CN109498486A - A kind of amphipathic titanium dioxide emulsifier, Pickering lotion and its preparation method and application - Google Patents
A kind of amphipathic titanium dioxide emulsifier, Pickering lotion and its preparation method and application Download PDFInfo
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- CN109498486A CN109498486A CN201910001998.XA CN201910001998A CN109498486A CN 109498486 A CN109498486 A CN 109498486A CN 201910001998 A CN201910001998 A CN 201910001998A CN 109498486 A CN109498486 A CN 109498486A
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- amphipathic
- emulsifier
- titanium
- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000006210 lotion Substances 0.000 title claims abstract description 43
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 36
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 150000003608 titanium Chemical class 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000002537 cosmetic Substances 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 229940043237 diethanolamine Drugs 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N tetraisopropyl titanate Substances CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical group Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 2
- 108010082495 Dietary Plant Proteins Proteins 0.000 claims description 2
- 241001465754 Metazoa Species 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 125000004442 acylamino group Chemical group 0.000 claims description 2
- -1 alkyl quaternary ammonium salts Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical group [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000787 lecithin Substances 0.000 claims description 2
- 229940067606 lecithin Drugs 0.000 claims description 2
- 235000010445 lecithin Nutrition 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 claims description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium(IV) ethoxide Substances [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical group 0.000 claims 1
- 239000004519 grease Substances 0.000 claims 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims 1
- RLJWTAURUFQFJP-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O.CC(C)O.CC(C)O RLJWTAURUFQFJP-UHFFFAOYSA-N 0.000 claims 1
- 150000003384 small molecules Chemical class 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 9
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000006071 cream Substances 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 230000001804 emulsifying effect Effects 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 235000002639 sodium chloride Nutrition 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound 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 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 241001494479 Pecora Species 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001568 sexual effect Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KZRXPHCVIMWWDS-AWEZNQCLSA-N (4S)-4-amino-5-dodecanoyloxy-5-oxopentanoic acid Chemical compound CCCCCCCCCCCC(=O)OC(=O)[C@@H](N)CCC(O)=O KZRXPHCVIMWWDS-AWEZNQCLSA-N 0.000 description 1
- 235000021357 Behenic acid Nutrition 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 229940116226 behenic acid Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229940071085 lauroyl glutamate Drugs 0.000 description 1
- 239000008308 lipophilic cream Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
-
- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/925—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of animal origin
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dermatology (AREA)
- Inorganic Chemistry (AREA)
- Zoology (AREA)
- Cosmetics (AREA)
- Colloid Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of amphipathic titanium dioxide emulsifier, Pickering lotion and preparation method thereof the following steps are included: S1, mixing titanium salt presoma and small organic molecule in alcohol-water solution, titanium salt solution is formed, makes small organic molecule surface hydrophilic and hydrophobic regulator to TiO2Surface is modified.S2, the aqueous solution of amphipathic titanium dioxide emulsifier is mixed, homogeneous with oiliness raw material, obtains Pickering lotion.The application is modified without cumbersome surface, only need to be in emulsifier TiO2Preparation when small organic molecule be added carry out that surface in situ is modified or modification, TiO can be made2With amphipathic and fabulous dispersibility, and then partial size can be formed at 1~20 μm, and the extremely stable Pickering miniemulsion with strong acid and alkali-resistance, high temperature resistant and electrolyte-resistant.
Description
Technical field
The present invention relates to filed of daily-use chemical industry, and in particular to a kind of amphipathic titanium dioxide emulsifier, Pickering lotion
And its preparation method and application.
Background technique
Pickering emulsion refers to using ultrafine particle as emulsion obtained from emulsifier, also referred to as
Pickering lotion.
Nano-solid particle replaces conventional surfactant to stablize oil-water interfaces and forms Pickering lotion, can avoid passing
System surfactant bring skin irritation, safety issue, the great application potential in cosmetics and personal-care supplies.
But often size droplet diameter is larger (reach at some tens of pm) for existing Pickering lotion, and vulnerable to pH value, ionic strength, temperature etc. because
Element influences and causes to be demulsified, and stability is lower, limits its application in cosmetics.Further, since ungroomed inorganic
Nano-solid particle dispersion is poor, easily reunites and hydrophily is strong, cause emulsifiability poor, need to often carry out thus to solid particle
Surface is modified, and by esterification, condensation, thus the reaction introducing portion lipophilic group such as cancellation may be used with obtaining suitable wetability
See, the method that nano-solid particle emulsifying agents are modified and are prepared in the prior art is relatively cumbersome, at high cost and modified
Degree is not easy to control.The problem of above problem is this field urgent need to resolve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of amphipathic titanium dioxide emulsifier, Pickering lotion and
Preparation method, it is modified without cumbersome surface, it only need to be in emulsifier TiO2Preparation when be added small organic molecule carry out table
Face is in-situ modified or modifies, and can make TiO2With amphipathic and fabulous dispersibility, and then partial size can be formed at 1~20 μm,
And the extremely stable Pickering miniemulsion with strong acid and alkali-resistance, high temperature resistant and electrolyte-resistant.
In order to solve the above technical problem, the present invention provides scheme be: a kind of system of amphipathic titanium dioxide emulsifier
Preparation Method, comprising the following steps:
S1, titanium salt presoma and small organic molecule are mixed in alcohol-water solution, forms titanium salt solution, and will be described
The pH of titanium salt solution is adjusted to 1.0-4.0, and the small organic molecule is the small organic molecule with hydrophobic grouping, the titanium
The concentration of small organic molecule described in salting liquid is 10-5~10-2mol/L；
By the titanium salt solution under the conditions of 25-160 DEG C, inhibitor is added and is hydrolyzed reaction, when the hydrolysis
Between be less than for 24 hours, obtain that there is amphipathic TiO2Nanoparticle sol；
By the TiO2Nanoparticle sol is dispersed in water to form dispersion liquid, and the alcohols removed in the dispersion liquid is molten
Agent, inhibitor and impurity obtain amphipathic titanium dioxide emulsifier.
Further, the titanium salt is alkoxy organic titanium or inorganic titanium salt；
The alkoxy organic titanium is tetraethyl titanate, butyl titanate, metatitanic acid orthocarbonate or tetraisopropyl titanate；
The inorganic titanium salt is titanium tetrachloride, titanium trichloride or sulfuric acid titanium salt.
Further, the inhibitor is hydrochloric acid, acetic acid, nitric acid or diethanol amine.
Further, alcohols is one of ethyl alcohol, propyl alcohol, isopropanol in the alcohol-water solution；The alcohol-is water-soluble
The volume of alcohol is 3~5 times of titanium salt presoma volume in liquid, the volume of water and the titanium salt presoma in the alcohol-water solution
Than being less than 4:1.
Further, the small organic molecule is C4~C22Fatty alcohol, C4~C22Fatty acid, C4~C22Rouge
Fat acylamino acid, alkyl quaternary ammonium salts, lecithin or vegetable protein.
A kind of Pickering emulsion preparation method, include the steps that it is above-mentioned prepare amphipathic titanium dioxide emulsifier, also wrap
Include following steps:
S2, the aqueous solution of the amphipathic titanium dioxide emulsifier is mixed with oiliness raw material, obtains dispersed phase, described point
Content of titanium dioxide is that 0.01-10wt% obtains Pickering lotion to the dispersed phase homogeneous in dephasing.Preferably, two
The pH of the aqueous solution of parent's property titanium dioxide emulsifier is maintained at 3~6, and content of titanium dioxide is 0.5~3wt%.
Further, the oiliness raw material is animal and plant fat, synthesizing ester, wax class, silicone oil or silicone oil derivative.
The application further provides a kind of amphipathic titanium dioxide emulsifier prepared according to the above method.
The application further provides a kind of Pickering lotion prepared according to the above method.
The application further provides a kind of application by above-mentioned Pickering lotion in cosmetics.
Beneficial effects of the present invention: (1) it can before emulsification pass through TiO2A small amount of organic matter is added in aqueous dispersions to be adsorbed on
Particle surface has carried out in-situ modification, and without cumbersome modification procedure, by adding suitable small organic molecule, a step can
To obtain the nano-TiO of infiltration sexual compatibility2Particle (oil-water interfaces contact angle is 70 °~110 °), and add the selection of organic matter
Face is wider.
(2) the Pickering lotion of invention preparation has different degrees of gelatination property, and can be used for preparing has not
With the emulsion of viscosity.
(3) lotion Dui Wen Du ﹑ time, pH value and ionic strength prepared by have extremely strong tolerance, stability of emulsion
It is splendid.
(4) miniemulsion obtained is alternatively arranged as the template of emulsion polymerization, to prepare the poly- of inorganic particle cladding
Object microballoon is closed, this kind of microballoon is also most common powder class raw material in cosmetics.
Detailed description of the invention
(a) is the Pickering lotion microphoto of embodiment 1 in Fig. 1, is (b) the Pickering lotion of embodiment 1
The contact angle of middle emulsion droplet；
(c1), (c2) are TiO in embodiment 1 in Fig. 22TEM figure, (c3) be embodiment 1 in TiO2Grain size distribution；
(d1) is that Pickering lotion is inverted in embodiment 1 in Fig. 3, Pickering emulsion emulsifiers in (d2) embodiment 1
The state of 1h, (d3) are 1 month states of Pickering emulsion emulsifiers in embodiment 1
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
It should be understood that the following title that the application occurs is the proprietary technology title of this field, this field skill
Art personnel can be beyond all doubt the meaning for checking title:
Pickering lotion: Pickering lotion refers to using ultrafine particle as emulsus obtained from emulsifier
Liquid.
TEM: transmission electron microscope.
Embodiment 1
S1,36mL ethyl alcohol is poured into the three-necked flask of 250mL 9mL butyl titanate is added dropwise, anhydrous acetic acid is added
PH value is adjusted to 1, and constantly uses 20~40min of magnetic stirrer, forms light yellow transparent solution；Under constant stirring will
1mL deionized water is added in solution with the speed of two seconds one drops and continues 30~40min of stirring after completion of dropwise addition, is obtained pale yellow
Color vitreosol.
Above-mentioned colloidal sol is moved into the hydrothermal reaction kettle of 150mL polytetrafluoroethyllining lining, and 0.03g behenic acid is added,
2 hours of 150 DEG C of reactions.
Product (white gels) are taken out after cooling and are centrifuged 10min with ethanol washing and at 15000r/min, abandon supernatant
(in triplicate).
Lower layer's white gels after collecting centrifugation are distributed in 200mL deionized water, with high speed disperser in 15000r/
Disperse 2min, ultrasonic 20min under min, then at 45 DEG C, rotation is evaporated to 100mL under 400r/min, adds 100mL deionization
Water continues to evaporate at 60 DEG C, and the mass fraction for being concentrated into titanium dioxide is greater than 3.0%, and ultrasonic 30min is obtained amphipathic
Titanium dioxide emulsifier.
S2, amphipathic titanium dioxide emulsifier is diluted with water, until TiO2Mass fraction be 0.5%, adjust pH value arrive
3, and ultrasound 2min.
It takes the above-mentioned solution of 6g as water phase, takes vinyl-terminated silicone oil 9g as oily phase, with high speed disperser in 20000r/
Emulsifying 2min under min obtains white oil-in-water ropy milk liquid, hardly flows after inversion.
As shown in Fig. 2 (c1) and (c2), by characterization, as shown in TEM, TiO in the present embodiment Pickering lotion2's
Average grain diameter is 7nm；As shown in Fig. 1 (a), the microphoto of lotion shows that the average grain diameter of emulsion droplet is 6 μm (1~20 μm)；It should
TiO2With appropriate hydrophilic and hydrophobic, as shown in Fig. 1 (b), the contact angle in vinyl-terminated silicone oil is 88 ± 3 °.
By the application prepare Pickering lotion respectively constant temperature 4 hours at 50 DEG C, 70 DEG C, 90 DEG C, as a result keep
Stable emulsion state, average grain diameter have the tendency that becoming larger (in the range of 2 μm) slightly；By the way that hydrochloric acid and sodium hydroxide tune is added
The pH value (1~12) of 12 groups of above-mentioned emulsions is saved, lotion is not demulsified；0~3% (based on the mass fraction for accounting for system) chlorine is added
Change sodium solution not to be demulsified, partial size increases 0~5 μm；There is no any lamination after room temperature one month, emulsion particle diameter changes not
To 1 μm, it is shown that the fabulous stability of the lotion.
Embodiment 2
S1,36mL isopropanol is poured into the three-necked flask of 250mL 9mL isopropyl titanate is added dropwise, hydrochloric acid tune is added
PH value is saved to 2, and constantly uses 20~40min of magnetic stirrer, forms light yellow transparent solution.
2mL deionized water is added in solution with the speed of two seconds one drops under constant stirring and is continued after completion of dropwise addition
30~40min is stirred, light yellow clear colloidal sol is obtained.
Above-mentioned colloidal sol is moved into the hydrothermal reaction kettle of 150mL polytetrafluoroethyllining lining, and 6 μ L butanol are added, in 160 DEG C
3 hours of reaction.
Product (white gels) are taken out after cooling and are centrifuged 10min with ethanol washing and at 15000r/min, abandon supernatant,
In triplicate.
Lower layer's white gels after collecting centrifugation are distributed in 200mL deionized water, with high speed disperser in 15000r/
Disperse 2min, ultrasonic 20min under min, then at 45 DEG C, rotation is evaporated to 100mL under 400r/min, adds 100mL deionization
Water continues to evaporate at 55 DEG C, and the mass fraction for being concentrated into titanium dioxide is greater than 3.0%, and ultrasonic 30min, what is obtained is amphipathic
Titanium dioxide emulsifier.
S2, amphipathic titanium dioxide emulsifier is diluted with water, until TiO2Content is 1.5wt%, adjusts pH value to 3, surpasses
Sound 2min.
It takes the above-mentioned solution of 10g as water phase, takes soybean oil 15g as oily phase, with high speed disperser at 10000r/min
Emulsifying 6min, obtains white Water-In-Oil ropy milk liquid, and inverting-flow is poor.
After tested, TiO in the Pickering lotion of embodiment preparation2Average grain diameter be 8nm；The micro- photograph of lotion
Piece shows that the average grain diameter of emulsion droplet is 9 μm (1~20 μm)；The TiO2Contact with appropriate hydrophilic and hydrophobic, in soybean oil
Angle is 109 ± 3 °；Respectively in the case where 90 DEG C of 50 DEG C ﹑, 70 DEG C ﹑ constant temperature 4 hours, stable emulsion state, average grain diameter are as a result kept
Have the tendency that becoming larger (in the range of 2 μm) slightly；The pH value (1 of 12 groups of above-mentioned emulsions is adjusted by the way that hydrochloric acid and sodium hydroxide is added
~12), lotion is not demulsified；Jia Ru≤3% (based on the mass fraction for accounting for system) sodium chloride solution is not demulsified, and partial size increases
1~5 μm；There is oil reservoir precipitation on upper layer after emulsification 5min, and oil reservoir height does not increase after room temperature one month, emulsion particle diameter variation
Less than 1 μm, it is shown that the fabulous stability of the lotion.
Embodiment 3
S1,6mL titanium tetrachloride is slowly added to constantly to use magnetic force in the 250mL three-necked flask for filling 100mL dehydrated alcohol
Blender stirs 30min, forms yellow to light yellow sol, 0.18g dodecyl trimethyl ammonium chloride is added, continues at 25 DEG C
Stirring for 24 hours, diethanol amine was slowly added to every 2 hours, and keeping pH value is 4, obtained nano titanium oxide dispersion；
100mL deionized water and ultrasound 20min are added into dispersion liquid, then at 45 DEG C, rotary evaporation under 400r/min
To 80mL, 100mL deionized water is added, continues evaporation removing solvent and by-product at 50 DEG C, is concentrated into the matter of titanium dioxide
Measuring score is the ultrasonic 30min greater than 3.0%, the aqueous solution of the titanium dioxide emulsifier obtained；
S2, titanium dioxide emulsifier are diluted with water, until TiO2Mass fraction be 3%, adjust pH value to 6, ultrasonic 2min,
It takes 8g as water phase, takes sheep oil 8g as oily phase, high speed disperser emulsifying at 20000r/min is used at 50 DEG C
20min obtains white Water-In-Oil creams.
TiO in the Pickering lotion prepared by characterization, the embodiment2Average grain diameter be 10nm；Lotion it is micro-
Photo shows that the average grain diameter of emulsion droplet is 13 μm (3~30 μm)；The TiO2With appropriate hydrophilic and hydrophobic, in atoleine (generation
For sheep oil) contact angle be 105 ± 3 °.
In Pickering lotion prepared by embodiment respectively constant temperature 4 hours at 50 DEG C, 70 DEG C, 90 DEG C, keep steady
Fixed emulsion state, average grain diameter have the tendency that becoming larger (in the range of 2 μm) slightly；It is adjusted by the way that hydrochloric acid and sodium hydroxide is added
The pH value (1~12) of 12 groups of above-mentioned creams is simultaneously stirred evenly at 8000r/min with homogenizer, and lotion is not demulsified；It is added 0
~3% (based on the mass fraction for accounting for system) sodium chloride solution is not demulsified, and partial size increases 0~2 μm；Do not have after room temperature one month
There is the phenomenon that any precipitation demulsification, emulsion particle diameter changes less than 1 μm, it is shown that the fabulous stability of the lotion.
Embodiment 4
S1,5mL titanium sulfate or titanyl sulfate are slowly added to fill in the 250mL three-necked flask of 100mL anhydrous propyl alcohol not
It is disconnected to use magnetic stirrer 30min, yellow is formed to light yellow sol, 0.25g lauroyl glutamate is added, then slowly
2~4mL diethanol amine is added, 60 DEG C of agings for 24 hours, form TiO 2 sol；
With the above-mentioned TiO 2 sol of the ultrafiltration membrance filter of 2nm, solvent and by-product are sloughed, is detected not until with barium ions
Sulfate ion into filtrate；
Titanium dioxide nano-particle after ultrafiltration is dispersed in middle addition 20mL deionized water and ultrasound 40min obtains dioxy
Change titanium emulsifier.
S2, titanium dioxide emulsifier is diluted with water, until TiO2Content be 1wt%, with salt acid for adjusting pH value to 4, surpass
Sound 2min.
It takes above-mentioned aqueous solution 9g as water phase, takes stearic acid 6g as oily phase, existed at 70 DEG C with high speed disperser
Emulsifying 10min under 20000r/min obtains oil-in-water white creams, does not flow after inversion.
TiO in the Pickering lotion prepared by characterization, the embodiment2Average grain diameter be 10nm；Emulsion droplet is averaged
Partial size is 15 μm (5~30 μm)；The TiO2Contact angle with appropriate hydrophilic and hydrophobic, in atoleine (instead of stearic acid)
It is 80 ± 3 °.
In Pickering lotion prepared by the embodiment respectively constant temperature 4 hours at 50 DEG C, 70 DEG C, 90 DEG C, as a result
Stable emulsion state is kept, average grain diameter has the tendency that becoming larger (in the range of 1 μm) slightly；By the way that hydrochloric acid and hydroxide is added
Sodium adjusts the pH value (1~12) of 12 groups of above-mentioned creams and is stirred evenly at 8000r/min with homogenizer, and lotion is without broken
Cream；0~3% (based on the mass fraction for accounting for system) sodium chloride solution is added not to be demulsified, partial size increases 1~5 μm；Room temperature one
There is no the phenomenon that any precipitation demulsification after a month, emulsion particle diameter changes less than 1 μm, it is shown that the fabulous stability of the lotion.
The application passes through TiO before emulsification2A small amount of small organic molecule is added in aqueous dispersions, keeps small organic molecule straight
It connects and is adsorbed on particle surface and has carried out in-situ modification, without cumbersome modification procedure, by adding suitable small organic molecule,
One step can be obtained by the nano-TiO of infiltration sexual compatibility2Particle, oil-water interfaces contact angle is 70 °~110 °, and is added organic
The selection face of object is wider, can according to emulsification when oily phase composition and adding proportion be in optimized selection.
Pickering lotion prepared by the application has different degrees of gelatination property, and can be used for preparing has not
With the emulsion of viscosity.
Pickering lotion prepared by the application has extremely strong tolerance to temperature, time, pH value and ionic strength
Property, stability of emulsion is splendid.
The application Pickering lotion obtained is alternatively arranged as the template of emulsion polymerization, to prepare inorganic particulate
The polymer microballoon of grain cladding, this kind of microballoon is also most common powder class raw material in cosmetics.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of preparation method of amphipathic titanium dioxide emulsifier, comprising the following steps:
S1, titanium salt presoma and small organic molecule are mixed in alcohol-water solution, forms titanium salt solution, and by the titanium salt
The pH of solution is adjusted to 1.0-4.0, and the small organic molecule is the small organic molecule containing hydrophobic grouping, and the titanium salt is molten
The concentration of small organic molecule described in liquid is 10-5~10-2mol/L；
By the titanium salt solution under the conditions of 25-160 DEG C, inhibitor is added, reaction is hydrolyzed, the hydrolysis time is small
In for 24 hours, obtaining that there is amphipathic TiO2Nanoparticle sol；
By the TiO2Nanoparticle sol is dispersed in water to form dispersion liquid, removes the alcohols solvent in the dispersion liquid, inhibits
Agent and impurity obtain amphipathic titanium dioxide emulsifier.
2. the preparation method of amphipathic titanium dioxide emulsifier as described in claim 1, which is characterized in that the titanium salt is alkane
Oxygroup organic titanium or inorganic titanium salt；
The alkoxy organic titanium is tetraethyl titanate, butyl titanate, metatitanic acid orthocarbonate or tetraisopropyl titanate；
The inorganic titanium salt is titanium tetrachloride, titanium trichloride or sulfuric acid titanium salt.
3. the preparation method of amphipathic titanium dioxide emulsifier as described in claim 1, which is characterized in that the inhibitor is
Hydrochloric acid, acetic acid, nitric acid or diethanol amine.
4. the preparation method of amphipathic titanium dioxide emulsifier as described in claim 1, which is characterized in that the alcohol-is water-soluble
Alcohols is one of ethyl alcohol, propyl alcohol, isopropanol in liquid；The volume of alcohol is the 3 of titanium salt presoma volume in the alcohol-water solution
~5 times, the volume ratio of water and the titanium salt presoma is less than 4:1 in the alcohol-water solution.
5. the preparation method of amphipathic titanium dioxide emulsifier as described in claim 1, which is characterized in that the small molecule has
Machine object is C4~C22Fatty alcohol, C4~C22Fatty acid, C4~C22Fatty acid acylamino acid, alkyl quaternary ammonium salts, lecithin
Or vegetable protein.
6. the amphipathic titanium dioxide emulsifier of any one of a kind of Pickering emulsion preparation method, including Claims 1 to 5
The step of, it is further comprising the steps of:
S2, the aqueous solution of the amphipathic titanium dioxide emulsifier is mixed with oiliness raw material, obtains dispersed phase, the dispersed phase
Middle content of titanium dioxide is that 0.01-10wt% obtains Pickering lotion to the dispersed phase homogeneous.
7. Pickering emulsion preparation method as claimed in claim 6, which is characterized in that the oiliness raw material is animals and plants
Grease, synthesizing ester, wax class, silicone oil or silicone oil derivative.
8. a kind of amphipathic titanium dioxide emulsifier of preparation according to claim 1~any one of 5.
9. a kind of Pickering lotion prepared according to any one of claim 6~7.
10. a kind of application according to the Pickering lotion of any one of claim 6~7 preparation in cosmetics.
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Denomination of invention: An Amphiphilic Titanium Dioxide Emulsifier, Pickering lotion and Its Preparation Method and Application Granted publication date: 20210803 Pledgee: Shandong Shanxian Rural Commercial Bank Co.,Ltd. Pledgor: Shandong Haidike Medical Products Co.,Ltd. Registration number: Y2024980009249 |