TW575613B - Method of making an aqueous dispersion of fluoropolymers - Google Patents
Method of making an aqueous dispersion of fluoropolymers Download PDFInfo
- Publication number
- TW575613B TW575613B TW090108921A TW90108921A TW575613B TW 575613 B TW575613 B TW 575613B TW 090108921 A TW090108921 A TW 090108921A TW 90108921 A TW90108921 A TW 90108921A TW 575613 B TW575613 B TW 575613B
- Authority
- TW
- Taiwan
- Prior art keywords
- item
- patent application
- dispersion
- scope
- fluoropolymer
- Prior art date
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 75
- 239000004811 fluoropolymer Substances 0.000 title claims abstract description 29
- 229920002313 fluoropolymer Polymers 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 11
- 239000012875 nonionic emulsifier Substances 0.000 claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005341 cation exchange Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229920001973 fluoroelastomer Polymers 0.000 claims 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 1
- 239000011707 mineral Substances 0.000 claims 1
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 30
- 239000007788 liquid Substances 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 6
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 6
- 150000001336 alkenes Chemical class 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 239000004815 dispersion polymer Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007962 solid dispersion Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 235000019687 Lamb Nutrition 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical compound FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000004446 fluoropolymer coating Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- -1 hexamethylene acrylic acid Chemical compound 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- 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
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/16—Purification
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Paints Or Removers (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10018853A DE10018853C2 (de) | 2000-04-14 | 2000-04-14 | Herstellung wässriger Dispersionen von Fluorpolymeren |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| TW575613B true TW575613B (en) | 2004-02-11 |
Family
ID=7638956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW090108921A TW575613B (en) | 2000-04-14 | 2001-04-13 | Method of making an aqueous dispersion of fluoropolymers |
Country Status (12)
| Country | Link |
|---|---|
| EP (1) | EP1274771B1 (enExample) |
| JP (1) | JP2003531232A (enExample) |
| CN (1) | CN1177883C (enExample) |
| AT (1) | ATE301151T1 (enExample) |
| AU (1) | AU2001249959A1 (enExample) |
| CA (1) | CA2403957A1 (enExample) |
| DE (2) | DE10018853C2 (enExample) |
| PL (1) | PL357819A1 (enExample) |
| RU (1) | RU2288923C2 (enExample) |
| TW (1) | TW575613B (enExample) |
| WO (1) | WO2001079332A1 (enExample) |
| ZA (1) | ZA200209244B (enExample) |
Families Citing this family (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7279522B2 (en) | 2001-09-05 | 2007-10-09 | 3M Innovative Properties Company | Fluoropolymer dispersions containing no or little low molecular weight fluorinated surfactant |
| WO2004050719A1 (ja) * | 2002-11-29 | 2004-06-17 | Daikin Industries, Ltd. | 含フッ素ポリマー水性エマルション精製方法、精製エマルション及び含フッ素加工品 |
| EP1441014A1 (en) * | 2003-01-22 | 2004-07-28 | 3M Innovative Properties Company | Aqueous fluoropolymer dispersion comprising a melt processible fluoropolymer and having a reduced amount of fluorinated surfactant |
| EP1452571B1 (en) * | 2003-02-28 | 2005-08-17 | 3M Innovative Properties Company | Fluoropolymer dispersion containing no or little low molecular weight fluorinated surfactant |
| ITMI20032050A1 (it) | 2003-10-21 | 2005-04-22 | Solvay Solexis Spa | Processo per la preparazione di dispersori di fluoropolimeri. |
| EP1529785B1 (en) | 2003-10-24 | 2011-03-16 | 3M Innovative Properties Company | Aqueous dispersions of polytetrafluoroethylene particles |
| ATE529451T1 (de) | 2003-11-17 | 2011-11-15 | 3M Innovative Properties Co | Wässrige ptfe-dispersionen mit einem niedrigen gehalt an fluorierten emulgatoren |
| ITMI20040031A1 (it) | 2004-01-14 | 2004-04-14 | Solvay Solexis Spa | Processo per la preparazione di dispersori di fluoropolimeri |
| ATE433350T1 (de) * | 2004-03-01 | 2009-06-15 | 3M Innovative Properties Co | Verfahren zum beschichten eines gegenstands mit einer fluorhaltigen kunststoffsdispersion |
| JP4788139B2 (ja) * | 2004-12-17 | 2011-10-05 | 旭硝子株式会社 | ポリテトラフルオロエチレン水性分散液 |
| ITMI20050705A1 (it) | 2005-04-20 | 2006-10-21 | Solvay Solexis Spa | Processo per la preparazione di dispersori di fluoropolimeri |
| US8814861B2 (en) | 2005-05-12 | 2014-08-26 | Innovatech, Llc | Electrosurgical electrode and method of manufacturing same |
| US8338518B2 (en) | 2005-06-10 | 2012-12-25 | Arkema Inc. | Aqueous process for making a stable fluoropolymer dispersion |
| US20060281845A1 (en) * | 2005-06-10 | 2006-12-14 | Ramin Amin-Sanayei | Aqueous process for making fluoropolymers |
| GB0523853D0 (en) | 2005-11-24 | 2006-01-04 | 3M Innovative Properties Co | Fluorinated surfactants for use in making a fluoropolymer |
| GB0525978D0 (en) | 2005-12-21 | 2006-02-01 | 3M Innovative Properties Co | Fluorinated Surfactants For Making Fluoropolymers |
| US7671112B2 (en) | 2005-07-15 | 2010-03-02 | 3M Innovative Properties Company | Method of making fluoropolymer dispersion |
| GB0514398D0 (en) | 2005-07-15 | 2005-08-17 | 3M Innovative Properties Co | Aqueous emulsion polymerization of fluorinated monomers using a fluorinated surfactant |
| US20080015304A1 (en) | 2006-07-13 | 2008-01-17 | Klaus Hintzer | Aqueous emulsion polymerization process for producing fluoropolymers |
| JP2007231072A (ja) * | 2006-02-28 | 2007-09-13 | Three M Innovative Properties Co | コーティング組成物及びそれを使用した物品 |
| EP1845116A1 (en) * | 2006-04-11 | 2007-10-17 | Solvay Solexis S.p.A. | Fluoropolymer dispersion purification |
| US7754795B2 (en) | 2006-05-25 | 2010-07-13 | 3M Innovative Properties Company | Coating composition |
| US8119750B2 (en) | 2006-07-13 | 2012-02-21 | 3M Innovative Properties Company | Explosion taming surfactants for the production of perfluoropolymers |
| US20100113691A1 (en) * | 2008-11-06 | 2010-05-06 | E. I. Du Pont De Nemours And Company | Fluoro olefin polymerization |
| US8329813B2 (en) | 2009-05-08 | 2012-12-11 | E I Du Pont De Nemours And Company | Thermal reduction of fluoroether carboxylic acids or salts from fluoropolymer dispersions |
| RU2012120435A (ru) | 2009-10-16 | 2013-11-27 | Асахи Гласс Компани, Лимитед | Способ получения водной политетрафторэтиленовой дисперсии для процесса коагуляции и водная политетрафторэтиленовая дисперсия для процесса коагуляции |
| US9644055B2 (en) | 2012-05-23 | 2017-05-09 | Daikin Industries, Ltd. | Method for producing aqueous fluorine-containing polymer dispersing element, and purified aqueous fluorine-containing polymer dispersing element |
| JP7311825B2 (ja) * | 2020-09-07 | 2023-07-20 | ダイキン工業株式会社 | 変性ポリテトラフルオロエチレン水性分散液 |
| LU601231A1 (en) * | 2023-08-28 | 2025-05-28 | George Alexander Ivey | Composition and Method for Remediation of PFAS Contaminants |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4609497A (en) * | 1985-03-14 | 1986-09-02 | E. I. Du Pont De Nemours And Company | Process for separating surfactants used in the manufacture of concentrated fluoropolymer dispersions |
| JPS61246142A (ja) * | 1985-03-14 | 1986-11-01 | イ−・アイ・デユポン・デ・ニモアス・アンド・カンパニ− | 弗素系表面活性剤の回収方法 |
| US4623487A (en) * | 1985-03-14 | 1986-11-18 | E. I. Du Pont De Nemours & Company | Process for recovery of fluorosurfactants |
| DE4340943A1 (de) * | 1993-12-01 | 1995-06-08 | Hoechst Ag | Wäßrige Dispersion von Fluorpolymerisaten, ihre Herstellung und Verwendung für Beschichtungen |
| DE19726802C1 (de) * | 1997-06-24 | 1998-06-10 | Dyneon Gmbh | Wäßrige Dispersion von Fluorpolymeren unterschiedlicher Teilchengröße |
| US6169139B1 (en) * | 1998-04-27 | 2001-01-02 | Dupont Dow Elastomers Llc | Fluoroelastomer latex |
| DE19857111A1 (de) * | 1998-12-11 | 2000-06-15 | Dyneon Gmbh | Wäßrige Dispersionen von Fluorpolymeren |
-
2000
- 2000-04-14 DE DE10018853A patent/DE10018853C2/de not_active Expired - Fee Related
-
2001
- 2001-04-10 DE DE60112420T patent/DE60112420T2/de not_active Expired - Lifetime
- 2001-04-10 CN CNB018079970A patent/CN1177883C/zh not_active Expired - Fee Related
- 2001-04-10 WO PCT/US2001/011628 patent/WO2001079332A1/en not_active Ceased
- 2001-04-10 RU RU2002127791/04A patent/RU2288923C2/ru not_active IP Right Cessation
- 2001-04-10 AU AU2001249959A patent/AU2001249959A1/en not_active Abandoned
- 2001-04-10 PL PL01357819A patent/PL357819A1/xx not_active Application Discontinuation
- 2001-04-10 CA CA002403957A patent/CA2403957A1/en not_active Abandoned
- 2001-04-10 EP EP01923247A patent/EP1274771B1/en not_active Expired - Lifetime
- 2001-04-10 JP JP2001576922A patent/JP2003531232A/ja not_active Ceased
- 2001-04-10 AT AT01923247T patent/ATE301151T1/de not_active IP Right Cessation
- 2001-04-13 TW TW090108921A patent/TW575613B/zh not_active IP Right Cessation
-
2002
- 2002-11-13 ZA ZA200209244A patent/ZA200209244B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CA2403957A1 (en) | 2001-10-25 |
| RU2288923C2 (ru) | 2006-12-10 |
| EP1274771A1 (en) | 2003-01-15 |
| EP1274771B1 (en) | 2005-08-03 |
| DE10018853A1 (de) | 2001-10-25 |
| AU2001249959A1 (en) | 2001-10-30 |
| PL357819A1 (en) | 2004-07-26 |
| CN1177883C (zh) | 2004-12-01 |
| DE60112420T2 (de) | 2006-06-01 |
| ZA200209244B (en) | 2003-07-18 |
| ATE301151T1 (de) | 2005-08-15 |
| WO2001079332A1 (en) | 2001-10-25 |
| DE60112420D1 (de) | 2005-09-08 |
| DE10018853C2 (de) | 2002-07-18 |
| CN1423671A (zh) | 2003-06-11 |
| JP2003531232A (ja) | 2003-10-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MM4A | Annulment or lapse of patent due to non-payment of fees |