CN102770469B - 制备具有改善的色彩稳定性的吸水性聚合物颗粒的方法 - Google Patents

制备具有改善的色彩稳定性的吸水性聚合物颗粒的方法 Download PDF

Info

Publication number
CN102770469B
CN102770469B CN201080052799.9A CN201080052799A CN102770469B CN 102770469 B CN102770469 B CN 102770469B CN 201080052799 A CN201080052799 A CN 201080052799A CN 102770469 B CN102770469 B CN 102770469B
Authority
CN
China
Prior art keywords
fatty
polymer particles
water
ammonia
acetal
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 - Fee Related
Application number
CN201080052799.9A
Other languages
English (en)
Chinese (zh)
Other versions
CN102770469A (zh
Inventor
N·赫佛特
T·丹尼尔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=43982460&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=CN102770469(B) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by BASF SE filed Critical BASF SE
Publication of CN102770469A publication Critical patent/CN102770469A/zh
Application granted granted Critical
Publication of CN102770469B publication Critical patent/CN102770469B/zh
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • 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
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/56—Wetness-indicators or colourants
    • 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
    • C08F2/00—Processes of polymerisation
    • C08F2/04—Polymerisation in solution
    • C08F2/10—Aqueous solvent
    • 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
    • C08F2/00—Processes of polymerisation
    • C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • 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
    • C08J3/12—Powdering or granulating
    • 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
    • C08J3/12—Powdering or granulating
    • C08J3/126—Polymer particles coated by polymer, e.g. core shell structures
    • 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
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C08J2300/10—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups
    • C08J2300/102—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing halogen atoms

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Materials Engineering (AREA)
  • Epidemiology (AREA)
  • Hematology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Veterinary Medicine (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Absorbent Articles And Supports Therefor (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
CN201080052799.9A 2009-11-23 2010-11-12 制备具有改善的色彩稳定性的吸水性聚合物颗粒的方法 Expired - Fee Related CN102770469B (zh)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US26341909P 2009-11-23 2009-11-23
US61/263,419 2009-11-23
PCT/EP2010/067382 WO2011061125A2 (de) 2009-11-23 2010-11-12 Verfahren zur herstellung wasserabsorbierender polymerpartikel mit verbesserter farbstabilität

Publications (2)

Publication Number Publication Date
CN102770469A CN102770469A (zh) 2012-11-07
CN102770469B true CN102770469B (zh) 2015-04-15

Family

ID=43982460

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201080052799.9A Expired - Fee Related CN102770469B (zh) 2009-11-23 2010-11-12 制备具有改善的色彩稳定性的吸水性聚合物颗粒的方法

Country Status (5)

Country Link
US (1) US8497337B2 (https=)
EP (1) EP2504368B1 (https=)
JP (1) JP2013511608A (https=)
CN (1) CN102770469B (https=)
WO (1) WO2011061125A2 (https=)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
HUE032284T2 (en) 2008-03-18 2017-09-28 Novo Nordisk As Protease-stabilized, acylated insulin analogues
US8703876B2 (en) * 2010-03-15 2014-04-22 Basf Se Process for producing water absorbing polymer particles with improved color stability
CN104619357B (zh) * 2012-08-29 2017-07-07 巴斯夫欧洲公司 用于制备吸水性聚合物颗粒的方法
ES2688532T3 (es) 2013-01-18 2018-11-05 Basf Se Composiciones de recubrimiento a base de dispersión acrílica
US11325990B2 (en) * 2016-08-10 2022-05-10 Basf Se Method for the production of superabsorbers
US11813589B2 (en) 2017-11-10 2023-11-14 Basf Se Superabsorbent complexed with aluminum ions

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5610208A (en) * 1994-02-17 1997-03-11 Nippon Shokubai Co., Ltd. Water-absorbent agent, method for production thereof, and water-absorbent composition
CN1939955A (zh) * 2005-09-30 2007-04-04 株式会社日本触媒 颗粒状吸水剂的制造方法以及颗粒状吸水剂
CN101198363A (zh) * 2005-04-22 2008-06-11 艾弗尼克施拖克豪森公司 用金属盐和金属氧化物处理并在其表面后交联的超吸收体

Family Cites Families (61)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2567575A (en) 1945-05-19 1951-09-11 Honeywell Regulator Co Resistance measuring apparatus
JPS6018690B2 (ja) 1981-12-30 1985-05-11 住友精化株式会社 吸水性樹脂の吸水性改良方法
JPS58180233A (ja) 1982-04-19 1983-10-21 Nippon Shokubai Kagaku Kogyo Co Ltd 吸収剤
US4734478A (en) 1984-07-02 1988-03-29 Nippon Shokubai Kagaku Kogyo Co., Ltd. Water absorbing agent
DE3713601A1 (de) 1987-04-23 1988-11-10 Stockhausen Chem Fab Gmbh Verfahren zur herstellung eines stark wasserabsorbierenden polymerisats
FI90554C (fi) 1987-07-28 1994-02-25 Dai Ichi Kogyo Seiyaku Co Ltd Menetelmä akryylipolymeerigeelin jatkuvaksi valmistamiseksi
WO1990015830A1 (en) 1989-06-12 1990-12-27 Weyerhaeuser Company Hydrocolloid polymer
CA2038779A1 (en) 1990-04-02 1991-10-03 Takumi Hatsuda Method for production of fluid stable aggregate
DE4020780C1 (https=) 1990-06-29 1991-08-29 Chemische Fabrik Stockhausen Gmbh, 4150 Krefeld, De
ES2097235T3 (es) 1991-09-03 1997-04-01 Hoechst Celanese Corp Polimero superabsorbente que tiene propiedades de absorcion mejoradas.
DE4138408A1 (de) 1991-11-22 1993-05-27 Cassella Ag Hydrophile, hochquellfaehige hydrogele
JP3045422B2 (ja) 1991-12-18 2000-05-29 株式会社日本触媒 吸水性樹脂の製造方法
DE69312126T2 (de) 1992-03-05 1997-11-06 Nippon Catalytic Chem Ind Verfahren zu Herstellung eines absorbierenden Harzes
GB9208449D0 (en) 1992-04-16 1992-06-03 Dow Deutschland Inc Crosslinked hydrophilic resins and method of preparation
DE69412547T2 (de) 1993-06-18 1999-04-22 Nippon Shokubai Co. Ltd., Osaka Verfahren zur Herstellung eines absorbierenden Harzes
EP0640330B1 (en) 1993-06-30 2000-05-24 The Procter & Gamble Company Hygienic absorbent articles
DE19543368C2 (de) 1995-11-21 1998-11-26 Stockhausen Chem Fab Gmbh Wasserabsorbierende Polymere mit verbesserten Eigenschaften, Verfahren zu deren Herstellung und deren Verwendung
DE19646484C2 (de) 1995-11-21 2000-10-19 Stockhausen Chem Fab Gmbh Flüssigkeitsabsorbierende Polymere, Verfahren zu deren Herstellung und deren Verwendung
DE19807502B4 (de) 1998-02-21 2004-04-08 Basf Ag Verfahren zur Nachvernetzung von Hydrogelen mit 2-Oxazolidinonen, daraus hergestellte Hydrogele und deren Verwendung
US6265488B1 (en) 1998-02-24 2001-07-24 Nippon Shokubai Co., Ltd. Production process for water-absorbing agent
US6503979B1 (en) 1998-02-26 2003-01-07 Basf Aktiengesellschaft Method for cross-linking hydrogels with bis- and poly-2-oxazolidinones
US6241928B1 (en) 1998-04-28 2001-06-05 Nippon Shokubai Co., Ltd. Method for production of shaped hydrogel of absorbent resin
DE19854574A1 (de) 1998-11-26 2000-05-31 Basf Ag Verfahren zur Nachvernetzung von Hydrogelen mit N-Acyl-2-Oxazolidinonen
DE19854573A1 (de) 1998-11-26 2000-05-31 Basf Ag Verfahren zur Nachvernetzung von Hydrogelen mit 2-Oxo-tetrahydro-1,3-oxazinen
DE60014054T2 (de) 1999-03-12 2005-02-03 Basf Ag Farbstabile superabsorbierende polymerzusammensetzung
JP2000327926A (ja) * 1999-05-25 2000-11-28 Sanyo Chem Ind Ltd 吸収剤組成物および吸収性物品
US6239230B1 (en) 1999-09-07 2001-05-29 Bask Aktiengesellschaft Surface-treated superabsorbent polymer particles
DE19955861A1 (de) 1999-11-20 2001-05-23 Basf Ag Verfahren zur kontinuierlichen Herstellung von vernetzten feinteiligen gelförmigen Polymerisaten
US6809158B2 (en) 2000-10-20 2004-10-26 Nippon Shokubai Co., Ltd. Water-absorbing agent and process for producing the same
US6979564B2 (en) 2000-10-20 2005-12-27 Millennium Pharmaceuticals, Inc. 80090, human fucosyltransferase nucleic acid molecules and uses thereof
BR0206396A (pt) 2001-01-12 2004-02-10 Degussa Processo contìnuo para preparação e purificação de ácido (met)acrìlico
DE10138150A1 (de) 2001-08-03 2003-02-13 Basf Ag Verfahren zur Herstellung wasserabsorbierender Harze
JP2005504865A (ja) 2001-10-05 2005-02-17 ビーエーエスエフ アクチェンゲゼルシャフト モルホリン−２，３−ジオンを用いたヒドロゲルの架橋法
AU2002349359A1 (en) * 2001-12-20 2003-07-09 Basf Aktiengesellschaft Absorbent article
JP3939988B2 (ja) * 2002-01-16 2007-07-04 住友精化株式会社 吸水性樹脂の製造方法
DE10204937A1 (de) 2002-02-07 2003-08-21 Stockhausen Chem Fab Gmbh Verfahren zur Nachvernetzung im Bereich der Oberfläche von wasserabsorbierenden Polymeren mit Harnstoffderivaten
DE10204938A1 (de) 2002-02-07 2003-08-21 Stockhausen Chem Fab Gmbh Verfahren zur Nachvernetzung im Bereich der Oberfläche von wasserabsorbierenden Polymeren mit beta-Hydroxyalkylamiden
DE10210124A1 (de) * 2002-03-08 2003-09-18 Basf Ag Polymergemische mit verbesserter Geruchskontrolle
DE10211686A1 (de) 2002-03-15 2003-10-02 Stockhausen Chem Fab Gmbh (Meth)Acrylsäurekristall und Verfahren zur Herstellung und Aufreinigung von wässriger (Meth)Acrylsäure
DE10225943A1 (de) 2002-06-11 2004-01-08 Basf Ag Verfahren zur Herstellung von Estern von Polyalkoholen
CA2487030A1 (en) 2002-06-11 2003-12-18 Basf Aktiengesellschaft (meth)acrylic esters of polyalkoxylated glycerine
CA2488226A1 (en) 2002-06-11 2003-12-18 Basf Aktiengesellschaft (meth)acrylic esters of polyalkoxylated trimethylolpropane
DE10247240A1 (de) 2002-10-10 2004-04-22 Basf Ag Verfahren zur Herstellung von Acrylsäure
CA2512000C (en) 2002-12-26 2011-08-09 Eisai Co., Ltd. Selective estrogen receptor modulator
TW200500046A (en) * 2003-03-26 2005-01-01 Basf Ag Color-stable superabsorbent polymer composition
DE10331450A1 (de) 2003-07-10 2005-01-27 Basf Ag (Meth)acrylsäureester monoalkoxilierter Polyole und deren Herstellung
DE10331456A1 (de) 2003-07-10 2005-02-24 Basf Ag (Meth)acrylsäureester alkoxilierter ungesättigter Polyolether und deren Herstellung
DE10334584A1 (de) 2003-07-28 2005-02-24 Basf Ag Verfahren zur Nachvernetzung von Hydrogelen mit bicyclischen Amidacetalen
DE10355401A1 (de) 2003-11-25 2005-06-30 Basf Ag (Meth)acrylsäureester ungesättigter Aminoalkohole und deren Herstellung
DE102004057874A1 (de) * 2004-11-30 2006-06-01 Basf Ag Verfahren zur Nachvernetzung wasserabsorbierender Polymerpartikel
US20090012488A1 (en) * 2006-03-10 2009-01-08 Basf Se Super-Absorber Having Improved Smell-Inhibition
JP5517622B2 (ja) 2006-10-05 2014-06-11 ビーエーエスエフ ソシエタス・ヨーロピア モノマー溶液の液滴の重合による吸収性ポリマー粒子の製造法
RU2467020C2 (ru) 2006-10-31 2012-11-20 Басф Се Регулирование в способе получения абсорбирующих воду полимерных частиц в нагретой газовой фазе
EP2112172B2 (en) * 2007-01-24 2018-10-17 Nippon Shokubai Co., Ltd. Particulate water-absorbent polymer and process for production thereof
EP2115019B2 (de) 2007-01-29 2019-07-10 Basf Se VERFAHREN ZUR HERSTELLUNG WEIßER UND FARBSTABILER WASSERABSORBIERENDER POLYMERPARTIKEL MIT HOHEM ABSORPTIONSVERMÖGEN UND HOHER FLÜSSIGKEITSLEITFÄHIGKEIT
CN101594889A (zh) * 2007-01-29 2009-12-02 巴斯夫欧洲公司 生产具有高吸收率和高盐水导流率的白色且颜色稳定的吸水性聚合物颗粒的方法
DE102007007203A1 (de) * 2007-02-09 2008-08-14 Evonik Stockhausen Gmbh Wasserabsorbierendes Polymergebilde mit hoher Ammoniak-Bindekapazität
DE102007053619A1 (de) * 2007-11-08 2009-05-20 Evonik Stockhausen Gmbh Wasserabsorbierende Polymergebilde mit verbesserter Farbstabilität
JP5377642B2 (ja) 2008-07-31 2013-12-25 ビーエーエスエフ ソシエタス・ヨーロピア 着色安定性超吸収剤
EP2313119B1 (de) 2008-08-12 2012-12-26 Basf Se Verfahren zur herstellung von superabsorbern mit niedrigem restmonomerengehalt
WO2011032876A1 (de) 2009-09-16 2011-03-24 Basf Se Farbstabiler superabsorber

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5610208A (en) * 1994-02-17 1997-03-11 Nippon Shokubai Co., Ltd. Water-absorbent agent, method for production thereof, and water-absorbent composition
CN101198363A (zh) * 2005-04-22 2008-06-11 艾弗尼克施拖克豪森公司 用金属盐和金属氧化物处理并在其表面后交联的超吸收体
CN1939955A (zh) * 2005-09-30 2007-04-04 株式会社日本触媒 颗粒状吸水剂的制造方法以及颗粒状吸水剂

Also Published As

Publication number Publication date
JP2013511608A (ja) 2013-04-04
US8497337B2 (en) 2013-07-30
US20110121230A1 (en) 2011-05-26
CN102770469A (zh) 2012-11-07
EP2504368A2 (de) 2012-10-03
EP2504368B1 (de) 2014-01-08
WO2011061125A2 (de) 2011-05-26
WO2011061125A3 (de) 2011-07-21

Similar Documents

Publication Publication Date Title
CN102361890B (zh) 制备表面后交联的吸水性聚合物颗粒的方法
CN103347548B (zh) 具有高溶胀速度的吸水性聚合物颗粒的制备方法
CN103068861B (zh) 具有改进的色彩稳定性的吸水聚合物颗粒
CN104936989A (zh) 制备具有高自由溶胀率和高离心保留容量且同时具有高溶胀凝胶床渗透性的吸水性聚合物颗粒的方法
CN103649130B (zh) 制备具有高溶胀速度的吸水性聚合物颗粒的方法
CN105237672A (zh) 一种通过单体溶液液滴的聚合而制备渗透性吸水聚合物颗粒的方法
CN104812418A (zh) 基于可再生原料制备超吸收剂的方法
US20110118114A1 (en) Color stable superabsorbent
CN102803316A (zh) 具有低结块倾向和在压力下的高吸收的吸水性聚合物颗粒的制备方法
CN107075030B (zh) 制备吸水性聚合物颗粒的方法
US20110257340A1 (en) Process for Producing Water-Absorbing Polymer Particles
CN102892795B (zh) 制备具有改善的颜色稳定性的吸水性聚合物颗粒的方法
CN102770469B (zh) 制备具有改善的色彩稳定性的吸水性聚合物颗粒的方法
CN104114591B (zh) 具有高溶胀率和高渗透率的吸水性聚合物颗粒
US8742024B2 (en) Mixture of surface postcrosslinked superabsorbers with different surface postcrosslinking
KR20210036368A (ko) 고흡수제의 제조 방법
CN106661166B (zh) 吸水性聚合物颗粒
CN104411732A (zh) 用于制备具有改进特性的吸水性聚合物颗粒的方法
US9833769B2 (en) Process for producing water-absorbing polymer particles with high free swell rate
CN103562240B (zh) 连续制备吸水性聚合物颗粒的方法
CN103561782B (zh) 制备吸水性聚合物颗粒的方法
CN102573932A (zh) 连续生产吸水聚合物颗粒的方法

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20150415

Termination date: 20181112

CF01 Termination of patent right due to non-payment of annual fee