JP2767759B2 - 特性を改良した超吸収性アクリルポリマーと、その製造方法 - Google Patents
特性を改良した超吸収性アクリルポリマーと、その製造方法Info
- Publication number
- JP2767759B2 JP2767759B2 JP6252987A JP25298794A JP2767759B2 JP 2767759 B2 JP2767759 B2 JP 2767759B2 JP 6252987 A JP6252987 A JP 6252987A JP 25298794 A JP25298794 A JP 25298794A JP 2767759 B2 JP2767759 B2 JP 2767759B2
- Authority
- JP
- Japan
- Prior art keywords
- acrylic
- crosslinking agent
- hlb
- superabsorbent
- acrylic monomer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229920000058 polyacrylate Polymers 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012530 fluid Substances 0.000 claims abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 26
- 239000000178 monomer Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 21
- 238000010521 absorption reaction Methods 0.000 claims description 19
- 238000006116 polymerization reaction Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical group CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 239000012429 reaction media Substances 0.000 claims description 3
- 229920000247 superabsorbent polymer Polymers 0.000 claims description 3
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 238000010557 suspension polymerization reaction Methods 0.000 claims description 2
- -1 acryl Chemical group 0.000 claims 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 claims 1
- 239000005720 sucrose Substances 0.000 claims 1
- 125000000185 sucrose group Chemical group 0.000 claims 1
- 230000000704 physical effect Effects 0.000 abstract description 2
- 239000007900 aqueous suspension Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000243 solution Substances 0.000 description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 235000013681 dietary sucrose Nutrition 0.000 description 5
- 229960004793 sucrose Drugs 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000004148 curcumin Substances 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 229940035044 sorbitan monolaurate Drugs 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012632 extractable Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010558 suspension polymerization method Methods 0.000 description 2
- 210000002700 urine Anatomy 0.000 description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- ARLZGEXVMUDUQZ-UHFFFAOYSA-N O.O.[Ca] Chemical compound O.O.[Ca] ARLZGEXVMUDUQZ-UHFFFAOYSA-N 0.000 description 1
- 206010046543 Urinary incontinence Diseases 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- FBDWCTWJJMORIU-UHFFFAOYSA-N magnesium;hexahydrate Chemical compound O.O.O.O.O.O.[Mg] FBDWCTWJJMORIU-UHFFFAOYSA-N 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Hematology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Graft Or Block Polymers (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9311231A FR2710342B1 (fr) | 1993-09-21 | 1993-09-21 | Polymères acryliques superabsorbants à propriétés améliorées et leur procédé d'obtention. |
| FR9311231 | 1993-09-21 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07116511A JPH07116511A (ja) | 1995-05-09 |
| JP2767759B2 true JP2767759B2 (ja) | 1998-06-18 |
Family
ID=9451073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6252987A Expired - Lifetime JP2767759B2 (ja) | 1993-09-21 | 1994-09-21 | 特性を改良した超吸収性アクリルポリマーと、その製造方法 |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US5563218A (enExample) |
| EP (1) | EP0644211B1 (enExample) |
| JP (1) | JP2767759B2 (enExample) |
| CN (1) | CN1102832A (enExample) |
| AT (1) | ATE158598T1 (enExample) |
| DE (1) | DE69405839D1 (enExample) |
| FR (1) | FR2710342B1 (enExample) |
| SG (1) | SG52726A1 (enExample) |
| TW (1) | TW300229B (enExample) |
Families Citing this family (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19600405A1 (de) * | 1996-01-08 | 1997-07-10 | Basf Ag | Verfahren zur Herstellung von wasserunlöslichen Polymerisaten |
| FR2748404B1 (fr) | 1996-05-09 | 1998-07-24 | Atochem Elf Sa | Poudres superabsorbantes a forte absorption et forte sucion capillaire |
| DE69815670T2 (de) | 1997-04-18 | 2004-04-22 | The Procter & Gamble Company, Cincinnati | Verwendung von hydrogelformende polymere in absorbierende materialen zur aufnahme von körperflüssigkeiten |
| DE19717968A1 (de) * | 1997-04-28 | 1998-10-29 | Henkel Kgaa | Verfahren zur Herstellung von Kohlenhydratpartialestern |
| US6304701B1 (en) | 1998-03-27 | 2001-10-16 | Corning Cable Systems Llc | Dry fiber optic cable |
| FR2815272B1 (fr) * | 2000-10-18 | 2002-12-27 | Braun Medical | Comprime de superabsorbant et ses utilisations |
| KR100697944B1 (ko) | 2003-02-10 | 2007-03-20 | 니폰 쇼쿠바이 컴파니 리미티드 | 수분-흡수제 |
| EP1609810B1 (en) | 2003-03-17 | 2013-01-16 | Sumitomo Seika Chemicals Co., Ltd. | Process for production of water-absorbing resin particles |
| CN100379764C (zh) * | 2003-05-13 | 2008-04-09 | 住友精化株式会社 | 制造吸水树脂的方法 |
| WO2005063825A1 (ja) * | 2003-12-25 | 2005-07-14 | Sumitomo Seika Chemicals Co., Ltd. | 吸水性樹脂の製造方法 |
| CN101589066B (zh) | 2007-01-24 | 2013-07-03 | 株式会社日本触媒 | 粒子状吸水性聚合物及其制造方法 |
| US9457048B2 (en) | 2008-02-05 | 2016-10-04 | Wellosophy Corporation | Absorbent ingestible agents and associated methods of manufacture and use |
| US8628837B2 (en) | 2011-11-14 | 2014-01-14 | Empire Technology Development Llc | Composite and methods of making and using the same |
| CN103113508B (zh) * | 2013-01-23 | 2015-05-20 | 江苏苏博特新材料股份有限公司 | 一种具有较慢吸液速率的高吸水树脂、其制备方法及其应用 |
| KR101871968B1 (ko) | 2015-06-01 | 2018-06-27 | 주식회사 엘지화학 | 고흡수성 수지 |
| KR101949454B1 (ko) | 2015-06-15 | 2019-02-18 | 주식회사 엘지화학 | 고흡수성 수지 |
| KR101949995B1 (ko) | 2015-07-06 | 2019-02-19 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 및 이로부터 제조된 고흡수성 수지 |
| KR101855351B1 (ko) | 2015-08-13 | 2018-05-04 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| KR101921278B1 (ko) | 2015-12-23 | 2018-11-22 | 주식회사 엘지화학 | 고흡수성 수지, 및 이의 제조 방법 |
| WO2017146347A1 (ko) | 2016-02-25 | 2017-08-31 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| KR101853401B1 (ko) | 2016-03-11 | 2018-04-30 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법, 및 고흡수성 수지 |
| KR101958014B1 (ko) | 2016-03-14 | 2019-03-13 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| KR102162500B1 (ko) | 2016-12-13 | 2020-10-06 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| KR20180067940A (ko) | 2016-12-13 | 2018-06-21 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| KR102075733B1 (ko) | 2016-12-13 | 2020-02-10 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| KR102094453B1 (ko) | 2016-12-23 | 2020-03-27 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| KR102167661B1 (ko) | 2017-02-10 | 2020-10-19 | 주식회사 엘지화학 | 고흡수성 수지 및 이의 제조 방법 |
| JP6681492B1 (ja) * | 2018-12-12 | 2020-04-15 | 住友精化株式会社 | 吸水性樹脂粒子 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61275355A (ja) * | 1985-05-29 | 1986-12-05 | Kao Corp | 吸収性物品 |
| FR2624864B1 (fr) * | 1987-12-18 | 1990-06-01 | Hoechst France | Dispersions eau dans l'huile de polymeres hydrophiles, a base d'acide acrylique partiellement ou totalement salifie par de l'ammoniac, leur procede de preparation et leur application notamment dans l'impression pigmentaire |
| JP2938920B2 (ja) * | 1990-01-31 | 1999-08-25 | 住友精化株式会社 | 吸水性樹脂の製造方法 |
| US5106929A (en) * | 1990-10-01 | 1992-04-21 | Phillips Petroleum Company | Superabsorbent crosslinked ampholytic ion pair copolymers |
| FR2694757B1 (fr) * | 1992-08-12 | 1994-10-07 | Atochem Elf Sa | Procédé pour la préparation de polyacrylates superabsorbants à faible teneur en monomères résiduels. |
| FR2694755B1 (fr) * | 1992-08-12 | 1994-09-23 | Atochem Elf Sa | Perfectionnement pour la préparation de poudre superabsorbantes par polymérisation en suspension inverse de monomères acryliques. |
-
1993
- 1993-09-21 FR FR9311231A patent/FR2710342B1/fr not_active Expired - Fee Related
-
1994
- 1994-07-19 SG SG1996008334A patent/SG52726A1/en unknown
- 1994-07-19 EP EP94401653A patent/EP0644211B1/fr not_active Expired - Lifetime
- 1994-07-19 AT AT94401653T patent/ATE158598T1/de active
- 1994-07-19 DE DE69405839T patent/DE69405839D1/de not_active Expired - Lifetime
- 1994-08-01 TW TW083107025A patent/TW300229B/zh active
- 1994-08-25 US US08/294,794 patent/US5563218A/en not_active Expired - Fee Related
- 1994-09-21 JP JP6252987A patent/JP2767759B2/ja not_active Expired - Lifetime
- 1994-09-21 CN CN94116454A patent/CN1102832A/zh active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| FR2710342A1 (fr) | 1995-03-31 |
| DE69405839D1 (de) | 1997-10-30 |
| EP0644211B1 (fr) | 1997-09-24 |
| TW300229B (enExample) | 1997-03-11 |
| ATE158598T1 (de) | 1997-10-15 |
| JPH07116511A (ja) | 1995-05-09 |
| EP0644211A1 (fr) | 1995-03-22 |
| CN1102832A (zh) | 1995-05-24 |
| SG52726A1 (en) | 1998-09-28 |
| FR2710342B1 (fr) | 1995-11-17 |
| US5563218A (en) | 1996-10-08 |
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