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CN-119185080-B - Quaternized oil-control composite powder, preparation method thereof and application thereof in oil-control cosmetics

CN119185080BCN 119185080 BCN119185080 BCN 119185080BCN-119185080-B

Abstract

A quaternized oil-control composite powder, a preparation method thereof and application thereof in oil-control cosmetics. The present invention belongs to the field of cosmetics. The invention solves the problems that the oil-control cosmetic in the prior art adsorbs oily nutritional components in the cosmetic and the make-up holding time is short while adsorbing grease secreted by human bodies. The quaternized oil-control composite powder is obtained by modifying and compounding porous minerals. The quaternized oil-control composite powder prepared by the experiment has rough surface and mesoporous pores, can selectively adsorb unsaturated fatty acid to be fixed in the porous structure of the quaternized oil-control composite powder through the electrostatic interaction of the grafted quaternary ammonium salt and carboxylate radical on the porous mineral, and has the characteristic of rapid flocculation and solidification of grease, so that the makeup appearance is more durable. The quaternized oil-control composite powder also has the characteristics of hydrophobicity and hydrophilicity, and can be selected according to the requirements of different cosmetics when in use.

Inventors

  • BAI YUNGANG
  • XU KUN
  • WANG PIXIN
  • WANG YIXUAN
  • ZHANG FAN
  • DONG XIAOTONG

Assignees

  • 中国科学院长春应用化学研究所

Dates

Publication Date
20260512
Application Date
20241115

Claims (10)

  1. 1. The preparation method of the quaternized oil-control composite powder is characterized by comprising the following steps: S1, adding porous mineral, surfactant, dispersing agent and water into a reactor, uniformly stirring, adding metal salt, continuously stirring, then dripping ammonium bicarbonate aqueous solution, continuously reacting, washing and filtering twice, drying, and calcining in a muffle furnace to obtain modified mineral composite powder; s2, dispersing the modified mineral composite powder of S1 in toluene, adding a silane coupling agent and a polymerization inhibitor, filtering, washing, filtering and drying after the reaction is completed to obtain the modified mineral composite powder with double bonds; s3, under the protection of nitrogen, mixing the modified mineral composite powder with the double bond of S2, a polymerization monomer and toluene, uniformly stirring, adding an initiator for reaction, washing, filtering and drying after the reaction is completed to obtain polymer modified mineral composite powder; S4, mixing the S3 polymer modified mineral composite powder and toluene under the condition of stirring, dripping a halogenated hydrocarbon toluene solution, performing quaternization reaction, filtering, washing, drying, ball-milling at 30rpm to obtain quaternization oil-control composite powder; wherein the porous mineral is diatomite or zeolite, and the metal salt is zinc sulfate, aluminum sulfate, zinc nitrate, aluminum nitrate, zinc acetate or zinc chloride.
  2. 2. The method according to claim 1, wherein the surfactant of S1 is cetyltrimethylammonium bromide, sodium dodecyl benzene sulfonate or Tween, the dispersing agent is polyethylene glycol 200 or polyethylene glycol 400, the mass ratio of the surfactant of S1 to the porous mineral is 1-5:100, the mass ratio of the dispersing agent to the porous mineral is 1-5:100, the mass ratio of the metal salt to the porous mineral is 1:1-10, the molar ratio of ammonium bicarbonate to the metal salt is 1-8:1, the silane coupling agent of S2 is vinyltrimethoxysilane, vinyltriethoxysilane, vinyl-tris [ 2-methoxyethoxy ] silane or gamma-methacryloxypropyl trimethoxysilane, the polymerization inhibitor is catechol, the mass ratio of the modified mineral composite powder of S2 to the silane coupling agent is 5-20:1, the mass ratio of the polymerization inhibitor to the silane coupling agent is 1:50-200, the halogenated hydrocarbon of S4 is chlorooctadecane, chlorohexadecane, bromohexadecane or bromooctadecane, and the mass ratio of the modified mineral composite powder of S4 polymer to the halogenated hydrocarbon is 20:1-4.
  3. 3. The method of claim 2, wherein the diatomaceous earth has a silica content greater than 75%, a particle size of 5-50 μm, a porosity of 30-150m 2 /g, a zeolite particle size of 5-50 μm, and a porosity of 150-300m 2 /g.
  4. 4. The method according to claim 1, wherein the polymerized monomer of S3 is a mixture of divinyl polydimethylsiloxane, vinyl-terminated polyoxyethylene ether and dimethylaminoethyl methacrylate, the initiator is an azo initiator, the mass ratio of the modified mineral composite powder with double bonds of S3 to the polymerized monomer is 5-20:1, and the mass ratio of the initiator to the polymerized monomer is 1:10-50.
  5. 5. The method according to claim 4, wherein the azo initiator is azobisisobutyronitrile or azobisisoheptonitrile, and the mass ratio of the divinyl polydimethylsiloxane, the vinyl-terminated polyoxyethylene ether and the dimethylaminoethyl methacrylate is 0.1-2:0.1-5:1.
  6. 6. The method according to claim 1, wherein the S1 stirring time is 0.5-2h, the continuous reaction temperature is 50-80 ℃, the continuous reaction time is 5-10h, the drying temperature is 80-120 ℃, the drying time is 6-12h, the calcining temperature is 350-500 ℃, the calcining time is 2-6h, the S2 reaction temperature is 50-100 ℃, the reaction time is 4-8h, the drying temperature is 50-80 ℃, the drying time is 3-6h, the S3 stirring time is 0.1-2h, the reaction temperature is 50-80 ℃, the reaction time is 4-8h, the S4 reaction temperature is 80-100 ℃ and the reaction time is 4-8h.
  7. 7. The hydrophobic quaternized oil control composite powder prepared by the method of any one of claims 1 to 6, wherein the content of divinyl polydimethylsiloxane in the polymerized monomers is not less than 20wt.%.
  8. 8. Hydrophilic quaternized oil control composite powder prepared by the process according to any one of claims 1 to 6, characterized in that the content of divinyl polydimethylsiloxane in the polymerized monomers is <20wt.%.
  9. 9. The use of the hydrophobic quaternized oil control composite powder of claim 7 in oil-soluble cosmetics.
  10. 10. The use of the hydrophilic quaternized oil control composite powder according to claim 8 in water-soluble cosmetics.

Description

Quaternized oil-control composite powder, preparation method thereof and application thereof in oil-control cosmetics Technical Field The invention belongs to the field of cosmetics, and particularly relates to quaternized oil control composite powder, a preparation method thereof and application thereof in oil control cosmetics. Background The skin surface of the human body naturally secretes grease, and particularly in summer, excessive sebum can cause the makeup to drop off and affect the makeup effect, so that the cosmetic system needs the oil control function. The commonly used oil-controlling cosmetics are porous oil-controlling powder, such as porous silicon dioxide, porous polymethyl methacrylate and the like, but the porous oil-controlling powder has the defects, one of the reasons is that the porous oil-controlling powder has no selective adsorptivity and can absorb oily nutrient components in the cosmetics while absorbing skin secretion grease, and the other is that the porous oil-controlling powder cannot flocculate and solidify grease, which can lead to the maintenance of cosmetic effect for a long time. Therefore, the oil control powder which can directionally absorb unsaturated fatty acid (main grease component of human sweat) and has good make-up effect and no safety risk is developed, and the oil control powder has great significance for oil control cosmetics. Disclosure of Invention The invention aims to solve the problems that the oil-control cosmetic in the prior art adsorbs oily nutritional components in the cosmetic and the make-up holding time is short while adsorbing grease secreted by a human body. The invention provides quaternized oil-control composite powder, a preparation method thereof and application thereof in oil-control cosmetics. The technical scheme of the invention is as follows: the invention aims at providing a preparation method of quaternized oil control composite powder, which comprises the following steps: S1, adding porous mineral, surfactant, dispersing agent and water into a reactor, uniformly stirring, adding metal salt, continuously stirring, then dripping ammonium bicarbonate aqueous solution, continuously reacting, washing and filtering twice, drying, and calcining in a muffle furnace to obtain modified mineral composite powder; s2, dispersing the modified mineral composite powder of S1 in toluene, adding a silane coupling agent and a polymerization inhibitor, filtering, washing, filtering and drying after the reaction is completed to obtain the modified mineral composite powder with double bonds; s3, under the protection of nitrogen, mixing the modified mineral composite powder with the double bond of S2, a polymerization monomer and toluene, uniformly stirring, adding an initiator for reaction, washing, filtering and drying after the reaction is completed to obtain polymer modified mineral composite powder; And S4, mixing the S3 polymer modified mineral composite powder with toluene under the condition of stirring, dripping a halogenated hydrocarbon toluene solution, performing quaternization reaction, filtering, washing, drying, ball-milling at 30rpm to obtain the quaternization oil-control composite powder. Further limited, the porous mineral of S1 is diatomite or zeolite, the surfactant is cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate or Tween, the dispersing agent is polyethylene glycol 200 or polyethylene glycol 400, the metal salt is zinc sulfate, aluminum sulfate, zinc nitrate, aluminum nitrate, zinc acetate or zinc chloride, the mass ratio of the surfactant of S1 to the porous mineral is 1-5:100, the mass ratio of the dispersing agent to the porous mineral is 1-5:100, the mass ratio of the metal salt to the porous mineral is 1:1-10, the mole ratio of ammonium bicarbonate to the metal salt is 1-8:1, the silane coupling agent of S2 is vinyl trimethoxysilane, vinyl triethoxysilane, vinyl-tris (2-methoxyethoxy) silane or gamma- (methacryloyloxy) propyl trimethoxysilane, the polymerization inhibitor is catechol, the mass ratio of the modified mineral composite powder of S2 to the silane coupling agent is 5-20:1, the mass ratio of the polymerization inhibitor to the silane coupling agent is 1:50-200, the halogenated hydrocarbon of S4 is chlorooctadecane, chlorohexadecane, bromohexadecane or bromooctadecane, and the modified mineral composite powder of S4 is 20:4. Further defined, the diatomaceous earth has a silica content greater than 75%, a particle size of 5-50 μm, a porosity of 30-150m 2/g, a zeolite particle size of 5-50 μm, and a porosity of 150-300m 2/g. Further limited, the polymerized monomer of S3 is a mixture of divinyl polydimethylsiloxane, vinyl-terminated polyoxyethylene ether and dimethylaminoethyl methacrylate, the initiator is azo initiator, the mass ratio of the modified mineral composite powder with double bonds to the polymerized monomer of S3 is 5-20:1, and the mass ratio of the initiator to the polymerized monom