KR960703952A - Cross-linked powder polymers that absorb aqueous and body fluids, methods for making and using the same (POWDER-FORM CROSS-LINKED POLYMERS CAPABLE OF ABSORBING AQUEOUS LIQUIDS AND BODY FLUIDS, METHOD OF PREPARING THEM AND THEIR USE) - Google Patents

Cross-linked powder polymers that absorb aqueous and body fluids, methods for making and using the same (POWDER-FORM CROSS-LINKED POLYMERS CAPABLE OF ABSORBING AQUEOUS LIQUIDS AND BODY FLUIDS, METHOD OF PREPARING THEM AND THEIR USE) Download PDF

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KR960703952A
KR960703952A KR1019960700083A KR19960700083A KR960703952A KR 960703952 A KR960703952 A KR 960703952A KR 1019960700083 A KR1019960700083 A KR 1019960700083A KR 19960700083 A KR19960700083 A KR 19960700083A KR 960703952 A KR960703952 A KR 960703952A
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KR100331343B1 (en
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쿠르트 다멘
에드가 헤르만
클라우스 플뤼거
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부르노 케레스·헬무트 클림멕
케미쉐 파브릭 스톡하우젠 게엠베하
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    • 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
    • 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
    • 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
    • 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
    • C08F220/52—Amides or imides
    • C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56—Acrylamide; Methacrylamide
    • 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
    • C08F291/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds according to more than one of the groups C08F251/00 - C08F289/00
    • 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
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/242—Applying crosslinking or accelerating agent onto compounding ingredients such as fillers, reinforcements
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide

Abstract

본 발명은 하중하에서 수성액, 구체적으로는 체액에 대하여 높은 흡수 성능을 갖는 수-팽윤성의 가교된 분말 중합체에 관한 것으로서, 상기 중합체는 a) 50몰% 이상이 중화된 산-원자단-함유 단량체 55~99.9중량%, b) 상기 a)와 공중합할 수 있는 단량체 0~40중량%, c) 1종 이상의 가교제 0.1~5.0중량%, 및 d) 수용성 중합체 0~30중량%로 구성된다.The present invention relates to a water-swellable crosslinked powder polymer having a high absorption capacity against an aqueous liquid, in particular a body fluid under load, the polymer comprising: a) an acid-atom-containing monomer 55 having at least 50 mol% neutralized; 99.9% by weight, b) 0-40% by weight of a monomer copolymerizable with a), c) 0.1-5.0% by weight of one or more crosslinking agents, and d) 0-30% by weight of a water-soluble polymer.

상기 a)의 염은 양이온으로서 Li+, Na+, 바람직하게는 K+, Cs+, Rb+및 일차, 이차, 및 삼차 메틸 암모늄이온을 단독 또는 조합체로 포함한다. 상기 중합체는 이산화 탄소를 주성분으로 하는 발포제를 단량체에 첨가하고, 중합시킨 다음, 상기 중합체를 건조시키고, 표면-가교제에 대하여 반응성이 있는 하나의 화합물 또는 수개의 화합물과 함께 100 내지 300℃로 가열시킴으로서 제조하였다. 이들 중합체는 체액을 흡수하는 위생 용품 및 붕대의 성분, 기저귀, 생리대 및 실금재 물품의 성분, 토질 개량제, 식물 육종용 인공 토양, 및 포장재의 성분으로서 적합하다.The salt of a) comprises Li + , Na + , preferably K + , Cs + , Rb + and primary, secondary, and tertiary methyl ammonium ions, alone or in combination, as cations. The polymer is prepared by adding a carbon dioxide-based blowing agent to the monomer, polymerizing, drying the polymer and heating it to 100 to 300 ° C. together with one compound or several compounds that are reactive towards the surface-crosslinking agent. Prepared. These polymers are suitable as components of hygiene articles and bandages that absorb body fluids, components of diapers, sanitary napkins and incontinence articles, soil improvers, artificial soil for plant breeding, and packaging materials.

Description

수성액 및 체액을 흡수하는 가교된 분말 중합체, 이의 제조 방법 및 사용 방법(POWER-FORM CROSS-LINKED POLYMERS CAPABLE OF ABSORBING AQUEOUS LIQUIDS AND BODY FLUIDS, METHOD OF PREPARING THEM AND THEIR USE)Cross-linked powder polymers that absorb aqueous and body fluids, methods for making and using the same (POWER-FORM CROSS-LINKED POLYMERS CAPABLE OF ABSORBING AQUEOUS LIQUIDS AND BODY FLUIDS, METHOD OF PREPARING THEM AND THEIR USE)

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음As this is a public information case, the full text was not included.

Claims (19)

a) 50몰% 이상이 중화된 염으로서 존재하는 중합된 불포화, 중압성의 산-원자단-함유 단량체 55~99.9중량%, b) 상기 a)와 공중합될 수 있는 중합된 불포화 단량체 0~40중량%, c) 1종 이상의 가교제 0.1~5.0중량%, 및 d) 수용성 중합체 0~30중량% (상기 a) 내지 d)의 총 합계가 100중량%가 됨)로 구성되고, 물, 수성액, 구체적으로는 체액을 흡수하는 수-팽윤성의 가교된 분말 중합체에 있어서, 60g/㎤의 하중하에서 중합체 1g당 0.9% NaCl 용액을 12g 이상, 바람직하게는 16g 이상을 흡수하는 흡수 성능을 가지는 중합체.a) 55 to 99.9 weight percent of polymerized unsaturated, heavy acid-atom-containing monomer, wherein at least 50 mole percent is present as a neutralized salt, b) 0 to 40 weight percent of polymerized unsaturated monomer copolymerizable with a) c) 0.1 to 5.0% by weight of at least one crosslinking agent, and d) 0 to 30% by weight of the water-soluble polymer (total sum of 100% by weight of a) to d) above, water, aqueous liquid, A water-swellable crosslinked powdered polymer that absorbs body fluids, wherein the polymer has an absorption capability of absorbing at least 12 g, preferably at least 16 g of 0.9% NaCl solution per gram of polymer under a load of 60 g / cm 3. 제 1항에 있어서, 중합체가 30초 이내에 중합체 1g당 0.9% NaCl 용액을 10g 이상, 바람직하게는 16g 이상을 흡수하는 흡수 선능을 가지는 중합체.A polymer according to claim 1 wherein the polymer has an absorption capacity to absorb at least 10 g, preferably at least 16 g, of 0.9% NaCl solution per gram of polymer within 30 seconds. 제 1항 또는 제 2항에 있어서, 입자 크기가 20 내지 3,000㎛, 바람직하게는 100 내지 1,000㎛인 중합체.3. The polymer according to claim 1, wherein the particle size is 20 to 3,000 μm, preferably 100 to 1,000 μm. a) 50몰% 이상이 중화된 염으로서 존재하는 중합된 불포화, 중합성의 산-원자단-함유 단량체 55~99.9중량%, b) 상기 a)와 공중합될 수 있는 종합된 불포화 단량체 0~40중량%, c) 1종 이상의 가교제 0.1~5.0중량%, 및 d) 수용성 중합체 0~30중량% (상기 a) 내지 d)의 총 합계가 100중량%가 됨)로 구성되고, 물, 수성액, 구체적으로는 체액을 흡수하는 수-팽윤성의 가교된 분말 중합체에 있어서, 상기 a)의 염은 양이온으로서 Li+, Na+, 바람직하게는 K+, Cs+, Rb+및 암모늄 이온과 일차, 이차, 및 삼차 메틸 암모늄이온을 단독 또는 조합체로 포함하고; 상기 중합체에 대하여 이산화탄소를 주성분으로 하여 발포제 0.1~5.0중량%를 중합반응전에 단량체에 첨가하고; 상기 중합체를 건조시키고, 2차(secondary) 표면-가교제에 대하여 반응성이 있는 하나의 화합물 또는 수개의 화합물, 또는 이들의 용액 또는 분산액을 첨가하고; 이것을 100 내지 300℃로 시키는 것을 특징으로 하는 중합체.a) 55-99.9% by weight of polymerized unsaturated, polymerizable acid-atom-containing monomer, wherein at least 50 mol% is present as a neutralized salt, b) 0-40% by weight of synthesized unsaturated monomers copolymerizable with a) c) 0.1 to 5.0% by weight of at least one crosslinking agent, and d) 0 to 30% by weight of the water-soluble polymer (total sum of 100% by weight of a) to d) above, water, aqueous liquid, In the water-swellable crosslinked powder polymer which absorbs body fluids, the salt of a) is used as a cation with Li + , Na + , preferably K + , Cs + , Rb + and ammonium ions, primary, secondary, And tertiary methyl ammonium ions alone or in combination; 0.1 to 5.0% by weight of a blowing agent is added to the monomer before the polymerization reaction with carbon dioxide as a main component of the polymer; Drying the polymer and adding one compound or several compounds, or solutions or dispersions thereof, that are reactive with a secondary surface-crosslinker; The polymer which makes this 100-300 degreeC. 제 1항 내지 제 4항 중 어느 한 항에 있어서, 산-원자단-함유 단량체 a) 아트릴산, 메타크릴산, 아크릴아미도메틸프로판 설폰산, 및 이들 단량체들의 혼합물로 이루어진 군에서 선택되고, 단량체 b)는 아크릴아미드, 메타크릴아미드, 히드록시알킬 아크릴레이트, 디메틸아미노-알킬(메타)-아크릴레이트, 디메틸아미노프로필(메타)아크릴아미드, 사차 아민 및 이들 단량체들의 암모늄염, 및 이들 단량체들의 혼합물로 이루어진 군에서 선택되고, 가교제 c)는 알킬렌 비스아크릴아미드, N-메틸올 아크릴아미드, 부탄디올 디아크릴레이트, 헥산디올 디메타크릴레이트, 폴리글리콜 디아크릴레이트, 트리메틸올프로판 트리아크릴레이트, 아릴 아크릴레이트, 디알릴 아크릴아미드, 트리알릴 아민, 디알릴 에테르, 폴리글리시딜 에테르, 예컨대 에틸렌 글리콜 디글리시딜 에테르 및 글리세롤 폴리글리시딜 에테르, 폴리올, 예컨대 글리세롤, 트리메틸올프로판, 폴리알킬렌 글리콜, 예컨대 폴리에틸렌 글리콜 200 내지 600, 및 폴리아민, 또는 이들 가교제들의 혼합물로 이루어진 군에서 선택되고, 이산화탄소를 주성분으로 하는 발포제는 Na2CO3, K2CO|3, (NH4)2CO3, MgCO3, CaCO3, NaHCO3, KHCO|3, 이들의 카르보네이트 혼합물, 또는 기체상 또는 고상 형태의 이산화 탄소로 이루어진 군에서 선택되는 것을 특징으로 하는 중합체.5. The monomer of claim 1, wherein the acid-atom-containing monomer a) is selected from the group consisting of atryl acid, methacrylic acid, acrylamidomethylpropane sulfonic acid, and mixtures of these monomers. b) is acrylamide, methacrylamide, hydroxyalkyl acrylate, dimethylamino-alkyl (meth) -acrylate, dimethylaminopropyl (meth) acrylamide, quaternary amines and ammonium salts of these monomers, and mixtures of these monomers And crosslinking agent c) is alkylene bisacrylamide, N-methylol acrylamide, butanediol diacrylate, hexanediol dimethacrylate, polyglycol diacrylate, trimethylolpropane triacrylate, aryl acryl Rate, diallyl acrylamide, triallyl amine, diallyl ether, polyglycidyl ether, such as ethylene glycol digle Cydyl ether and glycerol polyglycidyl ether, polyols such as glycerol, trimethylolpropane, polyalkylene glycols such as polyethylene glycol 200 to 600, and polyamines, or mixtures of these crosslinking agents, selected from the group consisting of carbon dioxide as a main component Blowing agent is Na 2 CO 3 , K 2 CO | 3 , (NH 4 ) 2 CO 3 , MgCO 3 , CaCO 3 , NaHCO 3 , KHCO | 3 , carbonate mixtures thereof, or polymers selected from the group consisting of carbon dioxide in gaseous or solid form. 수용성 중합체 d)의 존재하에서, 단량체 a), 상기 a)와 공중합할 수 있는 단량체 b), 및 가교제 c)를 중합시킴으로써 제 1항 내지 제 5항의 중합체를 제조하는 방법에 있어서, 상기 a)의 염이 리튬 이온, 나트륨 이온, 및 바람직하게는 칼륨 이온, 세슘 이온, 루비듐 이온, 암모늄 이온, 일차, 이차, 및 삼차 메틸 암모늄 이온, 또는 이들 이온들의 혼합물의 이온들로 이루어진 군에서 선택되고; 상기 중합체에 대하여 이산화탄소를 주성분으로 하는 발포제 0.1~5.0중량%를 중합반응을 수행하기 전에 단량체에 첨가하고; 수득한 단량체 혼합물의 중합반응은 하이드로겔의 형성하에서 광에 노출시키거나 또는 조사에 의해 개시되거나 또는 라디칼 형성 개시제를 첨가함으로서 수행하고; 상기 중합체를 건조시키고; 상기 중합체에 2차 근(近;near)-표면-가교제에 대하여 반응성이 있는 하나의 화합물 또는 수개의 화합물, 또는 이들의 용액 또는 분산액을 첨가하고; 이것을 100 내지 300℃로 시키는 것을 특징으로 하는 방법.A process for producing the polymer of claims 1 to 5 by polymerizing monomer a), a monomer b) copolymerizable with a) and a crosslinking agent c) in the presence of a water-soluble polymer d). The salt is selected from the group consisting of lithium ions, sodium ions, and preferably ions of potassium ions, cesium ions, rubidium ions, ammonium ions, primary, secondary, and tertiary methyl ammonium ions, or mixtures of these ions; 0.1 to 5.0% by weight of carbon dioxide-based blowing agent based on the polymer is added to the monomer before the polymerization reaction; The polymerization of the obtained monomer mixture is carried out by exposure to light under the formation of a hydrogel or by irradiation or by the addition of a radical forming initiator; Drying the polymer; To the polymer is added one compound or several compounds, or solutions or dispersions thereof, which are reactive toward secondary near-surface-crosslinking agents; The method characterized by making this 100-300 degreeC. 제 6항에 있어서, 중합체를 80 내지 200℃, 구체적으로는 100 내지 180℃, 바람직하게는 120 내지 150℃에서 건조시키는 방법.The process according to claim 6, wherein the polymer is dried at 80 to 200 ° C, specifically 100 to 180 ° C, preferably 120 to 150 ° C. 제 6항에 있어서, 중합체를 건조시킨 후, 분쇄시키는 방법.The method of claim 6, wherein the polymer is dried and then ground. 제 7항 또는 제 8항에 있어서, 중합체를 체질(screening)하여 입자 크기가 20 내지 3,000㎛, 바람직하게는 100 내지 1,000㎛로 만드는 방법.9. Process according to claim 7 or 8, wherein the polymer is screened to make the particle size from 20 to 3,000 mu m, preferably from 100 to 1,000 mu m. 제 6항에 있어서, 100 내지 300℃에서 가열시켜 근-표면-가교를 수행하는 방법.The method of claim 6, wherein near-surface-crosslinking is performed by heating at 100 to 300 ° C. 8. 제 6항에 있어서, 중합반응을 수성액에서 수행하는 방법.The process according to claim 6, wherein the polymerization is carried out in an aqueous liquid. 제 6항에 있어서, 중합반응을 물/오일(w/o)-분산액에서 수행하는 방법.The process of claim 6 wherein the polymerization is carried out in a water / oil (w / o) -dispersion. 제 1항 내지 제 5항의 중합체를 체액을 흡수하는 위생 용품 및 붕대에 혼입하는 성분으로서 사용하는 방법.A method of using the polymer of claim 1 as a component to be incorporated into a hygiene article and bandage that absorbs body fluids. 제 1항 내지 제 5항의 중합체를 기저귀, 생리대, 및 실금재 물품에 혼입하는 성분으로서 사용하는 방법.A method of using the polymer of claims 1 to 5 as a component to be incorporated into diapers, sanitary napkins, and incontinence articles. 중합체와 솜털(fluff)의 중량을 기준으로 제 1항 내지 제 5항의 중합체를 15~100중량%, 바람직하게는 35~100중량%, 가장 바람직하게는 30~70중량%로 기저귀에 사용하는 방법.15 to 100% by weight, preferably 35 to 100% by weight and most preferably 30 to 70% by weight of the polymer of claims 1 to 5, based on the weight of the polymer and fluff. . 제 1항 내지 제 5항의 중합체를 전류-전도 케이블 및 광-전송 케이블의 성분으로서 사용하는 방법.A method of using the polymer of claim 1 as a component of a current-conducting cable and an optical-transmission cable. 제 1항 내지 제 5항의 중합체를 토질 개량제로서 사용하는 방법.A method of using the polymer of claim 1 as a soil improver. 제 1항 내지 제 5항의 중합체를 식물 육종용 인공 토양으로서 사용하는 방법.A method of using the polymer of claims 1 to 5 as artificial soil for plant breeding. 제 1항 내지 제 5항의 중합체를 포장재의 성분으로서 사용하는 방법.A method of using the polymer of claim 1 as a component of a packaging material. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
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