CN1135724A - 制备无水流散粒的糖表面活性剂粉末的方法 - Google Patents
制备无水流散粒的糖表面活性剂粉末的方法 Download PDFInfo
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- CN1135724A CN1135724A CN94194235A CN94194235A CN1135724A CN 1135724 A CN1135724 A CN 1135724A CN 94194235 A CN94194235 A CN 94194235A CN 94194235 A CN94194235 A CN 94194235A CN 1135724 A CN1135724 A CN 1135724A
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- Prior art keywords
- alkyl
- carbon atoms
- formula
- acid
- alkenyl
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 41
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 40
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000000344 soap Substances 0.000 claims abstract description 4
- -1 alkenyl sulfate Chemical compound 0.000 claims description 39
- 239000004094 surface-active agent Substances 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 24
- 125000004432 carbon atom Chemical group C* 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 150000002632 lipids Chemical class 0.000 claims description 21
- 239000003945 anionic surfactant Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 229930182470 glycoside Natural products 0.000 claims description 13
- 150000002338 glycosides Chemical class 0.000 claims description 13
- 238000006253 efflorescence Methods 0.000 claims description 12
- 206010037844 rash Diseases 0.000 claims description 12
- 229910052728 basic metal Inorganic materials 0.000 claims description 10
- 150000003818 basic metals Chemical group 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 5
- 150000001342 alkaline earth metals Chemical group 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 4
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 125000003147 glycosyl group Chemical group 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- QFWSIJKSJPEHCF-BTVCFUMJSA-N azane;(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal Chemical compound N.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O QFWSIJKSJPEHCF-BTVCFUMJSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical class [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 125000003473 lipid group Chemical group 0.000 claims 1
- 239000013543 active substance Substances 0.000 abstract description 12
- 239000000606 toothpaste Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 238000001035 drying Methods 0.000 description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 17
- 229930182478 glucoside Natural products 0.000 description 16
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 12
- 150000002148 esters Chemical class 0.000 description 12
- 239000003921 oil Substances 0.000 description 11
- 235000019198 oils Nutrition 0.000 description 11
- 239000004115 Sodium Silicate Substances 0.000 description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 10
- 229910052911 sodium silicate Inorganic materials 0.000 description 10
- 239000008103 glucose Substances 0.000 description 9
- 229940034610 toothpaste Drugs 0.000 description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000012752 auxiliary agent Substances 0.000 description 7
- 235000019353 potassium silicate Nutrition 0.000 description 7
- 244000060011 Cocos nucifera Species 0.000 description 6
- 235000013162 Cocos nucifera Nutrition 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 150000002191 fatty alcohols Chemical class 0.000 description 6
- 229920000151 polyglycol Polymers 0.000 description 6
- 239000010695 polyglycol Substances 0.000 description 6
- 229960001866 silicon dioxide Drugs 0.000 description 6
- 239000003760 tallow Substances 0.000 description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 159000000000 sodium salts Chemical group 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 4
- BTFJIXJJCSYFAL-UHFFFAOYSA-N arachidyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCO BTFJIXJJCSYFAL-UHFFFAOYSA-N 0.000 description 4
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 235000019253 formic acid Nutrition 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 229940055577 oleyl alcohol Drugs 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical group [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229940096386 coconut alcohol Drugs 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 230000001180 sulfating effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- CFOQKXQWGLAKSK-KTKRTIGZSA-N (13Z)-docosen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCCO CFOQKXQWGLAKSK-KTKRTIGZSA-N 0.000 description 2
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 2
- DJYWKXYRGAMLRE-QXMHVHEDSA-N (z)-icos-9-en-1-ol Chemical compound CCCCCCCCCC\C=C/CCCCCCCCO DJYWKXYRGAMLRE-QXMHVHEDSA-N 0.000 description 2
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 2
- CFOQKXQWGLAKSK-UHFFFAOYSA-N 13-docosen-1-ol Natural products CCCCCCCCC=CCCCCCCCCCCCCO CFOQKXQWGLAKSK-UHFFFAOYSA-N 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ZFMSMUAANRJZFM-UHFFFAOYSA-N Estragole Chemical compound COC1=CC=C(CC=C)C=C1 ZFMSMUAANRJZFM-UHFFFAOYSA-N 0.000 description 2
- 239000005792 Geraniol Substances 0.000 description 2
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
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- 241000208317 Petroselinum Species 0.000 description 2
- 240000004760 Pimpinella anisum Species 0.000 description 2
- 235000012550 Pimpinella anisum Nutrition 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 125000005233 alkylalcohol group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 2
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
- 239000008116 calcium stearate Substances 0.000 description 2
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- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 230000001877 deodorizing effect Effects 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
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- 238000004821 distillation Methods 0.000 description 2
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- 150000004665 fatty acids Chemical class 0.000 description 2
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- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 239000001683 mentha spicata herb oil Substances 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/42—Amides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
- A61K8/604—Alkylpolyglycosides; Derivatives thereof, e.g. esters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C233/00—Carboxylic acid amides
- C07C233/01—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C233/16—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by singly-bound oxygen atoms
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Abstract
用100至225℃温度范围的过热水蒸汽处理含(a1)烷基和/或链烯基低聚苷和/或(a2)脂肪酸-N-烷基多羟基烷基酰胺的含水制剂,并分离干燥的产物,得到无水流散粒的糖表面活性剂粉。该产物具有优越的气味和味道,适合用于制备表面活性剂,尤其适合于制备牙膏和香皂。
Description
发明的领域
本发明涉及一种用于制备无水、流散粒的糖表面活性剂粉末的方法,其中用100至225℃的过热水蒸汽处理烷基和/或链烯基低聚苷和/或脂肪酸-N-烷基多羟基烷基酰胺,并涉及该物质在制备表面活性剂方面的应用。
背景技术
烷基和/或链烯基低聚苷和优选的烷基低聚葡糖苷是基于可再生的原料的非离子表面活性剂,由于其优异的工业应用性能和其特别的生态毒理学上可适应性,它对制备表面活性剂越来越重要。同样也适用于另一类糖表面活性剂,即脂肪酸-N-烷基多羟基烷基酰胺,尤其是脂肪酸-N-烷基葡糖酰胺。
这两种糖表面活性剂特别适用的市场领域是口腔及牙齿保护制剂领域。例如在国际专利申请WO91/02046(Henkel)中提出了含有硅酸和烷基低聚葡糖苷并适合用于制作牙膏的粉状配制品。国际专利申请WO91/02513(Henkel)公开了抑制牙垢的牙膏,它含有抗微生物有效的双胍、氧化铝三水合物作研磨剂和例如烷基低聚葡糖苷作表面活性剂组分。德国专利申请DE-A14101505(Henkel)公开了含有烷基醚硫酸盐和烷基低聚葡糖苷混合物的口腔卫生和牙齿护理剂。最后,日本专利申请JP1/068,312(Shiseido)建议了一种发泡性能良好的牙膏,它含有磷酸氢钙、甘油、羧甲基纤维素和十一烷基葡糖苷。
尽管有这些公知的现有技术,但含有烷基低聚葡糖苷和脂肪酸-N-烷基葡糖酰胺的牙齿护理剂至今仍未上市。对此有多种原因:
1、由于生产中,烷基低聚葡糖苷含有约1至2%(重量)游离的脂肪醇,它通常不能通过蒸馏除去。然而,该微量含量在牙膏中会产生不可接受的恶劣的口味。
2、不仅烷基低聚葡糖苷而且脂肪酸-N-烷基葡糖酰胺可能由于过氧化物漂白处理而含有约0.5%(重量)蚁酸或甲酸酯。该含量在生理学上虽不重要,但对产品口味的影响却非常明显。
3、在配制牙膏时,必须使用无水形式或至少高度脱过水的糖表面活性剂,优选以粉末形式使用。按照传统的工业工艺,烷基低聚葡糖苷和脂肪酸-N-烷基葡糖酰胺都不能制得无水形式,因为敏感的糖基在喷雾干燥或薄膜蒸发器条件下通过热的金属壁的热传递会发生大量的碳化现象。
4、在无机盐存在下过热蒸汽干燥含水的糖表面活性剂虽然原则上已公知[参见DE-A14030688,WO93/15813(Henkel)],但在申请人的这两篇文献中所述的在约300℃的典型温度下,虽然设想会有正常的干燥作用,但却在塔壁上出现部分的碳化和烧结。另外,其中所述的方法仅仅通过实施例说明了对于阴离子表面活性剂的热蒸汽干燥。
5、另一个困难还在于,用传统方法干燥的糖表面活性剂粉末尤其当含有阴离子表面活性剂例如烷基硫酸酯类作为另一种成分时不能充分溶于冷水中,且表观密度不适宜的低。
因此,本发明的综合任务在于,提出一种制备无水固体形式的糖表面活性剂的方法,该方法不具有所述的缺点。
发明的说明
本发明的主题是一种用于制备无水、流散粒的糖表面活性剂粉末的方法,其中使用100至225,优选150至200℃的温度范围的过热水蒸汽处理含a1)烷基和/或链烯基低聚苷和/或a2)脂肪酸-N-烷基多羟基烷基酰胺的含水配制品,并分离出于燥的物料。
令人惊奇地发现,用本发明方法得到的含糖表面活性剂和必要时的阴离子表面活性剂的无水糖表面活性剂粉末不但有特别优异的流动性和色质,而且还特别易溶于水。对产品口味和气味有不利影响的游离脂肪醇、蚁酸及其盐实际上可以和水一起完全除去,或者至少降低到从工业应用角度不再有影响的浓度。因此,第一次提供了糖表面活性剂及其与阴离子表面活性剂的混合物的一种干燥方法,其中的热传递不是通过与一个热的金属壁接触而进行的。
本发明包括,如果要将干燥温度降低到既不形成碳化产物又不烧结的程度,从而得到一种不粘的、干燥的、可流散粒的粉末,则使用特定的硅酸盐载体是特别有利的。
本发明方法得到的糖表面活性剂粉末的优越性还在于大大改善了气味和口味。
烷基和/或链烯基低聚苷
烷基和/或链烯基低聚苷如下式(I)所示,
R1O-[G]p (I)式中R1为含6至22个碳原子的烷基和/或链烯基,G为含5或6个碳原子的糖基,P是1至10之内的一个数值。它仍是可用制剂有机化学的有关方法获得的已知物质。作为众多文献的代表可参见EP-A1-0301298和WO90/03977。
烷基和/或链烯基低聚苷可由含5或6个碳原子的醛糖或酮糖衍生,优选的由葡糖衍生。因此,优选的烷基和/或链烯基低聚苷为烷基和/或链烯基低聚葡糖苷。
通式(1)中的指数P表示低聚度(DP度),也就是说单和低聚苷的分布,为1至10之间的一个数值。P在给定化合物中必须是整数,首先可认为P=1至6,但对于一定的烷基低聚苷来说,分析计算得到P值常常为一个分数。优先使用平均低聚度P为1.1至3.0的烷基和/或链烯基低聚苷。从应用观点看,优选的是那些低聚度小于1.7尤其在1.2和1.4之间的烷基和/或链烯基低聚苷。
烷基或链烯基R1可由含6至11,优选8至10个碳原子的伯醇衍生。典型的实例是丁醇、己醇、辛醇、癸醇和十一醇以及其所得的工业混合物,例如在氢化工业脂肪酸甲酯或氢化由Roelen′schen羰基合成所形成的醛的过程中所得的混合物。优选的是链长C8-C10的烷基低聚葡糖苷(DP=1至3),它是蒸馏分离工业的C8-C18-椰子油脂肪醇时得到的初馏物,可以混杂有低于6%(重量)的C12-醇,还优选基于工业C9/11-羰基合成醇的烷基低聚葡糖苷(DP=1至3)。
烷基或链烯基R1还可以由含12至22,优选12至14个碳原子的伯醇衍生。典型的实例是月桂醇,肉豆蔻醇,鲸蜡醇,棕榈油醇,硬脂醇,异硬脂醇,油醇,反油醇,岩芹醇,花生醇,二十碳烯醇,山萮醇,瓢儿菜醇,以及上述可获得的其工业混合物。优选的基于固化C12/14-椰子油脂肪醇的DP为1至3的烷基低聚葡糖苷。
脂肪酸-N-烷基多羟基烷基酰胺
脂肪酸-N-烷基多羟基烷基酰胺如式(II)所示,式中R2CO为6至22个碳原子的脂族酰基,R3为氢、1至4个碳原子的烷基或羟基烷基,[Z]为含3至12个碳原子和3至10个羟基的直链或支链的多羟基烷基。
脂肪酸-N-烷基多羟基烷基酰胺是已知化合物,它可以通过用氨、烷基胺或烷基醇胺对还原糖进行还原性胺化,并接着用脂肪酸、脂肪酸烷基酯或脂肪酰氯进行酰化而获得。关于其制备方法可参考美国专利US1985424、US2016962和US2703798以及国际专利申请WO92/06984。H.Kelkenberg对该主题的综述列于Tens.Surf.Det.25,8(1988)上。
脂肪酸-N-烷基多羟基烷基酰胺优选的是由含5或6个碳原子的还原糖衍生,尤其由葡糖衍生。优选的脂肪酸-N-烷基多羟基烷基酰胺是式(III)所示的脂肪酸-N-烷基葡糖酰胺:
作为脂肪酸-N-烷基多羟基烷基酰胺,优选使用式(III)的葡糖酰胺,其中R3为氢或氨基,R2CO为下列酸的酰基,这些酸是己酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、硬脂酸、异硬脂酸、油酸、反油酸、岩芹酸、亚油酸、亚麻酸、花生酸、二十碳烯酸、山嵛酸、或芥酸及其工业混合物。特别优选的式(III)脂肪酸-N-烷基葡糖酰胺是用甲胺对葡糖进行还原性胺化,并接着用月桂酸或C12/14-椰子油脂肪酸或相应的衍生物酰化而得到的。另外,多羟基烷基酰胺也可由麦芽糖和苯二甲酸糖(Palatinose)衍生。
阴离子表面活性剂
在本发明的一种特别的实施方式中,除糖表面活性剂外还干燥含有阴离子表面活性剂的含水制剂。
对此典型的实例是烷基苯磺酸酯,烷基磺酸酯,烯烃磺酸酯,烷基醚磺酸酯,甘油醚磺酸酯,α-磺酸甲酯,磺基脂肪酸,烷基和/或链烯基硫酸酯,脂肪醇醚硫酸酯,甘油醚硫酸酯,羟基混合醚硫酸酯,单甘油(醚)硫酸酯,脂肪酰胺(醚)硫酸酯,单-和二-烷基磺基丁二酸酯,单-和二-烷基磺基丁二酰胺酯,磺基三甘油酯,酰胺皂,醚羧酸及其盐,脂肪酸羟乙磺酸酯,脂肪酸肌氨酸酯,脂肪酸牛磺酸酯(tauride),酰基乳酸酯,酰基谷氨酸酯,酰基酒石酸酯,烷基低聚葡糖苷硫酸酯,蛋白脂肪酸缩合物(尤其是大豆基植物的产物)和烷基(醚)磷酸酯。只要阴离子表面活性剂含有聚乙二醇醚的链,它就可以具有常规的但优选的是窄的同系物分布。
烷基和/或链烯基硫酸盐
在本发明的一种优选实施方式中,除糖表面活性剂外还干燥含有烷基和/或链烯基硫酸盐作阴离子表面活性剂的含水制剂。烷基和/或链烯基硫酸盐是伯醇的硫酸化产物,相应于式(IV)
R4O-SO3X (IV)式中R4为含6至22,优选12至18个碳原子的直链或支链的脂族烷基和/或链烯基,X为碱金属和/或碱土金属、铵、烷基铵、链烷醇铵或葡糖铵。
本发明可以应用的烷基硫酸盐的典型实例是己醇、辛醇、癸醇、2-乙基已醇、月桂醇、肉豆蔻醇、鲸蜡醇、棕榈油醇、硬脂醇、异硬脂醇、油醇、反油醇、岩芹醇、花生醇、二十碳烯醇、山嵛醇和瓢儿菜醇及其工业混合物的硫酸化产物,该工业混合物是通过工业甲酯馏分或由Roelen′schen羰基合成的醛的高压加氢所制得的。该硫酸化产物可以优选的以其碱金属盐、尤其是其钠盐形式使用。
特别优选的式(IV)的烷基硫酸盐中,***R4为含16至18个碳原子的烷基,X为钠,或***R4为含12至18个碳原子的烷基,X为钠,但要符合其中16至
18个碳原子与12至14个碳原子的烷基之比为50∶50至90∶10重
量份的条件。
典型的实例是C16/18-牛脂醇硫酸钠盐或C16/18-牛脂醇硫酸钠盐与C12/14-椰子脂醇硫酸钠盐以60∶40或80∶20重量比的混合物。
会水制剂
本发明中,含水制剂可理解为可以含有所述糖表面活性剂和另外的阴离子表面活性剂的含水制剂,它具有固体含量为5至70,优选40至60%(重量)的溶液或浆料。考虑到蚁酸及甲酸盐的分离,已证明采用PH值为6至11,优选6.5至9的制剂特别有利。例如柠檬酸适用于调节PH值。
碱金属和/或碱土金属硅酸盐
在水蒸汽处理时,由于晶核的存在,容易形成固体表面活性剂颗粒。例如无机和/或有机盐即适合用于此目的。由于要制备流散粒、非粘性、干燥、易溶于水的粉末,从大量可以考虑的物质中选择载体是重要的。业已证明,碱金属和/或碱土金属的硅酸盐尤其可使粉末具有所需的性能。
因此,作为载体可以用水玻璃,尤其是所谓的“过干燥的”水玻璃,其“模数”即(SiO2)∶(M2O)之比为0.5至5,尤其是1至3.5。优选采用模数约为2的钠水玻璃。过度干燥的水玻璃本身可由通常的水玻璃通过过热蒸汽干燥或在含水制剂干燥期间就地干燥而制备。典型的实例是Henkel KGaA(Dusseldolf/FRG)的两种产品“钠水玻璃N50/55(模数2.O)”和“钠水玻璃N37/40(模数3.45)”以及Süd-chemie AG(München/FRG)的硅酸镁Optigel(R)SH。
基于最终粉末的固体含量,碱金属和/或碱土金属硅酸盐的用量为0.1至50,优选15至30%(重量)。
载体
虽然碱金属硅酸盐是优选用作载体,但它们也可易于与其它材料例如无机或有机盐混合。无机盐典型的实例是碱金属和/或碱土的金属氧化物、硫酸盐、碳酸盐、碳酸氢盐、磷酸盐,焦磷酸盐、硅酸盐和卤化物。特别优选使用的是硫酸钠、碳酸钠、碳酸钙、磷酸钠、焦磷酸钙、氯化钠、层状硅酸盐、沸石、水滑石和氧化镁。
SiO2含量大于99.8%(重量)的高分散性硅石已证明是特别适用的助载体,它不应与水玻璃型的助剂混淆。高分散二氧化硅(Aqero-sil)由非晶形球状颗粒构成,其直径为10至20nm,其内表面为100至400m2/g。高分散二氧化硅的表面上有SiOH基团,它们通过较弱的氢桥键相互连结,由此形成构架。高分散二氧化硅例如为Degu-ssa(Hanau/FRG)的市售产品。其详细结构可参见Seifen-Ole-Fette-Wachse,94,849(1968)。
有机盐典型的实例是碱金属和/或碱土金属皂,尤其是醋酸钠、硬脂酸镁和硬脂酸钙。其它的有机载体也可以考虑多糖如天然的和/或化学改性、酸降解的(玉米)淀粉。后者在提高粉末的胶凝温度方面是有利的。
上述助载体的用量可为载体材料总量的1至25%,优选5至15%(重量)。
水蒸汽处理
在本发明的方法中,使非离子表面活性剂的含水制剂和盐以及必要时的载体物质一起在没有空气氧的存在下用过热水蒸汽处理。这种新型工艺方法的原理已由中请人在德国专利申请DE-A14030688、DE-A14204035、DE-A1-4204090、DE-A1-4206050、DE-A14206495和DE-A14206521中公开。
该方法的原理是,通过热蒸汽在较冷物料上的冷凝并向待干燥物料释放冷凝热量,而将水滴自发地加热到操作条件下水的沸点,也即在常压下100℃的温度。在整个停留期间的物料滴中保持该沸点温度作为最低温度。在通常条件下不能或仅在苛刻条件下并用相当高昂的设备才能除去的水蒸汽挥发性杂质例如脂肪醇或蚁酸,按本方式可快速、完全而准确地与水相一起分离出去。
在本发明方法一含优选的实施方式中,使含水制剂与150至225℃范围的温度的过热水蒸汽一起喷雾入一个密闭体系,则冷凝水与溶于其中的杂质一起除去,而干燥和提纯的有用物质由系统中排出。
从根本上讲,方法是在密闭体系中用水蒸汽循环流进行,其中去除由物料中蒸发的水含量,而将放出的能量重新回到循环流。因而,在常规方法中,在高温下操作常常会有要净化物料部分碳化的危险,而这里由于没有空气氧,所以有可能使用特别是150至225℃,优选170至200℃的操作温度。在分离出溶解的杂质后分出的水蒸汽支流可以有利地作为工业蒸汽用于其它场合。
粉化
根据本发明方法的一种特别优选的实施方式,为了可靠地排除仍有可能存在的残留粘性,用合适的细粒固体处理“粉化”干燥的有用物料,可以得到具有流动性能特别好的糖表面活性剂。这里作为适宜固体基本上可以考虑那些在用水蒸汽处理时已经作为合适的载体提出的物质,或者在任何情况下可以用于表面活性制剂的物质。典型的实例是盐,例如硅酸盐,氯化钠,硫酸钠,磷酸钠,焦磷酸钠,硬脂酸钙,尤其是具有高内表面的二氧化硅(高分散性二氧化硅)。以糖表面活性剂粉末为基,用于粉化固体的用量通常为0.1至5,优选0.5至1%(重量)。
粉化可以作为其后的步骤进行。但优选是在喷雾干燥塔中进行,这样可以保证粉均匀地排放,并可靠地避免在塔壁上的烧结。在本发明一种优选的实施方式中,在喷雾干燥塔顶部送入粉化的物质,这里用载体材料进行粉化是特别有利的。在这种情况下,粉化材料的量优选为整个载体量的约30%,而整个载体量在特别有利的情况下约为最终干燥物料的30%(重量)。若粉末中的糖表面活性剂含量超过50%(重量),则粉化步骤是特别有利的。在粉化步骤中可能形成容积大的集块,但它们在冷却时及通过机械运动时即迅速分解。
表面活性剂
需要时,可将用于其后制备所需的助剂和添加剂补充混合到后续步骤的糖表面活性剂粉末中。然而,当该组分具有足够的热稳定性时,也可以使其与糖表面活性剂一起进行水蒸汽处理。
在助剂和添加剂中首先包括其它的表面活性剂:非离子表面活性剂的典型实例是脂肪醇聚乙二醇醚、烷基酚聚乙二醇醚、脂肪酸聚乙二醇醚、脂肪酰胺聚乙二醇醚、脂肪胺聚乙二醇醚、烷氧基化三酸甘油酯、多元醇脂肪酸酯、糖酯、山梨醇酯和多山梨酸酯。如果非离子表面活性剂含有聚乙二醇醚链,则它仍就可以具有正常的同系物分布,但优选的是具有窄范围的同系物分布。
阳离子表面活性剂典型的实例是季铵化合物和季胺化二脂肪酸三链烷醇胺酯。两性或两性离子表面活性剂典型的实例是烷基甜菜碱,烷基酰胺甜菜碱,氨基丙酸酯,氨基甘氨酸酯,咪唑甜菜碱和磺基甜菜碱。
所述的表面活性剂都是已知化合物。其结构及物质的制备可参见有关综述文章,例如J.Falbe(ed.)“Surfactants in ConsumerProducts”,Springer出版社,柏林,1987,54-124页或J.Fal-be(ed.),“Katalysatoren,Tenside und Mineraloladditive”,Thieme出版社,斯图加特,1978,123-217页。
香料
作为其它助剂和添加剂,考虑下面的香料,例如薄荷油、绿薄荷油、大茴香油、八角茴香油、黄蒿子油、桉树油、小茴香油、肉桂油、荨麻油、香叶油、鼠尾草油、甘椒油、麝香油、马郁兰油、罗勒油、柑桔油、白珠树油或者一或多种由这些油分离或合成制备的成分,例如甲醇、香芹酮、茴香脑、桉树脑、丁子香酚、肉桂醛、子丁香烯、香叶醇、香茅醇、沉香醇、鼠尾草烯、百里酚,萜品烯、萜品醇、甲基佳味酚和水杨酸甲酯。其它合适的香料是,例如醋酸甲酯、香子兰醛、芷香酮、乙酸里哪酯、玖红醇和薄荷酮。适合用作甜味剂的不仅有天然糖如蔗糖、麦芽糖、乳糖和果糖,还有合成的甜味剂如糖精钠盐、环己烷氨基磺酸钠和天冬酰苯丙氨酸甲酯。
助剂和添加剂
此外,特别是在牙膏中,作为助剂和添加剂,还可以加入保湿剂如山梨醇或甘油,稠度调节剂,脱臭剂,治疗口腔和牙病的活性成分,水溶性氟化物例如氟化钠或一氟磷酸钠和研磨剂或抛光剂。
助剂和添加剂的用量基本上并不严格,由最终配制的制剂性质决定。通常,以糖表面活性剂粉末为基准,其用量为5至70%,优选10至50%(重量)。
工业实用性
按本发明方法得到的糖表面活性剂粉末含有低于10%,优选低于5%,特别优选低于1%(重量)的水。其流动性能良好,不粘结,易溶于水且气味和口味性能突出。
因此,本发明的另一个主题是其在制备表面活性剂,优选是化妆品如牙膏或合成皂方面的应用,其中以制剂为基准,可以含有0.5到50%,优选1至10%(重量)的糖表面活性剂粉末。
下面用实施例进一步说明本发明,但并不限制本发明。
实施例
1、含水糖表面活性剂的过热蒸汽干燥
Z1)C12/16-椰子烷基低聚葡糖苷(DP=1.3,Plantaren(R)APG1200CS UP,Henkel KGaA,杜塞尔多夫/联帮德国,含50%(重量)固体,45%(重量)活性物质,1.2%(重量)游离脂肪醇和0.4%(重量)甲酸钠)。
Z2)C12/14-椰子脂肪酸-N-甲基葡糖酰胺(50%(重量)固体)。
实施例1至10,对比例V1至V3
通用制备方法:在NIRO ATOMIZER公司的一个试验喷雾干燥塔中将由一种糖表面活性剂桨料Z1或Z2和必要时的一种载体所组成的混合物在744毫巴的减压下用过热水蒸汽干燥和除臭。这里,由糖表面活性剂和载体组成的含水浆液从下面喷入喷雾干燥塔中(喷泉原理)。过热的水蒸汽(180-200℃)从上面与液体逆向吹入干燥塔中,并从塔体下面(130℃)排出。必要时在紧靠塔顶盖下方连续地计量加入粉化料。该粉化料通过蒸汽流均匀地分布在于燥塔中,以使实际上所有颗粒都被粉化。粉末通过在废蒸汽管下方的一个双振动阀而排放。其它工艺参数列于表1中:
表1:工艺数据
水蒸汽
排出物
喷气 干燥剂入口温度(℃) 70 130 180-200出口温度(℃) 130处理量(kg/h) 15 2 400*压力巴 1,5 0,4*)数量级m3/h
在干燥器中的停留时间约为10秒钟。由水蒸汽夹带入的杂质可在冷凝后在两相分离器中通过微过滤或超过滤而从冷凝水中分离。试验结果列于表2中(百分数以重量%表示)。
表2.试验混合物与表观密度
说明:
例 | ZT | [ZT]% | TR | [TR]% | PM | [PM]% | 表观密度g/l |
12345678910 | Z1Z1Z1Z1Z1Z1Z1Z1Z1Z2 | 87797070707070707070 | T1T4T4T6T7T4T9T0T4T4 | 5202020202020203020 | T2T1T6T4T7T8T9T0-- | 81101010101010-- | 327597407425519421465#647#380405 |
V1V2V3 | Z1Z1Z1 | 757585 | T1T1T5 | 15515 | T3T3- | 1020- | 无产物无产物无产物 |
ZT=糖表面活性剂
TR=载体
PM=粉
[X]=X的浓度(以最终产物为基准)
#=低的产物产率
T1=硫酸钠
T2=亲水化的SiO2(Aerosil(R)R972)
T3=甲基纤维素(Culminal(R))
T4=钠水玻璃N55
T5=纤维素纤维(Arbocel(R))
T6=空气干燥的水玻璃(Portil(R)N)
T7=硅酸镁(Optigel(R)SH)
TB=空气干燥的水玻璃(Portil(R)A)
T9=膨润土(Optigel(R)CL)
T0=滑石α CT 12X
对比例V4:
使一种由70%(重量)Plantaren(R)APG1200 CS UP和30%(重量)钠水玻璃N55组成的混合物在一台旋转蒸发器中脱水。
对比例V5:
使一种由70%(重量)Plantaren(R)ApG1200 CS UP和30%(重量)钠水玻璃N55组成的混合物在一台薄膜蒸发器中脱水。
对比例V6:
使一种由70%(重量)C12/14-椰子脂肪酸-N-甲基葡糖酰胺和30%(重量)钠水玻璃N55组成的混合物在一台旋转蒸发器中脱水。
在牙膏中应用:
将本发明实施例3至5以及9和10及对比例V4至V6的无水产物(“表面活性剂”)加入一种标准的牙膏配方中(水加至100%(重量)):
21.0g沉淀二氧化硅(Sident(R)12 DS)
1.0g浓缩凝胶二氧化硅(Syloblanc(R)34)
1.2g羧基甲基纤维素钠
0.1g糖精钠盐
0.1g苯甲酸钠盐
1.0g口腔护理芳香油1/074568(Dragoco)
15.0g山梨醇(70%(重量),于水中)
25.0g甘油(86%(重量),于水中)
0.2g氟化钠
2.0g表面活性剂
由5个无关的测试人刷牙后按以下标准评价口味(见表3):
++=香味为主,无异味
+ =有轻微的异味
- =异味强烈
NG=余味
按以下标准主观评价产物的流动性:
+++=流动性优越,颗粒无粘性
++ =流动性好,颗粒有轻度粘结
+ =流动性尚可,中度粘结
- =流动性差,颗粒粘结并结块
表3:产物的组成及评价[百分数以%(重量)表示]
说明:FS=固体含量
例 | [FSt]% | [FF]% | [NF]% | [H2O]% | 口味 | RF |
345910 | 99,799,799,799,7- | 0,30,30,30,3- | 0,10,10,10,1- | 0,10,10,10,1- | +++++++ | +++++++++++ |
V4V5V6 | 97,9-97,9 | --- | 0,4-0,4 | 2,1-2,1 | -NG-NG-NG | --- |
FF=游离脂肪醇含量
NF=甲酸钠含量
H2O=水含量
RF=流动性
II.含水糖/阴离子表面活性剂的热蒸汽干燥
实施例11至21:
类似于实施例1使由糖表面活性剂和阴离子表面活性剂以及必要时的载体盐组成且固含量共50%(重量)的含水制剂干燥。得到干燥的、易流动并在水中迅速溶解的浅色产物。结果列于表4中。
对比例V7至V15:
为了对比,对无载体的牛脂醇硫酸酯或椰子烷基低聚葡糖苷用热蒸汽进行处理(V7,V8)。再以公知的方式在旋转蒸发器中使不同的含水制剂脱水。得到黄褐色的物料,在其粉化后呈现了相当低的溶解速度(V9至V15)。结果列于表4中。
产物的颜色和溶解性:对发明以及对比产物的颜色进行主观评价(1=白至6=褐色)。为了确定溶解性,将25g粉状产物放入20℃的100ml 16°d的水中,搅拌15秒,然后通过过滤器中。将滤渣干燥至恒量并称重。计算出滤渣量与所用粉末重量之比。细节可由表4得到(百分数据为重量%)。
表4.颜色及溶解性
说明:A1=C16/18-牛脂醇硫酸钠盐
例 | A | [A]% | B | [B]% | C | [C]% | 色 | 滤渣% |
1112131415161718192021 | A1A2A1A2A1A1A1A1A1A1A2 | 9590858075408080808080 | B1B2B2B1B1B3B3B4B1B2B2 | 510152025602020151510 | --------C1C2C2 | --------5510 | 22222222111 | 887781077776 |
V7V8V9V10V11 | A1-A1A2A1 | 100-959085 | -B1B1B2B2 | -10051015 | ----- | ----- | 22344 | 1919394138 |
V12V13V14V15 | A2A1A1A1 | 80758080 | B1B1B3B4 | 20252020 | ---- | ---- | 5655 | 35424039 |
A2=C12/18-椰子醇硫酸钠盐
B1=C12/14-椰子烷基低聚葡糖苷
B2=C8/16-烷基低聚葡糖苷
B3=月桂酸-N-甲基葡糖酰胺
B4=C12/14-椰子脂肪酸-N-甲基葡糖酰胺
C1=钠水玻璃(模量约为3.4)
C2=钠水玻璃(模量约为1)
该实施例和对比例表明,用热蒸汽干燥糖表面活性剂和阴离子表面活性剂的混合物可导致相对于原料来说有协同地改进溶解度的产物,而且有利地使表观密度高达400至550g/l。与传统的干燥方法相比,最终可得到水溶性和颜色都得到改进的粉末。
产物的流动性和粘性:类似于实施例11,按重量比为80∶20的糖表面活性剂或非离子表面活性剂与阴离子表面活性剂的不同混合物进行热蒸汽干燥,以标度1(流动性很好或很干燥)至6(结块或很粘)评价其流动性能(R)及粘性(K)。另外,还测定其表现密度(SG)。用热蒸汽干燥的钠水玻璃作为载体(干燥物料重量的10%)。结果列在表5中。
表5.流动性、粘性和表观密度例序阴离子表面活性剂非离子表面活性剂 R K SG
(Niotensid) g/l22 牛脂醇硫酸钠盐 椰子低聚葡糖苷 1 1 22023 牛脂醇硫酸钠盐/
椰子醇硫酸钠盐 椰子低聚葡糖苷 1 2 220
(60∶40)24 椰子醇硫酸钠盐 椰子低聚葡糖苷 1 3 220V16 十二烷基苯磺酸 椰子低聚葡糖苷 2 5 175
钠盐V17 十二烷基苯磺酸 椰子醇-2EO 2 6 150
钠盐 加成物
该实施例和对比例表明;本发明可以获得较高表现密度和改进的流动性能且具有低粘性的粉末。
Claims (17)
1、制备无水流散粒的糖表面活性剂粉的方法,其中用100至225℃温度的过热的水蒸汽处理含有(a1)烷基和/或链烯基低聚苷和/或(a2)脂肪酸-N-烷基多羟基烷基酰胺的含水制剂,并分离出干燥的物料。
2、按照权利要求1的方法,其特征是,用式(I)的烷基和/或链烯基低聚苷作为组分(a1),
R1O-[G]p (I)式中R1为含6至22个碳原子的烷基和/或链烯基,G为含5或6个碳原子的糖基,P为1至10之内的一个数值。
4、按照权利要求1至3的方法,其特征是,使用另外还含有阴离子表面活性剂的含水制剂。
5、按照权利要求4的方法,其特征是,用式(IV)的烷基和/或链烯基硫酸盐作阴离子表面活性剂(组分b)。
R4O-SO3X (IV)式中R4为含8至22个碳原子的烷基和/或链烯基,X为碱金属和/或碱土金属、铵、烷基铵、链烷醇铵或葡糖铵。
6、按照权利要求5的方法,其特征是,所用式(IV)的烷基硫酸盐中,R4为含16至18个碳原子的烷基,X为钠。
7、按照权利要求5的方法,其特征是,所用式(IV)的烷基硫酸盐中,R4为含12至18个碳原子的烷基,X为钠,而且含16至18个碳原子与含12至14个碳原子的烷基之比为50∶50至90∶10重量份。
8、按照权利要求1至7的方法,其特征是,所用组分(a)和(b)的重量比为40∶60至99∶1。
9、按照权利要求1至8的方法,其特征是,所用含水制剂中的固体含量为5至70%(重量)。
10、按照权利要求1至9的方法,其特征是,在碱金属和/或碱土金属硅酸盐作为载体的存在下而进行干燥的。
11、按照权利要求1至10的方法,其特征是,用选自碱金属和/或碱土金属的氧化物、硫酸盐、碳酸盐、碳酸氢盐、磷酸盐、焦磷酸盐和卤化物的无机盐作为另一种载体。
12、按照权利要求1至11的方法,其特征是,用高分散硅酸作为另一种载体。
13、按照权利要求1至12的方法,其特征是,用碱金属和/或碱土金属有机盐皂作为另一种载体。
14、按照权利要求1至13的方法,其特征是,以产品粉末中的固含量为基准,使用的载体量为0.1∶50%(重量)。
15、按照权利要求1至14的方法,其特征是,使含水制剂与温度为120至280℃的过热水蒸汽一起喷雾入一个密封系统中,冷凝水与溶于其中的杂质一起除去,并将干燥和提纯的有用物质由系统中排出。
16、按照权利要求1至15的方法,其特征是,对干燥的有用物料进行粉化。
17、权利要求1至16所述方法所得到的无水流散粒糖表面活性剂粉用于制备表面活性制剂。
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DE4340015A DE4340015C2 (de) | 1993-11-24 | 1993-11-24 | Verfahren zur Herstellung wasserfreier, rieselfähiger Zuckertensidpulver und deren Verwendung |
DEP4340015.9 | 1993-11-24 | ||
DEP4431157.5 | 1994-09-01 | ||
DE4431157 | 1994-09-01 |
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CN1135724A true CN1135724A (zh) | 1996-11-13 |
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CN94194235A Pending CN1135724A (zh) | 1993-11-24 | 1994-11-22 | 制备无水流散粒的糖表面活性剂粉末的方法 |
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EP (1) | EP0730484A1 (zh) |
JP (1) | JPH09505621A (zh) |
KR (1) | KR960705608A (zh) |
CN (1) | CN1135724A (zh) |
WO (1) | WO1995014519A1 (zh) |
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DE19524464C2 (de) * | 1995-07-10 | 2000-08-24 | Cognis Deutschland Gmbh | Verfahren zur Herstellung von Zuckertensidgranulaten |
DE19533539A1 (de) * | 1995-09-11 | 1997-03-13 | Henkel Kgaa | O/W-Emulgatoren |
DE19534371C1 (de) * | 1995-09-15 | 1997-02-20 | Henkel Kgaa | Verfahren zur Herstellung wasser- und staubfreier Zuckertensidgranulate |
DE19548068C1 (de) * | 1995-12-21 | 1997-06-19 | Henkel Kgaa | Verfahren zur Herstellung hellfarbiger, niedrigviskoser Tensidkonzentrate |
DE19710153C1 (de) | 1997-03-12 | 1998-02-12 | Henkel Kgaa | Verfahren zur Herstellung neutraler Zuckertensidgranulate |
DE19961333B4 (de) * | 1999-12-17 | 2006-12-14 | Henkel Kgaa | Verfahren zur Herstellung von Zuckertensidgranulaten |
DE10018812A1 (de) | 2000-04-15 | 2001-10-25 | Cognis Deutschland Gmbh | Verfahren zur Herstellung von nichtionischen Tensidgranulaten |
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DE4030688A1 (de) * | 1990-09-28 | 1992-04-02 | Henkel Kgaa | Verfahren zur spruehtrocknung von wertstoffen und wertstoffgemischen unter verwendung von ueberhitztem wasserdampf |
KR950700104A (ko) * | 1992-02-12 | 1995-01-16 | 게오르그 챠이트, 한스-크리스토프 빌크 | 습윤제, 세제 및/또는 클리닝제로 유용한 과립의 제조방법(process for producing granulates useful as wetting, washing and/or cleaning agents) |
DE4234376A1 (de) * | 1992-10-12 | 1994-04-14 | Henkel Kgaa | Wertstoffe und Wertstoffgemische für Netz-, Wasch- und/oder Reinigungsmittel in neuer Zubereitungsform |
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1994
- 1994-11-22 JP JP7514826A patent/JPH09505621A/ja active Pending
- 1994-11-22 CN CN94194235A patent/CN1135724A/zh active Pending
- 1994-11-22 KR KR1019960702663A patent/KR960705608A/ko not_active Application Discontinuation
- 1994-11-22 EP EP95902081A patent/EP0730484A1/de not_active Withdrawn
- 1994-11-22 WO PCT/EP1994/003855 patent/WO1995014519A1/de not_active Application Discontinuation
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KR960705608A (ko) | 1996-11-08 |
WO1995014519A1 (de) | 1995-06-01 |
JPH09505621A (ja) | 1997-06-03 |
EP0730484A1 (de) | 1996-09-11 |
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