JP2016525582A - アルカリ膨潤性エマルションポリマー - Google Patents
アルカリ膨潤性エマルションポリマー Download PDFInfo
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- JP2016525582A JP2016525582A JP2016506648A JP2016506648A JP2016525582A JP 2016525582 A JP2016525582 A JP 2016525582A JP 2016506648 A JP2016506648 A JP 2016506648A JP 2016506648 A JP2016506648 A JP 2016506648A JP 2016525582 A JP2016525582 A JP 2016525582A
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- monomer
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- alkyl
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- 239000004908 Emulsion polymer Substances 0.000 title claims abstract description 8
- 239000003513 alkali Substances 0.000 title description 5
- 239000000178 monomer Substances 0.000 claims abstract description 94
- 229920000642 polymer Polymers 0.000 claims abstract description 51
- 239000002245 particle Substances 0.000 claims abstract description 38
- 239000004971 Cross linker Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 72
- 125000000217 alkyl group Chemical group 0.000 claims description 34
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 19
- 238000009472 formulation Methods 0.000 description 16
- -1 C 6 carboxylic acid Chemical class 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 9
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 7
- 238000007792 addition Methods 0.000 description 7
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- 229940073507 cocamidopropyl betaine Drugs 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 229940057950 sodium laureth sulfate Drugs 0.000 description 7
- SXHLENDCVBIJFO-UHFFFAOYSA-M sodium;2-[2-(2-dodecoxyethoxy)ethoxy]ethyl sulfate Chemical compound [Na+].CCCCCCCCCCCCOCCOCCOCCOS([O-])(=O)=O SXHLENDCVBIJFO-UHFFFAOYSA-M 0.000 description 7
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
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- JQRRFDWXQOQICD-UHFFFAOYSA-N biphenylen-1-ylboronic acid Chemical compound C12=CC=CC=C2C2=C1C=CC=C2B(O)O JQRRFDWXQOQICD-UHFFFAOYSA-N 0.000 description 5
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- 239000011976 maleic acid Chemical group 0.000 description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Chemical group OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Chemical group CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 3
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- 238000004851 dishwashing Methods 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
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- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
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- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 239000000118 hair dye Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229940119170 jojoba wax Drugs 0.000 description 1
- 239000011021 lapis lazuli Substances 0.000 description 1
- 229940094522 laponite Drugs 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000011929 mousse Nutrition 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- OFESGEKAXKKFQT-UHFFFAOYSA-N n-ethenyl-n-methylformamide Chemical compound C=CN(C)C=O OFESGEKAXKKFQT-UHFFFAOYSA-N 0.000 description 1
- NCFAAXNAPQCDBL-UHFFFAOYSA-N n-ethenylacetamide;prop-2-enoic acid Chemical compound OC(=O)C=C.CC(=O)NC=C NCFAAXNAPQCDBL-UHFFFAOYSA-N 0.000 description 1
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical compound C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 229940086560 pentaerythrityl tetrastearate Drugs 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical class OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940043810 zinc pyrithione Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8152—Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
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- A—HUMAN NECESSITIES
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- A61Q5/06—Preparations for styling the hair, e.g. by temporary shaping or colouring
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- A61Q5/00—Preparations for care of the hair
- A61Q5/10—Preparations for permanently dyeing the hair
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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
- C08F2/00—Processes of polymerisation
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
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Abstract
Description
o BA=ブチルアクリレート
o MAA=メタクリル酸
o EHA=2−エチルヘキシルアクリレート
o EA=エチルアクリレート
o Lipo1は、18〜26オキシエチレン残基からを通じてメタクリロイル基に結合する直鎖状飽和C16〜18アルキル基を有する親油性に変成されたモノマーである。
o Lipo2は、20〜28オキシエチレン残基を通じてメタクリロイル基に結合する直鎖状飽和C10〜14アルキル基を有する親油性に変成されたモノマーである。
o TMPDE:トリメチロールプロパンジアリルエーテル
o SR399:ジペンタエリスリトールペンタアクリレート
o TMPTMA=トリメチロールプロパントリメタクリレート
o TMPDAE=(トリメチロールプロパンジアリルエーテル)
o SLES=ラウレス硫酸ナトリウム
o CAPB=コカミドプロピルベタイン
機械攪拌機、熱電対、冷却器、及び窒素スパージを装備した3リットルの4首丸底フラスコに、350gmの脱イオン水及び2gmのナトリウムラウリル硫酸を添加した。反応器を窒素でパージして、90℃に温めた。別個に、1)モノマーエマルション(A)を、935gmの脱イオン水、25gmのナトリウムラウリル硫酸、419gmのEA、242gmのMAAから調製した。2)モノマーエマルション添加剤(B)を、5.3gmのTMPTA及び38gのEAを混合することによって調製した。3)開始溶液C1を、19gmの脱イオン水中に0.4gmの過硫酸アンモニウムを溶解することによって調製した。4)開始溶液C2を、42gmの脱イオン水中に0.7gmの過硫酸アンモニウムを溶解することによって調製した。約90℃の反応器温度で、反応器を開始溶液C1で充填した。モノマーエマルション添加剤(B)をモノマーエマルション(A)に充填すると同時に、モノマーエマルション(A)を反応器中に充填した。いずれの供給も120分後に終了するように速度を制御した。別個に、開始溶液C2を、120分で反応器中に供給した。これらの添加が完了した後、モノマーエマルション及び開始剤供給ラインを脱イオン水ですすぎ、その後、モノマーをフリーラジカル触媒及び活性化剤で追跡した。得られたラテックスを濾過して、固体%、pH、残基モノマー、粒径、ゲル含有量、及び粘度に関して分析した。
機械攪拌機、熱電対、冷却器、及び窒素スパージを装備した3リットルの4首丸底フラスコに、350gmの脱イオン水及び2gmのナトリウムラウリル硫酸を添加した。反応器を窒素でパージして、90℃に温めた。別個に、1)モノマーエマルション(A)を、935gmの脱イオン水、25gmのナトリウムラウリル硫酸、457gmのEA、242gmのMAA、及び5.3gmのTMPTAから調製した。3)開始溶液C1を、19gmの脱イオン水中に0.4gmの過硫酸アンモニウムを溶解することによって調製した。4)開始溶液C2を、42gmの脱イオン水中に0.7gmの過硫酸アンモニウムを溶解することによって調製した。約℃90℃の反応器温度で、反応器を開始溶液C1で充填した。次いで、モノマーエマルション(A)を反応器中に充填した。供給が120分後に終了するように速度を制御した。別個に、開始溶液C2を、120分で反応器中に供給した。これらの添加が完了した後、モノマーエマルション及び開始剤供給ラインを脱イオン水ですすぎ、その後、モノマーをフリーラジカル触媒及び活性化剤で追跡した。得られたラテックスを濾過して、固体%、pH、残基モノマー、粒径、ゲル含有量、及び粘度に関して分析した。
ポリマー試料2〜7を、表1に記載の通りの組成物変更を除いて、実施例1に記載される通りの手順に従って調製した。
比較実施例2〜5を、表1に記載の通りの組成物変更を除いて、実施例1に記載される通りの手順に従って調製した。
表2にまとめられる通りの中和水溶液特性(粘度及び濁度)を測定するための手順
1%のポリマー活性のための可溶化粘度手順:
1.十分なポリマー試料を秤量し分けて最終の配合物中に1.0%のポリマーを有する。
2.DI水で予め希釈して500gの溶液を作製する。
3.水に4.2gの20%の重量/重量の水酸化ナトリウム溶液を添加して、オーバーヘッド攪拌機で均質になるまで効率的に撹拌する。
4.測定したpHは、7.2〜7.5の範囲に属するべきである。必要な場合20%のNaOHを使って調整する。
5.対応するスピンドルで構成されるBrookfield粘度計を用いて30rpmで粘度を測定して、少なくとも10%のスケールで測定値を得る。
6.試料を、濁度測定のために1ozのバイアル中に移動させる。
1.十分なポリマー試料を秤量し分けて最終の配合物中に2.5%のポリマーを有する。
2.DI水で予め希釈して500gの溶液を作製する。
3.水に3.5gの20%の重量/重量の水酸化ナトリウム溶液を添加して、オーバーヘッド攪拌機で完全に均質になるまで効率的に撹拌する。
4.測定したpHは、6.4〜6.8の範囲に属するべきである。必要な場合20%のNaOHを使って調整する。
5.対応するスピンドルで構成されるBrookfield粘度計を用いて30rpmで粘度を測定して、少なくとも10%のスケールで測定値を得る。
6.試料を、濁度測定のために1ozのバイアル中に移動させる。
1.試料入りの1ozのバイアルを、30分間3500rpmの遠心機で回転させる。
2.濁度メータで濁度を測定する。
A.パーソナルケア配合物の調製のための手順:
1.十分なポリマー実施例試料を秤量し分けて最終の配合物中に1.8〜2.2%のポリマーを有する。脱イオン水で予め希釈する。
2.エチレンジアミン4酢酸の4ナトリウム塩を添加して(VERSENE100XL、The Dow Chemical Companyから入手可能)最終の配合物中に0.1%の活性成分を有する。
3.ラウレス硫酸ナトリウムを添加して(EMPICOL ESB−70、Hunstmanから入手可能)最終の配合物中に12.5%の活性成分を有する。
4.コカミドプロピルベタイン(EMPIGEN BS/FA、Hunstmanから入手可能)を添加して、最終の配合物中に2.5%の活性成分を有する。
5.配合物のpHを30%のNaOH溶液を使ってpH7より上に調整する。
6.クエン酸を使った仕様にpHを調整し戻す。
7.メチルイソチアゾリンオン(及び)フェノキシエタノール(NEOLONE PE、The Dow Chemical Companyから入手可能)を添加する。
8.脱イオン水を総体積に添加する。
B.配合物可変パラメータ:
− ラウレス硫酸ナトリウム(SLES)とコカミドプロピルベタイン(CAPB)との比率及びレベルは、以下の通りの範囲に及ぶ:
レオロジー分析を、2つの異なる方法によって行った:
1.20℃に設定した40mmの4°アクリルコーンで構成されるTA器具AR1000レオメータを、用いる。低から高剪断応力方法に流動する標準定常状態を使用して、0.006Pa〜1000Paの剪断応力勾配を分析した。レオロジープロファイルを、最低でも24時間エイジングした試料において実行し、室温または40℃で貯蔵する。Ellisモデルを使用して、ゼロ応力粘度(ZSV)を提供した。
2.23℃に設定したスピンドル4で構成されるLV Brookfieldレオメータを、用いる。粘度を、12または60rpmのcPsで報告し、粘度は、2〜7日間エイジングして室温で貯蔵した試料の粘度に対応する。
透明性を、2つの異なる技術を用いて評価した:
1.HACH18900−00濁度計及び1cmの円筒形ガラス試料セルを用いる。透明性を、NTU値で報告する。
2.HACH DR2000分光光度計及び2.2cmの四角のガラスセルを用いる。透明性を、320nmまたは400nmのAbs値で報告する。
懸濁液を、異なる方法で評価した:
1.試験温度で最低でも4週間にわたってビーズ及び/または空気泡懸濁液及び安定性を検査して「合格」試験結果として報告した。ホホバエステルビーズ(FlorabeadsからのLapis28/60)を使用した。空気泡を、試料中に手動で導入した(気泡サイズはランダムに分散させることが予期される)。
2.上のゼロ応力値(Ellisモデル)
pH調整及び値を、室温でSCHOTT CG−837pHメータを用いて実施した。
懸濁ビーズまたは空気泡を有する未希釈のポリマーまたは配合物試料の熱エイジング試験を、40+/−2℃の制御された温度で、PROLABO EBオーブン、モデルRA6015を用いて実施した。
Claims (10)
- 25〜45重量%の少なくとも1つのC3〜C6カルボン酸モノマーの重合残基及び0.1〜3重量%の少なくとも1つの架橋剤の重合残基を含むエマルションポリマー粒子であって、架橋剤の割合が、粒子中心から粒子表面に連続的に増加する、前記ポリマー粒子。
- 54〜74重量%の少なくとも1つのC1〜C12アルキル(メタ)アクリレートの重合残基を更に含む、請求項1に記載の前記ポリマー粒子。
- 29〜41重量%の少なくとも1つのC3〜C6カルボン酸モノマーの重合残基、0.4〜1.5重量%の少なくとも1つの架橋剤の重合残基、及び58〜70重量%の少なくとも1つのC1〜C12アルキル(メタ)アクリレートの重合残基を含む、請求項2に記載の前記ポリマー粒子。
- 前記ポリマー粒子の平均粒径が、100〜1000nmの範囲である、請求項3に記載の前記ポリマー粒子。
- 前記架橋剤中のエチレン性不飽和基の数で割った前記架橋剤の分子量が、150以下である、請求項4に記載の前記ポリマー粒子。
- (a)25〜45重量%の少なくとも1つのC3〜C6カルボン酸モノマーを含む第1のモノマー混合物を提供するステップと、(b)0.1〜3重量%の少なくとも1つの架橋剤を含む第2のモノマー混合物を提供するステップと、(c)前記第2のモノマー混合物を前記第1のモノマー混合物に添加すると同時に、前記第1のモノマー混合物を重合反応容器に添加するステップと、による、エマルションポリマー粒子を生成するための方法であって、重量割合が、前記第1及び第2のモノマー混合物の総重量に基づく、前記方法。
- 前記第1のモノマー混合物が、54〜74重量%の少なくとも1つのC1〜C12アルキル(メタ)アクリレートの重合残基を更に含む、請求項6に記載の前記方法。
- 前記モノマーの5重量%未満が、前記第1のモノマー混合物の添加前に、前記重合反応容器内に存在する、請求項7に記載の前記方法。
- 前記第1のモノマー混合物が、29〜41重量%の少なくとも1つのC3〜C6カルボン酸モノマーの重合残基及び58〜70重量%の少なくとも1つのC1〜C12アルキル(メタ)アクリレートの重合残基を含み、前記第2のモノマー混合物が、0.4〜1.5重量%の少なくとも1つの架橋剤の重合残基を含む、請求項8に記載の前記方法。
- 前記第1のモノマー混合物への前記第2のモノマー混合物の添加の時期が、前記重合反応容器への前記第1のモノマー混合物の50〜100%の添加の時期である、請求項9に記載の前記方法。
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WO2019023116A1 (en) | 2017-07-24 | 2019-01-31 | Dow Global Technologies Llc | POLYACRYLATE OIL GEL COMPOSITION FOR PERSONAL CARE |
WO2019023114A1 (en) | 2017-07-24 | 2019-01-31 | Dow Global Technologies Llc | PERSONAL CARE POLYACRYLATE OIL GEL COMPOSITION |
WO2019023107A1 (en) | 2017-07-24 | 2019-01-31 | Dow Global Technologies Llc | SOLAR SCREEN COMPOSITIONS FOR PERSONAL CARE |
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