JP6805144B2 - 吸水性ポリマー粒子を懸濁重合によって製造する方法 - Google Patents
吸水性ポリマー粒子を懸濁重合によって製造する方法 Download PDFInfo
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- JP6805144B2 JP6805144B2 JP2017529731A JP2017529731A JP6805144B2 JP 6805144 B2 JP6805144 B2 JP 6805144B2 JP 2017529731 A JP2017529731 A JP 2017529731A JP 2017529731 A JP2017529731 A JP 2017529731A JP 6805144 B2 JP6805144 B2 JP 6805144B2
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- 239000004633 polyglycolic acid Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229940035023 sucrose monostearate Drugs 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- AOBORMOPSGHCAX-DGHZZKTQSA-N tocofersolan Chemical compound OCCOC(=O)CCC(=O)OC1=C(C)C(C)=C2O[C@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C AOBORMOPSGHCAX-DGHZZKTQSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
-
- 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
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
-
- 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
- C08F20/00—Homopolymers and 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
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/04—Acids, Metal salts or ammonium salts thereof
- C08F20/06—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
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F2013/530131—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium being made in fibre but being not pulp
- A61F2013/530226—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium being made in fibre but being not pulp with polymeric fibres
-
- 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
- C08J2333/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
-
- 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
- C08J3/245—Differential crosslinking of one polymer with one crosslinking type, e.g. surface crosslinking
Description
a)少なくとも部分的に中和されていてよい、少なくとも1種のエチレン性不飽和の酸基含有モノマー、
b)任意で1種又は複数の架橋剤、
c)少なくとも1種の開始剤、
d)任意で1種又は複数の、a)に挙げたモノマーと共重合可能なエチレン性不飽和モノマー、及び
e)任意で1種又は複数の水溶性ポリマー
を含有するモノマー溶液の重合によって吸水性ポリマー粒子を製造する方法であって、ここでモノマー溶液を、重合の間に疎水性有機溶媒中で懸濁し、重合の間又はその後に疎水性有機溶媒中で凝集させ、得られた凝集ポリマー粒子を、有機表面後架橋剤を用いて熱により表面後架橋する方法において、凝集ポリマー粒子が、表面後架橋の前に少なくとも37g/gの遠心分離保持容量を有するように、架橋剤b)の量が選択され、熱による表面後架橋が100〜190℃で実施されることを特徴とする方法により解決される。
(A)上部液体透過層、
(B)下部液体不透過層、
(C)繊維材料を0〜30質量%及び本発明による方法によって得られる吸水性ポリマー粒子を70〜100質量%含有する、層(A)と層(B)との間にある液体吸収性貯蔵層、
(D)任意で、繊維材料を80〜100質量%及び本発明による方法によって得られる吸水性ポリマー粒子を0〜20質量%含有する、層(A)と層(C)との間にある捕捉層及び分配層、
(E)任意で、層(C)の真上及び/又は真下の織布層、及び
(F)さらなる任意の構成要素
を含む衛生用品である。
特に記載のない限り、23±2℃の周囲温度、50±10%の相対湿度で測定するものとする。吸水性ポリマー粒子は、測定前に十分に混合する。
吸水性ポリマー粒子の残留モノマーの含有量は、EDANAにより推奨される試験法WSP No.210.2−05「Residual Monomers」に従って特定する。
吸水性ポリマー粒子の含水量は、EDANAにより推奨される試験法No.WSP230.3(11)「Mass Loss Upon Heating」に従って特定する。
遠心分離保持容量(CRC)は、EDANAにより推奨される試験法No.WSP241.3(11)「Fluid Retention Capacity in Saline,After Centrifugation」に従って特定する。
0.0 g/cm2の圧力下での吸収量(AUNL)は、EDANAにより推奨される試験法No.WSP242.3(11)「Gravimetric Determination of Absorption Under Pressure」と同様に特定し、ここで21.0g/cm2の圧力(AUL0.3psi)の代わりに、0.0g/cm2の圧力(AUL0.0psi)に調整する。
吸水性ポリマー粒子における、21.0g/cm2の圧力での吸収量(AUL)は、EDANAにより推奨される試験法No.WSP242.3(11)「Gravimetric Determination of Absorption Under Pressure」に従って特定する。
49.2g/cm2の圧力下での吸収量(AUHL)は、EDANAにより推奨される試験法No.WSP242.3(11)「Gravimetric Determination of Absorption Under Pressure」に従って特定し、ここで21.0g/cm2の圧力(AUL0.3psi)の代わりに、49.2g/cm2の圧力(AUL0.7psi)に調整する。
かさ密度は、EDANAにより推奨される試験法No.WSP250.3(11)「Gravimetric Determination of Density」に従って特定する。
吸水性ポリマー粒子の抽出可能な構成要素の含分は、EDANAにより推奨される試験法No.WSP270.3(11)「Extractable」に従って特定する。抽出時間は16時間である。
膨潤速度(FSR)を特定するために、1.00g(=W1)の吸水性ポリマー粒子を25mLビーカーに秤量して入れ、ビーカーの底部に均一に分配する。そして、0.9質量%の食塩水20mlをディスペンサにより第2のビーカー中に計量供給し、このビーカーの内容物を第1のビーカーに迅速に追加し、ストップウォッチで計時を開始する。食塩水の最後の液滴が吸収されたら(このことは、液体表面における反射が消滅することで認識される)、ストップウォッチを止める。第2のビーカーから流し込まれ、第1のビーカー中のポリマーによって吸収された正確な液体量を、第2のビーカーを再計量することによって正確に特定した(=W2)。ストップウォッチで測定された、吸収に必要とされる時間間隔をtとして表す。表面上における最後の液滴の消滅を、時点tとして特定する。
30mm×6mmのサイズのマグネチックスターラー撹拌子を含む100mLビーカー中に、0.9質量%の食塩水50.0ml±1.0mlを入れる。マグネチックスターラーによって、食塩水を600rpmで攪拌する。そして、できるだけ迅速に、吸水性ポリマー粒子2.000g±0.010gを添加し、撹拌ダマ(Ruehrtraube)が吸水性ポリマー粒子による食塩水の吸収によって消失するまでに経過した時間を測定する。ここで、ビーカーの内容物全体は均一なゲルの塊としてまだ回転してよいが、ゲル化した食塩水の表面はもはや個別の乱流を示してはならない。必要とされた時間をボルテックスとして報告する。
ベースポリマーの製造:
実施例1
プロペラ式攪拌機及び還流冷却器を備える2Lのフランジ容器に、ヘプタン340.00g及びステアリン酸スクロース(Ryoto(登録商標)Sugar Ester S−370、Mitsubishi Chemical Europe GmbH、Duesseldorf、ドイツ)0.92gを予め装入し、70℃で加熱し、ステアリン酸スクロースを完全に溶解させた。
表1に示される量で、ベースポリマーの製造を実施例1と同様に行った。
表1に示される量で、ベースポリマーの製造を実施例1と同様に行ったが、ここで第一のモノマー溶液(第一の計量供給分)はさらに、2−プロパノール(イソプロパノール)を3.0g含有していた。
プロペラ式攪拌機及び還流冷却器を備える2Lのフランジ容器に、シクロヘキサン896.00g、Span(登録商標)20(モノラウリン酸ソルビタン)2.00g、Tixogel(登録商標)VZ(有機親和性ベントナイト)3.20g、及び0.015%のアスコルビン酸水溶液20.0gを予め装入し、攪拌及び窒素導入下で75℃の内部温度に加熱した。
プロペラ式攪拌機及び還流冷却器を備える2Lのフランジ容器に、シクロヘキサン896.00g、Span(登録商標)20(モノラウリン酸ソルビタン)2.00g、Tixogel(登録商標)VZ(有機親和性ベントナイト)3.20g、及び0.015%のアスコルビン酸水溶液20.0gを予め装入し、攪拌及び窒素導入下で75℃の内部温度に加熱した。
実施例1−1及び1−2
実施例1からのベースポリマー20gを、Waring(登録商標)−Blender32BL80(8011)タイプのミキサーに充填した。引き続き、ミキサーのスイッチを入れて段階1にした。その直後に、エチレンカーボネート0.5g及び水1.0gから成る1.5gの水溶液を表3に従い、注入器内に充填し、2秒以内にミキサーに計量供給した。3秒後、ミキサーのスイッチを切り、得られたポリマー粒子を、20cmの直径のガラスシャーレにおいて均一に分配した。熱により表面後架橋するために、ポリマー粒子で満たされたガラスシャーレを、空気循環式乾燥キャビネット内で、160℃で60分又は120分熱処理した。ポリマー粒子を冷たいガラスシャーレに移した。最後に、比較的粗い粒子を、850μmのメッシュ幅を有する篩で除去した。
熱による表面後架橋を実施例1−1及び1−2と同様に行ったが、但し、実施例2からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は、60分又は120分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1及び1−2と同様に行ったが、但し、実施例3からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は、60分又は120分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1と同様に行ったが、但し、実施例3からのベースポリマーを使用し、N,N,N’,N’−テトラキス(2−ヒドロキシエチル)エチレンジアミン(Primid(登録商標)XL552)を表面後架橋剤として使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は60分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1と同様に行ったが、但し、実施例3からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は、90℃又は200℃であった。熱処理時間は60分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1及び1−2と同様に行ったが、但し、実施例4からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は、60分又は120分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1及び1−2と同様に行ったが、但し、実施例5からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は、60分又は120分であった。これらの条件は、表3にまとめてある。
熱による表面後架橋を実施例1−1及び1−2と同様に行ったが、但し、実施例6からのベースポリマーを使用した。循環式乾燥キャビネット内の温度は160℃であった。熱処理時間は、60分又は120分であった。これらの条件は、表3にまとめてある。
米国特許第8003210号明細書(US8003210)からの実施例1を後追いした。
Claims (21)
- a)少なくとも部分的に中和されていてよい、少なくとも1種のエチレン性不飽和の酸基含有モノマー、
b)任意で1種又は複数の架橋剤、
c)少なくとも1種の開始剤、
d)任意で1種又は複数の、a)に挙げたモノマーと共重合可能なエチレン性不飽和モノマー、及び
e)任意で1種又は複数の水溶性ポリマー
を含有するモノマー溶液の重合によって吸水性ポリマー粒子を製造する方法であって、
ここでモノマー溶液を、重合の間に疎水性有機溶媒中で懸濁し、重合の間又はその後に疎水性有機溶媒中で凝集させ、得られた凝集ポリマー粒子を、有機表面後架橋剤を用いて熱により表面後架橋する方法において、凝集ポリマー粒子が、表面後架橋の前に少なくとも37g/gの遠心分離保持容量を有するように、架橋剤b)の量が選択され、熱による表面後架橋が、100〜190℃で実施されることを特徴とする前記方法。 - 請求項1に記載の方法において、疎水性有機溶媒中での重合後に凝集されることを特徴とする前記方法。
- 請求項1又は2に記載の方法において、重合が連鎖移動剤の存在下で実施されることを特徴とする前記方法。
- 請求項1から3までのいずれか一項に記載の方法において、ポリマー粒子が、表面後架橋の前に少なくとも40g/gの遠心分離保持容量を有するように、架橋剤b)の量が選択されることを特徴とする前記方法。
- 請求項1から4までのいずれか一項に記載の方法において、熱による表面後架橋が、120〜170℃で実施されることを特徴とする前記方法。
- 請求項1から5までのいずれか一項に記載の方法において、有機表面後架橋剤が、アルキレンカーボネート、2−オキサゾリジノン、ビス−2−オキサゾリジノン、ポリ−2−オキサゾリジノン、2−オキソテトラヒドロ−1,3−オキサジン、N−アシル−2−オキサゾリジノン、環状尿素、二環式アミドアセタール、オキセタン、及びモルホリン−2,3−ジオンから選択されていることを特徴とする前記方法。
- 請求項1から6までのいずれか一項に記載の方法において、得られたポリマー粒子を基準として1〜5質量%の有機表面後架橋剤が使用されることを特徴とする前記方法。
- 請求項1から7までのいずれか一項に記載の方法において、重合時に、少なくとも1種の分散助剤が使用されることを特徴とする前記方法。
- 請求項1から8までのいずれか一項に記載の方法において、得られたポリマー粒子が、重合後に、少なくとも部分的に共沸により脱水されることを特徴とする前記方法。
- 請求項9に記載の方法において、得られたポリマー粒子が、共沸脱水後に、濾過され、乾燥されることを特徴とする前記方法。
- 請求項1から10までのいずれか一項に記載の方法において、熱による表面後架橋が、可動式の混合器具を有するミキサー内で実施されることを特徴とする前記方法。
- 請求項1から11までのいずれか一項に記載の方法により得られる吸水性ポリマー粒子であって、遠心分離保持容量が少なくとも37g/gであり、21.0g/cm2の圧力下での吸収量が少なくとも30g/gであり、49.2g/cm2の圧力下での吸収量が少なくとも14g/gであり、遠心分離保持容量と21.0g/cm2の圧力下での吸収量との合計が少なくとも69g/gであり、遠心分離保持容量と49.2g/cm2の圧力下での吸収量との合計が少なくとも54g/gであり、及び抽出可能成分が20質量%未満である前記吸水性ポリマー粒子。
- 請求項12に記載の吸水性ポリマー粒子であって、遠心分離保持容量が少なくとも41g/gである前記吸水性ポリマー粒子。
- 請求項12又は13に記載の吸水性ポリマー粒子であって、21.0g/cm2の圧力下での吸収量が少なくとも34g/gである前記吸水性ポリマー粒子。
- 請求項12から14までのいずれか一項に記載の吸水性ポリマー粒子であって、49.2g/cm2の圧力下での吸収量が少なくとも20g/gである前記吸水性ポリマー粒子。
- 請求項12から15までのいずれか一項に記載の吸水性ポリマー粒子であって、遠心分離保持容量と21.0g/cm2の圧力下での吸収量との合計が少なくとも74g/gである前記吸水性ポリマー粒子。
- 請求項12から16までのいずれか一項に記載の吸水性ポリマー粒子であって、遠心分離保持容量と49.2g/cm2の圧力下での吸収量との合計が少なくとも59g/gである前記吸水性ポリマー粒子。
- 請求項12から17までのいずれか一項に記載の吸水性ポリマー粒子であって、14質量%未満の抽出可能成分を有する前記吸水性ポリマー粒子。
- 請求項12から18までのいずれか一項に記載の吸水性ポリマー粒子であって、1.0g/cm3未満のかさ密度を有する前記吸水性ポリマー粒子。
- 請求項12から19までのいずれか一項に記載の吸水性ポリマー粒子であって、300〜600μmの粒径を有する粒子の割合が少なくとも30質量%である前記吸水性ポリマー粒子。
- (A)上部液体透過層、
(B)下部液体不透過層、
(C)繊維材料を0〜30質量%及び請求項12から20までのいずれか一項に記載の吸水性ポリマー粒子を70〜100質量%含有する、層(A)と層(B)との間にある液体吸収性貯蔵層、
(D)任意で、繊維材料を80〜100質量%及び請求項12から20までのいずれか一項に記載の吸水性ポリマー粒子を0〜20質量%含有する、層(A)と層(C)との間にある捕捉層及び分配層、
(E)任意で、層(C)の真上及び/又は真下の織布層、及び
(F)さらなる任意の構成要素
を含む衛生用品。
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