks of acute inflammatory arthritis, e.g., a red, tender, hot, swollen joint. Goat can be hypercuricemia, recurrent acute monoarthrities, and tophi. Gouty nephropathy is the symptom of serious goat. The metatarsal-phalangeal joint at the base of the big toe is the most commonly affected. However, it may also present as tophi, kidney stones, or urate nephropathy. It is caused by elevated levels of uric acid in the blood which crystallize and are deposited in joints, tendons, and surrounding tissues.
[0009] Hypercuricemia is the main cause of gout. About 5-18.8% patients suffering hypercuricemia may have gout in the end period. It is fatal in some cases.
[0010] Uricase differential spectrophotometric method can be used to cure hyperuricemia. Hyperuricemia is a level of uric acid in the blood that is abnormally high. In humans, the upper end of the normal range is 360 μmol/L (6 mg/dL) for women and 400 μmol/L (6.8 mg/dL) for men. Many factors contribute to hyperuricemia including genetics, insulin resistance, hypertension, renal insufficiency, obesity, diet, use of diuretics, and consumption of alcoholic beverages.
[0011] Hyperuricemia has four stages including asymptomatic hyperuricemia, acute gouty arthritis, inter-critical gout, and chronic tophaceous gout.
[0012] Diagnosis is confirmed clinically by the visualization of the characteristic crystals (e.g., monosodium urate crystal) in joint fluid. Shown negative birefringent means gout symptom. Other parts of a patient including toes, feet, and ankles can be also observed for gout symptom.
[0013] Treatment with steroids or colchicine improves gout symptoms. Once the acute attack has subsided, levels of uric acid are usually lowered via lifestyle changes, and in those with frequent attacks allopurinol or probenecid provide long-term prevention.
[0014] Precipitation of uric acid crystals, and conversely their dissolution, is known to be dependent on the concentration of uric acid in solution, pH, sodium concentration, and temperature. Established treatments address these parameters.
[0015] Uricosuric agents are substances that increase the excretion of uric acid in the urine, thus reducing the concentration of uric acid in blood plasma. In general, this effect is achieved by action on the proximal tubule. Drugs that reduce blood uric acid are not all uricosurics. Blood uric acid can be reduced by administered uricosuric agents for seven to ten days gradually increased in amount. Other drugs such as probenecid and benzbromarone can also be used.
[0016] Treatment with xanthine oxidase inhibitor, allopurinol, hypoxanthine, and xanthine oxidase improves symptoms. Also, mercaptopurine or azathioprine can be used to treat gout but caution should be taken due to its side effects.
[0017] (3) Wound healing is an intricate process in which the skin repairs itself after injury. In normal skin, the epidermis (i.e., outermost layer) and dermis (i.e., inner or deeper layer) exists in a steady-state equilibrium, forming a protective barrier against the external environment. Once the protective barrier is broken, the normal process of wound healing is immediately set in motion. The classic model of wound healing is divided into four sequential phases: hemostasis, inflammatory, proliferative, and remodeling. Upon injury to the skin, a set of complex biochemical events takes place in a closely orchestrated cascade to repair the damage. Within minutes post-injury, platelets aggregate at the injury site to form a fibrin clot. This clot acts to control active bleeding.
[0018] Growth factors related to wound healing include fibroblast growth factor 2 (FGF2), platelet-derived growth factor (PDFG), epidermal growth factor (EFG), keratinocyte growth factor (KGF), transforming growth factor-α (TGF-α), transforming growth factor-β (TGF-β), and vascular endothelial growth factor (VEGF). These growth factors including PDFG, EFG, TGF-β, and VEGF are secreted by cells. Further, PDGF can absorb macrophages and fibroblasts and facilitates matrix protein growth. EGF can autocrine for growth. TGF-β can facilitate fibroblasts growth. VEGF can facilitate proangiogenic matrix growth and accelerate monocyte movement. These factors are closely related to wound healing.
[0019] In the inflammatory phase, bacteria and debris are phagocytosed and removed, and factors are released that cause the migration and division of cells involved in the proliferative phase. The proliferative phase is characterized by angiogenesis, collagen deposition, granulation tissue formation, epithelialization, and wound contraction. In angiogenesis, new blood vessels are formed by vascular endothelial cells. In fibroplasia and granulation tissue formation, fibroblasts grow and form a new, provisional extracellular matrix by excreting collagen and fibronectin.
[0020] The invention discussed below is novel and nonobvious as far as the present inventor is aware.
SUMMARY OF THE INVENTION
[0021] It is therefore one object of the invention to provide an extraction method comprising the steps of (1) choosing an extraction solvent; (2) heating the extraction solvent to a first predetermined temperature; (3) adding pulverized longan seed to the extraction solvent to prepare a solution; (4) maintaining the solution at a second temperature for a predetermined period of time to obtain an extracted substance; (5) filtering the extracted substance; and (6) drying and cooling the filtered extracted substance to produce an extract.
[0022] In a first aspect of the invention, the extraction solvent is either water or inorganic compound.
[0023] In a second aspect of the invention, the inorganic compound is a solvent having a predetermined volume concentration of ethanol.
[0024] In a third aspect of the invention, the predetermined volume concentration of ethanol is about 20-95%.
[0025] In a fourth aspect of the invention, the first predetermined temperature is about 70-90° C.
[0026] In a fifth aspect of the invention, the second predetermined temperature is about 70-90° C.
[0027] In a sixth aspect of the invention, the predetermined period of time is about 1-3 hours.
[0028] In a seventh aspect of the invention, the extract comprises corilagin, ellagic acid, and gallic acid.
[0029] In an eighth aspect of the invention, the longan seed extraction can cure inflammation.
[0030] In a ninth aspect of the invention, the longan seed extraction can cure hyperuricemia.
[0031] In a tenth aspect of the invention, the longan seed extraction can heal wound.
[0032] In an eleventh aspect of the invention, the longan seed extraction can inhibit microorganism growth.
[0033] In a twelfth aspect of the invention, the longan seed extraction has the following advantages including curing inflammation, curing hyperuricemia, healing wound, and inhibiting microorganism growth.
[0034] The above and other objects, features and advantages of the invention will become apparent from the following detailed description taken with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0035] FIG. 1 is a chart of results obtained by processing a solution comprising gallic acid, corilagin, and ellagic acid chosen as a control group according to the invention by means of an HPLC apparatus;
[0036] FIG. 1A shows the structural formulas of corilagin, gallic acid, and ellagic acid;
[0037] FIG. 1B is a table showing conditions of operating the HPLC apparatus;
[0038] FIG. 2 is a graph of results obtained by processing a longan seed extract comprising gallic acid, corilagin, and ellagic acid chosen as a control group according to the invention by means of an HPLC apparatus;
[0039] FIG. 2A is a table showing results of original IL-β and after stress IL-β in the anti-inflammation test;
[0040] FIG. 3 plots TNF-α versus IL-β for LPS, longan seed extract, longan seed extract after one-week, and control group;
[0041] FIG. 3A is a table showing results of original TNF-α and after stress TNF-α in the anti-inflammation test;
[0042] FIG. 4 plots the effect of decreasing serum of SD rats for treatment group, longan seed extract group, and control group;.
[0043] FIG. 4A is a table of uric acid concentrations of control group, treatment group and longan seed extract group for anti-gout experiment;
[0044] FIG. 5 plots the number of Escherichia coli for control group and treatment group;
[0045] FIG. 5A plots the number of staphylococcus aureus for control group and treatment group;
[0046] FIG. 5B is a table showing results of anti-gout experiment with respect to xanthine oxidase and other samples;
[0047] FIG. 6 plots the number of propionibacterium acne for control group and treatment group;
[0048] FIG. 6A is a table showing results of toxicity test by subjecting to consecutive oral feeding;
[0049] FIG. 7 plots the number of Trichophyton rubrum for control group and treatment group;
[0050] FIG. 7A is a table showing results of micro-organisms inhibition with respect to Escherichia coli and Staphylococcus aureus;
[0051] FIG. 8 plots growth times versus time for crystal violet having different dose percentages;
[0052] FIG. 8A is a table showing results of micro-organisms inhibition with respect to propionibacterium acne;
[0053] FIG. 9 plots FN for 0% longan seed extract, 5% longan seed extract, and 10% longan seed extract;
[0054] FIG. 9A is a table showing results of micro-organisms inhibition with respect to Trichophyton rubrum;
[0055] FIG. 10 is a table showing results of growth factors when subjecting to crystal violet dyeing method by using different doses; and
[0056] FIG. 11 is a table showing results when subjecting to ELISA test.
DETAILED DESCRIPTION OF THE INVENTION
[0057] Referring to FIGS. 1 to 11 , a method of making longan seed extract in accordance with the invention comprises the following steps:
[0058] (a) An extraction solvent such as water or inorganic compound is chosen. In this embodiment, a solvent having 20-95% of ethanol is chosen as the extraction solvent.
[0059] (b) The extraction solvent is heated to a temperature of about 70-90° C.
[0060] (c) Pulverized longan seed is added to the extraction solvent to prepare a solution.
[0061] (d) The solution is maintained at a temperature of about 70-90° C. for about 1 to 3 hours for extraction.
[0062] (e) The extracted substance is filtered.
[0063] (f) The filtered extracted substance is dried at a low temperature and low atmospheric pressure environment.
[0064] (g) Finally, longan seed extract is obtained.
[0065] Above steps of the invention are done in a high performance liquid chromatography (HPLC) apparatus. The extract is comprised of gallic acid, corilagin, and ellagic acid. The structural formulas of gallic acid, corilagin, and ellagic acid are shown in FIG. 1A . Further, equipment and conditions of the HPLC apparatus are shown in FIG. 1B .
[0066] The solution comprising gallic acid, corilagin, and ellagic acid is chosen as a control group. The solution is processed by the HPLC apparatus and its results are shown in FIG. 1 . Retention time of gallic acid of 42.42 μg/ml is 14.409 minutes, retention time of corilagin of 52.72 μg/ml is 43.304 minutes, and retention time of ellagic acid of 22.4 μg/ml is 63.489 minutes respectively. The longan seed extract is processed by the HPLC apparatus and its results are shown in FIG. 2 . Peaks of the longan seed extract have retention time of 14.461, 43.302, and 63.476 minutes respectively. Contents of the longan seed extract are the same as that of the solution (i.e., gallic acid, corilagin, and ellagic acid).
[0067] Symptoms improvements by treating with the longan seed extract of the invention are discussed in the following experiments:
Experiment 1
[0068] Treatments with longan seed extract obtained from a solvent having 50% of ethanol, longan seed extract A obtained from a solvent having 100% pure water, and longan seed extract obtained from a solvent having 20% of ethanol improve inflammation symptoms as discussed below.
[0069] 24 Sprague Dawley (SD) rats are grouped into nine groups of different SD rats in which one group is chosen as control group and the remaining groups chosen as treatment groups. It is noted that all SD rats are male in the invention. Each SD rat has a weight of 200-250 g. Room temperature is kept at 23° C. Room is kept bright for 12-hour and dark for next 12-hour repeatedly. Water is treated by reverse osmosis.
[0070] SD rats in the control group is fed with water only.
[0071] Longan seed extract is oral fed to the SD rats of a first treatment group in the weight of 0.5 g/Kg of SD rat. After one week, LPS (lipopolysaccharides) of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat. Another one day is waited.
[0072] Longan seed extract is oral fed to each SD rat of a second treatment group in the weight of 0.5 g/Kg of SD rat, waiting for one week, LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat, and waiting for 48 hours.
[0073] LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat of a third treatment group, waiting for 24 hours, and oral feeding longan seed extract A of 0.5 g/Kg of SD rat to each SD rat.
[0074] LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat of a fourth treatment group, waiting for 24 hours, and oral feeding longan seed extract B of 0.5 g/Kg of SD rat to each SD rat.
[0075] LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat of a fifth treatment group, waiting for 24 hours, and oral feeding longan seed extract of 0.5 g/Kg of SD rat to each SD.
[0076] LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat of a sixth treatment group, waiting for 48 hours, and oral feeding longan seed extract of 0.5 g/Kg of SD rat to each SD rat.
[0077] LPS of 2.5 mg/Kg of SD rat is abdomen injected into each SD rat of a seventh treatment group, and waiting for 24 hours.
[0078] Oral feeding longan seed extract of 0.5 g/Kg of SD rat to each SD rat of an eight treatment group.
[0079] After one night of abstaining from food and drink, ether as anesthesia agent is administered to each SD rat. Next, serum from arterial blood of the SD rat is withdrawn for check by using an Enzyme-linked immunosorbent assay (ELISA) test. It is noted that data obtained by the experiment is subject to ANOVA (one-way analysis of variance).
[0080] As shown in columns “IL-β (ng/L) original” and “IL-β (ng/L) after stress” of FIG. 2A , oral feeding of longan seed extract and abdomen injection of LPS can enhance the immune system of the SD rats. As shown in columns “TNF-α (ng/L) original” and “TNF-α (ng/L) after stress” of FIG. 3A and FIG. 3 , oral feeding of longan seed extract and subsequent abdomen injection of LPS as well as only oral feeding of longan seed extract can enhance the capability of resisting inflammation of the SD rats.
Experiment 2
[0081] Treatments with longan seed extract obtained from a solvent having 50% of ethanol improve gout symptoms as discussed below.
[0082] 24 SD rats are grouped into three groups of eight SD rats in which first group is chosen as control group, second group chosen as treatment group, and third group chosen as longan seed group. Each SD rat has a weight of 200-250 g. Room temperature is kept at 23° C. Room is kept bright for 12-hour and dark for next 12-hour repeatedly. Water is treated by reverse osmosis.
[0083] SD rats in the control group is fed with water only.
[0084] Hypoxathine in the weight of 300 mg/Kg of SD rat and oxonic acid in the weight of 250 mg/Kg of SD rat are oral fed to the SD rats of the treatment group. Hypoxathine in the weight of 300 mg/Kg of SD rat, oxonic acid in the weight of 250 mg/Kg of SD rat, and longan seed of 0.1 wt % are oral fed to the SD rats of the longan seed group.
[0085] After one night of abstaining from food and drink, ether as anesthesia agent is administered to each SD rat. Next, serum from arterial blood of the SD rat is withdrawn for checking blood concentrations of uric acid by using Ciba-cornint 550. It is noted that data obtained by the experiment is subject to ANOVA.
[0086] As shown in FIGS. 4 and 4A , longan seed extract obtained from a solvent having 50% of ethanol lower about 32% of blood concentrations of uric acid of SD rats.
Experiment 3
[0087] 50 mmol/L of xanthine is prepared by using a buffer solution called PBS (phosphate buffered saline). 0.1-0.2 unit/ml of xanthine oxidase is prepared by using PBS. Following samples are prepared: (1) Preparation of pure water and preparation of longan seed extract therefrom. (2) Preparation of solution having 20% ethanol and preparation of longan seed extract therefrom. (3) Preparation of solution having 50% ethanol and preparation of longan seed extract therefrom. (4) Preparation of solution having 95% ethanol and preparation of longan seed extract therefrom. Allopurinol is taken as a positive control group. Xanthine oxidase is added to the control group. After five minutes, xanthine is added to the control group. Water is added to a blank control group. Xanthinie oxidase is added to each sample. After five minutes, xanthine is added to each sample. A spectrometer is used to emit light of wavelength of 290 nm to impinge on the samples and the control groups. Light absorption change is measured every 20-second for five minutes. Finally, enzyme activity is calculated. Xanthine oxidase inhibition ratio is defined by 1 minus enzyme activity of treatment group divided by enzyme activity of control group. As shown in FIG. 5B , a maximum of 60% xanthine oxidase inhibition ratio can be obtained.
Experiment 4
[0088] Gout toxicity elimination is tested below. Material is longan seed extract.
[0089] In an acute toxicity test, there are two groups each having 8-10 SD rats. Food is abstained from the groups but water is not abstained for one night. Oral feeding longan seed extract of 1 g/kg and 3 g/kg, and de-ionized water 1 ml/100 g to each SD rat for 28 consecutive days in which observing weight of each SD rat twice per day and weight of each SD rat is measured once per week. Thereafter, food is abstained from the SD rats for one night. Ether as anesthesia agent is administered to each SD rat. Next, serum from arterial blood of the SD rat is withdrawn for checking GOT, GPT (Glutamate Pyruvate Transaminase), albumin, globulin, and greatinine by using Ciba-cornint 550. It is noted that data obtained by the experiment is subject to ANOVA. Further, Dunnett check is conducted with value P less than 0.01 as great improvement.
[0090] Results are discussed below.
[0091] Acute toxicity test aims at obtaining a maximum sample in one administration that causes deaths of half of the tested animals. 1.0 ml/100 g of SD rat and 450 mg/ml concentration are the maximum amount per sample. 15 g/kg is the standard sample. Longan seed extract of 15 g/kg is administered to each of ten SD rats. Observation for 14 days. No deaths occur. Sample of LD50 is greater than 15 g/kg causing deaths of half of the SD rats. No significant differences are observed between SD rats of the control group and that of the treatment group after 14 days.
[0092] 28-day toxicity test aims at finding a sample that causes death of half SD rats. Further, one-fifth of the sample is taken as a maximum sample. 3 g/kg and 1 g/kg are taken as the maximum samples. Two treatment groups each have 8-1 SD rats. Oral feeding 3 g/kg of longan seed extract to SD rats of one treatment group and oral feeding 1 g/kg of longan seed extract to SD rats of the other treatment group are performed for 28 consecutive days. Thereafter, no deaths are found and there are no significant weight differences between the SD rats of treatment groups and the SD rats of a control group.
[0093] Serum from arterial blood of the SD rats of the treatment groups is withdrawn for check. As shown in FIG. 6A , there are no significant serum composition differences between the SD rats of treatment groups and the SD rats of a control group. Further, there are no significant weight differences of the liver and the kidneys between the SD rats of treatment groups and the SD rats of a control group. It is concluded that the administration of longan seed extract does not affect weight of organs of an SD rat, organs such as heart, liver, kidneys, testes, etc. of the SD rats of treatment groups functions normally, and no adverse effects to SD rats is confirmed.
Experiment 5
[0094] This is a sterilization experiment. Materials include 2.5 mg/ml of longan seed extract. A solution is made y adding water (obtained by reverse osmosis) to the longan seed extract. The solution is next filtered by a mini pore to produce a sterilized PBS.
[0095] Escherichia coli and Staphylococcus aureua are grown in an LB broth at 37° C. for 16 hours. Next, 1× PBS is used to wash the grown Escherichia coli and Staphylococcus aureua for three times in which a rotation of 3,000 rpm/minute for ten minutes is performed after each washing. A spectrometer is used to test OD value of the washed Escherichia coli and Staphylococcus aureua. Finally, Escherichia coli and Staphylococcus aureua having OD value of 0.3 is added to 1× PBS to prepare a solution which is in turn diluted with pure water to form a solution having the amount of Escherichia coli and Staphylococcus aureua 10% less than that prior to dilution. Next, the solution is reacted at 37° C. for one hour. Next, adding 5, 10, 20, 50, and 100 μl to the LB broth. Next, the solution is reacted at 37° C. for 18 hours. Next, calculate the number of Escherichia coli and Staphylococcus aureua. The solution treated with PBS is taken as treatment group and that treated with water (obtained from reverse osmosis) is taken as control group.
[0096] Above test is performed three times and results thereof are shown in FIGS. 5 , 5 A and 7 A. It is found that the number of Escherichia coli and Staphylococcus aureua of the treatment group is greatly decrease as compared with that of the control group. It is concluded that longan seed extract has the effect of killing Escherichia coli and Staphylococcus aureua. It is useful for inhibiting acne.
Experiment 6
[0097] This is also a sterilization experiment. Above sterilized PBS is used. Propionibacterium acne is grown in a BAP broth at 37° C. for 48 hours. Next, 1× PBS is used to wash the grown propionibacterium acne for three times in which a rotation of 3,000 rpm/minute for ten minutes is performed after each washing. A spectrometer is used to test OD value of the washed propionibacterium acne. Finally, propionibacterium acne having OD value of 0.3 is added to 1× PBS to prepare a solution which is in turn diluted with pure water to form a solution having the amount of propionibacterium acne 10% less than that prior to dilution. Next, the solution is reacted at 37° C. for one hour. Next, adding 5, 10, 20, 50, and 100 μl to the BAP broth. Next, the solution is reacted at 37° C. for 48 hours. Next, calculate the number of propionibacterium acne. The solution treated with PBS is taken as treatment group and that treated with water (obtained from reverse osmosis) is taken as control group.
[0098] Above test is performed three times and results thereof are shown in FIGS. 6 and 8A . It is found that the number of propionibacterium acne of the treatment group is greatly decrease as compared with that of the control group. It is concluded that longan seed extract has the effect of killing propionibacterium acne. It is useful for inhibiting acne.
Experiment 7
[0099] This is also a sterilization experiment. Above sterilized PBS is used. Trichopyhton rubrum is grown in an IMA (Inhibit mold agar) broth at 30° C. for 96 hours. Next, 1× PBS is used to wash the grown Trichopyhton rubrum for three times in which a rotation of 3,000 rpm/minute for ten minutes is performed after each washing. A spectrometer is used to test OD value of the washed Trichopyhton rubrum. Finally, Trichopyhton rubrum having OD value of 0.1 is added to 1× PBS to prepare a solution which is in turn diluted with pure water to form a solution having the amount of Trichopyhton rubrum 10% less than that prior to dilution. Next, the solution is reacted at 30° C. for one hour. Next, adding 5, 10, 20, 50, and 100 μl to the IMA broth. Next, the solution is reacted at 30° C. for 96 hours. Next, calculate the number of Trichopyhton rubrum. The solution treated with PBS is taken as treatment group and that treated with water (obtained from reverse osmosis) is taken as control group.
[0100] Above test is performed three times and results thereof are shown in FIGS. 9 and 9A . It is found that the number of Trichopyhton rubrum of the treatment group is greatly decrease as compared with that of the control group. It is concluded that longan seed extract has the effect of killing Trichopyhton rubrum. It is useful for inhibiting athlete's foot.
Experiment 8
[0101] This is a wound healing experiment. Materials include solving 5 g longan seed extract in 250 ml water to make a solution. The solution is then initially filtered by a filter paper. And in turn, the solution is filtered by a filter of 0.45 μm and another filter of 0.22 μm sequentially. A solution having 0 wt % of longan seed extract, a solution having 0.25 wt % of longan seed extract, a solution having 2.5 wt % of longan seed extract, a solution having 5.0 wt % of longan seed extract, and a solution having 10.0 wt % of longan seed extract are made for growing human epidermal keratinocytes (HEKa-C005-5C) as detailed below
[0102] Cells growth: 1×10 4 cells/ml human epidermal keratinocytes (HEKa-C005-5C) is prepared. KC (keratinocytes) and penicillian-streptomycin available from Cascade biologics, USA are grown in an incubator having 5% CO 2 at 37° C. Cells grown in this stage are called first cells. KC and penicillian-streptomycin are replenished every two days until the incubator is about 80% full of grown cells. Next, adding 0.25% trypsin-EDTA (ethylenediaminetetraacetate acid) solution having 0.25% trypsin and 0.02% EDTA. Next, it is reacted at 37° C. for 5 minutes. Cells grown in this stage called second cells. Floated KC is washed with a solution having more than 10% clean water for neutralization. Next, the solution is poured into a centrifuge which is in turn rotated at 1,500 rpm for 10 minutes for removing fine solids. Next, KC and penicillian-streptomycin are used again to float cells. Next, the solution is diluted in a 1:3 ratio with water. Finally, cells are grown in an incubator having 5% CO 2 at 37° C. Cells grown in this stage called third cells.
[0103] Cells growth test is next performed by means of crystal violet. HEKa-C005-5C is grown for 24, 48, and 72 hours continuously. Next, a microscope is used to observe cells growth. Clean water of 200 μl is used to wash the grown cells. Next, cells are fixed for 20 minutes by a cells fixation solution. PBST of 200 μl is used to wash the grown cells twice. Adding crystal violet of 100 μl into the solution to change color in room temperature for 30 minutes. Next, clean water of 200 μl is used to wash the grown cells trice. 1% SDS (sodium dodecyl sulfate) is used to solve cells. Rotating the solution in room temperature for 1 hour. Crystal violet attached to cells are extracted. A spectrometer is used to emit light of wavelength of 595 nm to impinge on the extract in order to measure the OD value. Further, light of wavelength of 650 nm is emitted to impinge on the extract to change the OD value. Solution without longan seed extract is taken as control group to obtain growth factors.
[0104] Human epidermal keratinocytes growth factors are determined by means of ELISA. Human epidermal keratinocytes are collected. Growth factors of the collected human epidermal keratinocytes are determined by means of commercial kits. Microtitration plate of 96 well plates is chosen. Bovine serum albumin is used for inhibition. Next, PBS-Tween is used to wash the microtitration plate. Clean solution of 100 μl is add for reaction at 37° C. for two hours. Next, PBS-Tween is used to was again. Next, rabbit-anti-growth factor Ab-HRP available from Chemicon, Temmecula, Calif. is added for reaction at 37° C. for two hours. Next, it is washed again. Next, colored substrate having O-phenyldiamine is added. Next, 50 μl of 2N H 2 SO 4 is added to stop reaction. Next, OD value at wavelength 450 nm is measured. Finally, vascular endothelial growth factor (VEGF) is determined
[0105] Results are shown in FIGS. 8 and 10 . It is found that effects of crystal violet dying method for determining growth factor can be observed by means of a microscope. It is shown that samples with 2.5%, 5.0% and 10% of dose can increase human epidermal keratinocytes growth factors more than 1.25, 1.26 and 1.50 times as compared with control group. Particularly, the sample with 10% of dose having a p-value less than 0.05 is advantageous because it means that 10% longan seed extract can greatly increase human epidermal keratinocytes growth factors.
[0106] Results obtained by means of ELISA test are shown in FIGS. 9 and 11 . In the columns “CI (collagen I) (μg/ml)” and “FN (fibronectin) (pg/ml)”, after adding 5% and 10% longan seed extract, VEGF is increased greatly (p<0.05). This means that wound treated with longan seed extract can be quickly healed.
[0107] It is envisaged by the invention that the advantages of healing inflammation, lowering uric acid, killing micro-organisms, increasing human epidermal keratinocytes growth, and helping wound healing without hurting organs can be obtained.
[0108] While the invention has been described in terms of preferred embodiments, those skilled in the art will recognize that the invention can be practiced with modifications within the spirit and scope of the appended claims. | A method of making longan seed extract is provided with choosing an extraction solvent; heating the extraction solvent to a first predetermined temperature; adding pulverized longan seed to the extraction solvent to prepare a solution; maintaining the solution at a second temperature for a predetermined period of time to obtain an extracted substance; filtering the extracted substance; and drying and cooling the filtered extracted substance to produce an extract. | 0 |
FIELD OF THE INVENTION
[0001] The present invention relates to an improved speaker enclosure. In particular, it relates to a speaker enclosure for producing improved sound performance.
BACKGROUND OF THE INVENTION
[0002] Conventionally, speaker enclosures are typically made of wood material having a rectangular shape. The range of speaker enclosures in the market are varied and are used for applications ranging from home use to professional use, including but not limited to outdoor performances.
[0003] Typically, the speaker enclosures used for professional use are generally large and heavy. The weight and bulk of the speaker enclosures make transportation and movement difficult. Apart from the weight, the materials used for speaker enclosures affect the sound performance of the speaker by absorbing vibrations. Speaker enclosures made of different material such as plywood, birch or Medium-Density Fibreboard (“MDF”) have different degree of effectiveness in absorbing undesirable vibrations. Such damping materials have been used internal of the speaker enclosures to reduce undesirable vibrations.
[0004] The panels for forming the speaker enclosure prevent sound waves generated by the rearward facing speaker driver interacting with sound waves generated at the front of the speaker driver, such forward and rearward-generated sound waves are out of phase with each other, any interaction between the two sound waves in the listening space creates distortion of the original sound waves as they were intended to be reproduced. It thus avoids internal standing sound waves. Such panels help to prevent distortion of the sound produced by the speakers and prevent the magnification of unwanted frequencies causing undesirable effects when sound is of a high frequency. It further enhances the quality of sound when it is of mid-frequency.
[0005] One way of addressing the above problems can be found in U.S. Pat. No. 3,804,195, which discloses a loudspeaker enclosure made out of corrugated sheets of material. The corrugated sheets of material include hollow portions. Each of these sheets is joined together in a box-like configuration. Another example can be found in U.S. Pat. No. 4,811,403 which discloses a lightweight loudspeaker enclosure that uses a rigid lightweight honeycombed material in part of the speaker enclosure.
[0006] While weight and improved sound performances resulted from the constructions of speaker enclosures found in the above patents, vibrations still remained due to seams joining each of the pieces of the enclosure. Vibrations are induced at the seams and joints reducing overall sound performance of the speakers.
[0007] To address this problem, U.S. Pat. No. 5,519,178 discloses a speaker enclosure having a substantially seamless rigid outer skin, a middle sound absorbing layer, and a substantially seamless flexible skin. The outer skin is formed from multiple layers of resin impregnated carbon fiber, the middle sound absorbing layer includes pieces of honeycomb material and the inner layer is formed from multiple layers of resin impregnated fiberglass. The layers of material are arranged in a substantially seamless manner into a mold and then cured by vacuum bagging and heating thereby producing a strong, lightweight speaker enclosure capable of producing overall good quality sound. However, due to the methods used to manufacture the enclosure, the manufacturing method requires precise quality control leading to high manufacturing costs.
[0008] There is therefore a need for a durable, light weight speaker enclosure capable of minimizing distortion of sound signals but yet relatively easy and inexpensive to manufacture.
[0009] Any discussion of documents, devices, acts or knowledge in this specification is included to explain the context of the invention. It should not be taken as an admission that any of the material forms a part of the state of the art or the common general knowledge in the relevant art in Singapore or elsewhere on or before the priority date of the disclosure and claims herein. All statements as to the date or representation as to the contents of these documents is based on the information available to the applicant and does not constitute any admission as to the correctness of the date or contents of these documents.
Object of the Invention
[0010] It is an object of the present invention to overcome, or at least substantially ameliorate, the disadvantages and shortcomings of the prior art.
[0011] Other objects and advantages of the present invention will become apparent from the following description, taken in connection with the accompanying drawings, wherein, by way of illustration and example, an embodiment of the present invention is disclosed.
SUMMARY OF THE INVENTION
[0012] According to a first aspect of the present invention, there is provided a loud speaker enclosure comprising a casing having a main body and a cap at each end of the main body to define the interior volume of the enclosure, the main body having a plurality of side walls, the side walls including a first layer, a middle layer and a second layer to form a panel, wherein the plurality of side walls are formed from a single panel for folding to form the main body of the enclosure.
[0013] In a preferred embodiment, a resilient material is laminated on the first layer which faces the interior volume of the enclosure.
[0014] In another preferred embodiment, the panel comprises a plurality of slit joints wherein each slit joint extends transversely across the panel for forming a fold.
[0015] Preferably, the slit joint is a groove extending at least partially through the depth of the panel.
[0016] Preferably, the groove has a V-shaped profile.
[0017] In a preferred embodiment, the groove has a L-shaped profile.
[0018] Preferably, the middle layer is a honeycomb configuration made of metal.
[0019] Preferably, the first layer and the second layer is a metal material, combination of carbon fibre, fibre glass, polypropylene or foam material.
[0020] Preferably, the first layer and second layer is aluminium.
[0021] Preferably, the plurality of side walls is of a curved configuration.
[0022] According to a second aspect of the present invention, there is provided a method of forming a loudspeaker enclosure comprising the following steps:
a) Combining a first layer of a sheet material, a middle layer of a cored configuration and a second layer of the sheet material by using adhesive to form a panel; b) Laminating a sheet of resilient material on the panel; c) Forming a plurality of grooves extending partially through the depth of the panel, each of the grooves extending transverse to the panel such that the panel can be folded at the groove to form an enclosed main body; d) Bending the panel at the location of the grooves to form the enclosed main body; e) Capping the enclosed main body with a top wall and a bottom wall with separate panels wherein the main body, the top wall and the bottom wall defines the interior volume of the enclosure.
[0028] In a preferred embodiment, forming the plurality of grooves comprises cutting at least partially through the depth of the panel.
[0029] In yet another preferred embodiment, each of the plurality of grooves has a V shaped profile.
[0030] Preferably, each of the plurality of grooves has a L shaped profile.
[0031] Preferably, the method comprises a further step of using adhesive to adhere the plurality of grooves to the panel.
[0032] Preferably, the method comprising a further step of heat treating the panel to adhere plurality of grooves to the panel.
[0033] Preferably, the first layer and second layer are made of metal, combination of carbon fibre, fibre glass, polypropylene or foam.
[0034] Preferably, the first and second layer is made of aluminium.
[0035] Preferably, the cored configuration includes a honeycomb arrangement.
[0036] In a preferred embodiment, the cored configuration includes a corrugated arrangement.
[0037] In a preferred embodiment, the cored configuration includes a fluted arrangement.
[0038] In a preferred embodiment, the cored configuration is made of foam.
[0039] This invention may also be said broadly to consist in the parts, elements and features referred to or indicated in the specification of the application, individually or collectively, and any or all combinations of any two or more of said parts, elements or features, and where specific integers are mentioned herein which have known equivalents in the art to which this invention relates, such known equivalents are deemed to be incorporated herein as if individually set forth.
BRIEF DESCRIPTION OF DRAWINGS
[0040] In order that the invention may be better understood and put into practical effect, the invention will now be described, by way of example only, with reference to the accompanying drawings, in which:
[0041] FIG. 1 is an exploded perspective view of a loudspeaker enclosure;
[0042] FIG. 2 a is a cross-sectional view of a panel for forming the loudspeaker enclosure;
[0043] FIG. 2 b is a cross-sectional view of an alternative panel for forming the loudspeaker enclosure;
[0044] FIG. 2 c is a cross-sectional view of another alternative panel for forming the loudspeaker enclosure;
[0045] FIG. 3 a is a cross-sectional perspective view of a panel having a middle layer which has honeycomb arrangement;
[0046] FIG. 3 b is a cross-sectional perspective view of a panel having a middle layer which is corrugated;
[0047] FIG. 3 c is a cross-sectional perspective view of a panel having a middle layer which is fluted;
[0048] FIG. 3 d is a cross-sectional perspective view of a panel having a middle layer which is made of foam;
[0049] FIG. 4 is an exploded perspective view of the layers of a panel for forming a loudspeaker enclosure;
[0050] FIG. 5 is a perspective view of the panel indicating the slots formed at various locations on the depth of the panel;
[0051] FIG. 6 is cross-sectional view of the panel indicating the different types of slots formed on the depth of the panel;
[0052] FIG. 7 is a perspective view of the top and bottom caps of the main body sandwiching a middle layer of a honeycomb arrangement;
[0053] FIG. 8 is a perspective view of the loudspeaker enclosure in its final assembled form;
[0054] FIG. 9 is a graph of decibels versus kilohertz comparing the quality of sound produced by a loudspeaker of the present invention and a conventional high end speaker.
DETAILED DESCRIPTION OF INVENTION
[0055] The present invention will now be described in detail in connection with preferred embodiments with reference to the accompanying drawings.
[0056] FIG. 1 illustrates a speaker enclosure 100 according to an embodiment of the present invention. The speaker enclosure 100 comprises three basic component parts, a main body 10 , a top cap 11 and a bottom cap 13 for the main body 10 to define the casing for the speaker enclosure. The main body 10 defines an interior volume of space in which one or more speakers or tweeters, speaker drivers and associated electronic hardware, such as crossover circuits and amplifiers (all not shown) are mounted. In the embodiment shown in FIG. 1 , the main body 10 is shown to have 6 side walls forming the main body. Alternatively, a rectangular shaped main body would be possible. The construction of the speaker enclosure 100 is therefore readily adaptable to various sizes and shapes and not limited to the exact enclosure shown in FIG. 1 .
[0057] The baffle section 12 comprises one of the side walls of the main body. The baffle section 12 includes one or more openings 14 where the speakers (not shown) are mounted within the enclosure such that the diaphragm portions of the speakers communicate through the openings 14 to the outside of the speaker enclosure.
[0058] The top cap 11 and the bottom cap 13 are dimensioned and cut to shape to fit the top and bottom of the side walls, of the main body. The top cap 11 and the bottom cap 13 may be formed of a panel of the same construction as that used for the main body 10 .
[0059] FIG. 2 illustrates a partial cross-sectional view of a cut away portion of the main body 10 . The main body 10 of the enclosure comprises of four main layers. A first layer 21 and a second layer 22 , both comprising sheets of a material made of metal, are spaced apart to provide for a middle layer 23 of general core configuration, the configuration of which will be explained in detail later. In a preferred embodiment, the sheets of material and the core configuration are made of aluminium. Alternatively, the sheets of material and the core configuration may be made of a combination of carbon fibre, fibre glass, polypropylene, or foam. A flexible sheet of resilient material 24 combines with either the first or second layers by adhesive means. In a preferred embodiment, the resilient material 24 may be made of rubber. Different configurations of resilient material may be possible. FIG. 2 a shows a sheet of resilient material 24 of a corrugated configuration. FIG. 2 b shows a relatively thin tapering sheet of resilient material 24 while FIG. 2 c shows a relatively thick and flat sheet of resilient material. The resilient material 24 is located within the interior volume of the speaker enclosure 100 . The resilient material 24 acts as a dampener and combines with the 3 layers to prevent sound waves generated by the rearward facing speaker driver interacting with sound waves generated at the front of the speaker driver, such forward and rearward-generated sound waves are out of phase with each other, any interaction between the two sound waves in the listening space creates distortion of the original sound waves as they were intended to be reproduced. It thus avoids internal standing sound waves. They help to prevent distortion of the sound produced by the speakers and prevent the magnification of unwanted frequencies causing undesirable effects when sound is of a high frequency. It further enhances the quality of sound when it is of mid-frequency. The plurality of air pockets within the material of the middle layer 23 also serve to reduce the vibration of the second layer 22 . This middle layer further serves to isolate sound from transmitting from the interior space of the speaker enclosure to the outside of the speaker enclosure.
[0060] FIGS. 3 a , 3 b , 3 c and 3 d illustrate middle layers of different core configurations 25 , 26 , 27 and 28 for the construction of the panel. The middle layer generally comprises a material having a plurality of air pockets located within. The middle layer and the resilient material 24 act as dampener, at the same time, they prevent sound waves generated by the rearward facing speaker driver interacting with sound waves generated at the front of the speaker driver, such forward and rearward-generated sound waves are out of phase with each other, any interaction between the two sound waves in the listening space creates distortion of the original sound waves as they were intended to be reproduced. It thus avoids internal standing sound waves. Such panels help to prevent distortion of the sound produced by the speakers and prevent the magnification of unwanted frequencies causing undesirable effects when sound is of a high frequency. It further enhances the quality of sound when it is of mid-frequency. The plurality of air pockets within the material of the middle layer 23 also serve to reduce the vibration of the second layer 22 . This middle layer 23 further serves to isolate sound from transmitting from the interior space of the speaker enclosure to the outside of the speaker enclosure.
[0061] FIG. 3 a illustrates ,a middle layer having a honeycomb arrangement 25 . FIG. 3 b shows a middle layer having a corrugated core configuration 26 . FIG. 3 c shows a middle layer having a fluted configuration 27 while FIG. 3 d shows a middle layer using foam core 28 which serves as an effective dampener. As mentioned above, the core configuration may be made of metal, a combination of carbon fibre, fibre glass, polypropylene, or foam. In a preferred embodiment, the core configuration is made of aluminium. The construction of the core configuration is therefore readily adaptable to various configurations and not limited to the shown in FIGS. 3 a , 3 b , 3 c and 3 d.
[0062] FIG. 4 illustrates a perspective view of how the main body 10 of the speaker enclosure is formed from a single panel 30 . The single panel 30 is constructed from combining the first layer, second layer and the middle layer using adhesive to combine the layers together. A single sheet of resilient material with the same dimensions as the panel 30 can be laminated over the first or second layer. The resilient material will define the interior volume of the enclosure. Forming the main body 10 from a single panel provides significant advantages. Firstly, the external part of the main body 10 of the speaker enclosure appears to be seamless. This design improves the quality of the sound produced from the speaker by reducing the painful effects of the high frequencies while making the mid frequencies more pronounced. It also minimizes internal standing waves. Secondly, costs of manufacturing such a speaker enclosure are lowered significantly due to the ease of constructing the main body 10 , the method of which will be explained hereinafter. FIG. 4 shows the panel 30 being folded to form side walls 34 of the enclosure with a side wall of one end of the panel joining the side wall at the opposing end of the panel to define the interior space of the speaker enclosure. One of the side walls 34 may include openings 14 to form the baffle section 12 for allowing the speaker mounted within the enclosure so that the diaphragm portions of the speakers can communicate through the openings 14 to the outside of the speaker enclosure.
[0063] FIG. 5 illustrates the single panel 30 flat on a surface (not shown) before being folded to form the main body 10 of the speaker enclosure. Once the panel 30 is formed from the four layers, a groove or slot 40 is formed at the part where the panel can be folded. The groove 40 is made by cutting partially through the depth of the panel 30 such that the panel will not be severed into separate parts. The cut may be made by a Computer Numerical Control (CNC) machine where precision cutting is possible. It is envisaged that many possible shapes of speaker enclosures can be formed by forming grooves 40 across the width of the panel 30 . For example, a main body having a rectangular or square profile would. require 3 grooves to form 3 foldable regions for folding into a main body.
[0064] FIG. 6 illustrates a cross sectional view of the panel 30 and the grooves 40 made along the panel for folding. For the purposes of folding to form the speaker enclosure, two types of grooves can be made through the depth of the panel. The first is a cut having a V-shaped profile. The second is a cut having a L-shaped profile. Typically, the type of groove to be formed depends on the degree of foldability required at the folding region. The greater the degree of foldability required to bend the side walls 34 into an enclosure, the more the groove will need to adopt a L-shaped profile.
[0065] FIG. 7 illustrates the method of forming the top and bottom caps of the main body in order to close the ends of the main body to define the interior volume of the speaker enclosure. A sheet of material 51 , preferably aluminium is cut to shape corresponding to the cross section profile of the main body. A plurality of openings is drilled into the sheet for mounting purposes. A similar sheet of material 52 , preferably also aluminium, is cut to shape corresponding to the cross section profile of the main body. Holes are similarly drilled into the sheet of material. A middle layer 23 having a cored configuration, as mentioned above, is then adhered together with the two sheets of materials 51 , 52 to form the top and bottom caps of the main body.
[0066] FIG. 8 illustrates the speaker enclosure 100 in its final assembled form.
[0067] FIG. 9 illustrates the graphical result of sound tests conducted on two speaker enclosures of similar dimensions, one a preferred embodiment of the present invention and a conventional speaker enclosure commercially available in the market. The conventional speaker is a Fohhn AT22 10″ 2 way speaker system. The result presented in the graph of decibels versus kilohertz compares the quality of sound produced by a loudspeaker enclosure of a preferred embodiment 60 and the conventional high end speaker 70 . The result shows that at the same frequency, particularly at the higher frequencies, the sound from the preferred embodiment of the present invention 60 had a relatively lower decibel result. In use, the effect of this result to a listener would mean that at sound of higher frequencies, the painful effects would be reduced, leading to a more pleasant hearing sensation to the ears. Further, sounds of mid frequencies are also more linear in the preferred embodiment of the present invention leading to a more pleasant listening experience.
[0068] Although the invention has been herein shown and described in what is conceived to be the most practical and preferred embodiment, it is recognized that departures can be made within the scope of the invention, which is not to be limited to the details described herein but is to be accorded the full scope of the appended claims so as to embrace any and all equivalent devices and apparatus.
[0069] ‘Comprises/comprising’ when used in this specification is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps, components or groups thereof. | A loud speaker enclosure and a method of forming the loudspeaker enclosure comprising the following steps: combining a first layer of a sheet material, a middle layer of a cored configuration and a second layer of the sheet material by using adhesive to form a panel; laminating a sheet of resilient material on the panel; forming a plurality of grooves extending partially through the depth of the panel, each of the grooves extending transverse to the panel such that the panel can be folded at the groove to form an enclosed main body; bending the panel at the location of the grooves to form the enclosed main body; capping the enclosed main body with a top wall and a bottom wall with separate panels wherein the main body, the top wall and the bottom wall defines the interior volume of the enclosure. | 8 |
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