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CN-122005365-A - Self-emulsifying amino silicone oil emulsion and preparation method thereof

CN122005365ACN 122005365 ACN122005365 ACN 122005365ACN-122005365-A

Abstract

The invention relates to the technical field of washing and caring products, in particular to self-emulsifying amino silicone oil emulsion and a preparation method thereof. The anti-corrosion agent comprises the following raw materials of amino modified silicone oil, PEG-7 glycerol cocoate, polyether block copolymer, organic acid, preservative and deionized water, wherein the mass ratio of the amino modified silicone oil to the PEG-7 glycerol cocoate is 2-9:1. According to the invention, through the molecular collaborative design of the amino modified silicone oil and the PEG-7 glycerol cocoate and the combination of gradient polymerization and self-assembly regulation technology, the whole process optimization from the molecular structure design to the precise control of the particle size of the emulsion is realized, the stability, the self-emulsifying efficiency and the conditioning performance of the emulsion are obviously improved, and the self-emulsifying amino silicone oil emulsion meeting the requirements of mild care and green consumption is prepared.

Inventors

  • TANG YONG
  • HU YAN
  • XIAO JUN

Assignees

  • 广东万翔宝诚实业有限公司

Dates

Publication Date
20260512
Application Date
20260415

Claims (8)

  1. 1. The preparation method of the self-emulsifying amino silicone oil emulsion is characterized by comprising the following steps of: Step S1, firstly weighing 20-40% of amino modified silicone oil, 5-20% of PEG-7 glycerol cocoate, 5-15% of polyether block copolymer, 0.1-0.5% of organic acid, 0.3-0.8% of preservative and the balance of deionized water according to the mass ratio; The amino modified silicone oil is polysiloxane with a ternary copolymer block structure, and is prepared from the following raw materials in percentage by mass through polymerization reaction: 5-15% of gamma-piperazinyl propyl methyl dimethoxy silane, 1-3% of hexamethyldisiloxane, 0.5-1% of alkaline catalyst and the balance of octamethyl cyclotetrasiloxane; The PEG-7 glycerol cocoate is prepared from the following raw materials in percentage by mass through esterification reaction: 30-40% of coconut oil acid, 0.3-0.8% of composite catalyst and the balance of glycerol polyoxyethylene ether-7; S2, mixing amino modified silicone oil with PEG-7 glycerol cocoate, adding polyether block copolymer and deionized water, and stirring to form a self-emulsifying pre-dispersion; s3, adding organic acid into the self-emulsifying pre-dispersion to adjust the pH to 6.0-7.0, and transferring the system to a homogenizer to refine the emulsion particle size to below 150 nm; And S4, transferring the homogenized emulsion to a stirring kettle, stirring at room temperature for 2-4 hours for stabilization treatment, finally adding a preservative, uniformly mixing, and filtering and discharging to obtain the self-emulsifying amino silicone oil emulsion.
  2. 2. The method for preparing the self-emulsifying amino silicone oil emulsion according to claim 1, wherein in the step S1, octamethyl cyclotetrasiloxane, gamma-piperazinyl propyl methyl dimethoxy silane, hexamethyldisiloxane and an alkaline catalyst are put into a reaction kettle, and are heated to 80-90 ℃ under the protection of nitrogen, and are reacted for 1-2 hours for ring-opening polymerization; And finally, heating to 130-140 ℃ under the condition that the vacuum degree is less than or equal to minus 0.095 MPa, removing low molecular substances for 1h, cooling and discharging to obtain the amino modified silicone oil.
  3. 3. The method for preparing the self-emulsifying amino silicone oil emulsion according to claim 1, wherein in the step S1, glycerol polyoxyethylene ether-7 and cocoanut acid are put into a reaction kettle, and a composite catalyst and an azeotropic solvent are added; Heating to 165-175 ℃, and carrying out azeotropic dehydration reaction for 4-6 hours until the theoretical water yield reaches more than 95%; After the reaction is finished, heating to 120-130 ℃ under the vacuum degree of less than or equal to minus 0.095 MPa, and recovering the azeotropic solvent by reduced pressure distillation; Cooling to 80-90deg.C, adding neutralizer to adjust pH to 6.0-7.0, adding activated clay or activated carbon, stirring for adsorption for 30min, and filtering to obtain PEG-7 glycerol cocoate.
  4. 4. The method for preparing the self-emulsifying amino silicone oil emulsion according to claim 3, wherein the composite catalyst is prepared by compounding p-toluenesulfonic acid and phosphorous acid according to a mass ratio of 2:1.
  5. 5. The method for preparing a self-emulsifying amino silicone oil emulsion according to claim 1, wherein in the step S2, amino modified silicone oil and PEG-7 glycerol cocoate are mixed according to a mass ratio of 2-9:1.
  6. 6. The method for preparing a self-emulsifying aminosilicone emulsion as defined in claim 1, wherein in step S2, the self-emulsifying pre-dispersion is formed by stirring at 40-60 ℃ for 30-60 minutes.
  7. 7. The method for preparing a self-emulsifying aminosilicone emulsion as defined in claim 1 wherein in step S3, the system is homogenized in a homogenizer at 5000-8000rpm for 10-20 minutes.
  8. 8. The self-emulsifying amino silicone oil emulsion prepared by the preparation method according to any one of claims 1 to 7, which is characterized by comprising the following raw materials: amino modified silicone oil, PEG-7 glycerol cocoate, polyether block copolymer, organic acid, preservative and deionized water.

Description

Self-emulsifying amino silicone oil emulsion and preparation method thereof Technical Field The invention relates to the technical field of washing and caring products, in particular to self-emulsifying amino silicone oil emulsion and a preparation method thereof. Background In the fields of personal care and household cleaning, amino silicone oil emulsion is a common core conditioning raw material, and can improve the softness and smooth feel of the washing and caring articles. Although the self-emulsifying technology can simplify the preparation process, the prior art still has obvious defects: Firstly, the traditional bulk emulsification method needs to synthesize crude silicon oil firstly, then the crude silicon oil is mixed with a large amount of emulsifying agents through high-energy consumption equipment, the process flow is long, the production efficiency is low, and the particle size among batches is unstable. Secondly, to maintain emulsion stability, more emulsifier must be used, which not only increases cost, but may also cause irritation to skin and environment, and it is difficult to meet the market demand for mild, green products. Moreover, the existing emulsion is low in solid content generally, high-concentration design of more than 30% is difficult to realize, so that the transportation cost is high, the formula is limited, meanwhile, the storage stability is poor, and the problems of layering, drifting and the like are easy to occur. In summary, the existing amino silicone oil emulsion has obvious defects in the aspects of preparation efficiency, emulsifier dosage, product stability and the like. Disclosure of Invention The invention aims to solve the comprehensive defects of the existing amino silicone oil emulsion in the aspects of preparation efficiency, emulsifier dosage and stability, and realize efficient and stable synergy unification. The invention aims to provide a self-emulsifying amino silicone oil emulsion and a preparation method thereof, wherein the molecular synergistic design of amino modified silicone oil and PEG-7 glycerol cocoate is combined with gradient polymerization and self-assembly regulation and control technology, so that the whole process optimization from molecular structure design to precise control of emulsion particle size is realized, and the stability, self-emulsifying efficiency and conditioning performance of the emulsion are obviously improved. In order to achieve the above purpose, one of the purposes of the invention is to provide a self-emulsifying amino silicone oil emulsion which comprises the following raw materials in percentage by mass: 20-40% of amino modified silicone oil, 5-20% of PEG-7 glycerol cocoate, 5-15% of polyether block copolymer, 0.1-0.5% of organic acid, 0.3-0.8% of preservative and the balance of deionized water; wherein the mass ratio of the amino modified silicone oil to the PEG-7 glycerol cocoate is 2-9:1; The amino modified silicone oil is polysiloxane with a ternary copolymer block structure, and is prepared by polymerization of the following raw materials in percentage by mass: 5-15% of gamma-piperazinyl propyl methyl dimethoxy silane, 1-3% of hexamethyldisiloxane, 0.5-1% of alkaline catalyst and the balance of octamethyl cyclotetrasiloxane; The PEG-7 glycerol cocoate is prepared from the following raw materials in percentage by mass through esterification reaction: 30-40% of coconut oil acid, 0.3-0.8% of composite catalyst and the balance of glycerol polyoxyethylene ether-7; Wherein the composite catalyst is prepared by compounding p-toluenesulfonic acid and phosphorous acid according to a mass ratio of 2:1. The second object of the present invention is to provide a method for preparing the self-emulsifying amino silicone oil emulsion, comprising the following steps: Step S1, firstly, weighing raw materials according to the mass ratio; S2, mixing amino modified silicone oil with PEG-7 glycerol cocoate, adding polyether block copolymer and deionized water, and stirring to form a self-emulsifying pre-dispersion; s3, adding organic acid into the self-emulsifying pre-dispersion to adjust the pH to 6.0-7.0, and transferring the system to a homogenizer to refine the emulsion particle size to below 150 nm; And S4, transferring the homogenized emulsion to a stirring kettle, stirring at room temperature for 2-4 hours for stabilization treatment, finally adding a preservative, uniformly mixing, and filtering and discharging to obtain the self-emulsifying amino silicone oil emulsion. As a further improvement of the technical scheme, in the step S1, octamethyl cyclotetrasiloxane, gamma-piperazinyl propyl methyl dimethoxy silane, hexamethyldisiloxane and an alkaline catalyst are put into a reaction kettle, and are heated to 80-90 ℃ under the protection of nitrogen, and are reacted for 1-2 hours for ring-opening polymerization; And finally, heating to 130-140 ℃ under the condition that the vacuum degree is less than or equal to minus 0.0