A method for preparing silicone emulsion

Abstract

The invention discloses a method for preparing an organosilicon emulsion, and relates to the technical field of organosilicon materials, including: step one: obtaining a polysiloxane polymer, an organosilicon material and a metal catalyst; step two: mixing and reacting a polysiloxane polymer, a cross-linking agent, a surfactant, water and an emulsifier; step three: when the preparation process is ongoing, the polysiloxane is pre-mixed with a cross-linking agent, and a mixture of the polysiloxane polymer and the cross-linking agent, a surfactant, water and an emulsifier are added at a uniform speed; step four: stirring at a shear rate lower than 1000rpm, and when the viscosity range of the organosilicon colloid reaches 0.02-1000Pa·s and remains stable, an organosilicon emulsion is obtained. By controlling the composition ratio of the polysiloxane polymer, the surfactant, the cross-linking agent and the emulsifier, the lubricity and viscosity of the generated organosilicon emulsion can be controlled within a range that makes the body feel more comfortable.

Description

Technical Field

[0001] The invention relates to the technical field of organosilicon materials, and in particular to a method for preparing an organosilicon emulsion. Background Art

[0002] Silicone emulsion is one of the important silicone products, and its industrial application is extensive. For example, silicone emulsion is widely used in textile, papermaking, leather, cosmetics, medicine, construction, electronic and electrical fields. Among them, silicone emulsion plays a more important role in cosmetics. When cosmetics are used, their viscosity and lubricity play a more critical role in the user experience. However, the existing silicone emulsion is limited by the types and proportions of reactants, and there is room for optimization in its viscosity and lubricity. Summary of the invention

[0003] In order to solve the above technical problems, a method for preparing an organosilicon emulsion is provided. This technical solution solves the problems raised in the above background technology.

[0004] In order to achieve the above purpose, the technical solution adopted by the present invention is: A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 70-80% polysiloxane polymer, 1% crosslinking agent, 1%-14% surfactant, 0.5%-20% water and 0.1%-10% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0005] Preferably, the polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 20-30:14-22:30-50.

[0006] Preferably, the organosilicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 10-20:12-24:20-30.

[0007] Preferably, the metal catalyst is platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 2~10:4~14:3~15.

[0008] Preferably, the emulsifier is lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 1-7:2-8:3-6.

[0009] Preferably, the surfactant is an alkyl sulfonate.

[0010] Preferably, the cross-linking agent is dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 3-6:4-9.

[0011] Compared with the prior art, the present invention has the following beneficial effects: By controlling the composition ratio of polysiloxane polymer, surfactant, cross-linking agent and emulsifier, the lubricity and viscosity of the generated silicone emulsion can be controlled within a range that makes the body feel more comfortable, so that when used in cosmetics, the use experience of the cosmetics can be improved. At the same time, by controlling the composition ratio, the unnecessary products remaining in the reaction can be reduced. By setting a metal catalyst, the reaction speed can be further promoted and the preparation efficiency can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 It is a schematic flow chart of the preparation method of the organosilicon emulsion of the present invention. DETAILED DESCRIPTION

[0013] The following description is used to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments described below are only examples, and those skilled in the art may think of other obvious variations. Example

[0014] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 70% polysiloxane polymer, 1% cross-linking agent, 5% surfactant, 19% water and 5% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0015] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 20:14:30.

[0016] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 10:12:20.

[0017] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 2:4:3.

[0018] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 1:2:3.

[0019] The surfactant is an alkyl sulfonate.

[0020] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 3:4. Example

[0021] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 72% polysiloxane polymer, 1% cross-linking agent, 6% surfactant, 17% water and 4% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0022] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 22:16:32.

[0023] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 12:14:22.

[0024] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 3:5:4.

[0025] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 2:3:3.5.

[0026] The surfactant is an alkyl sulfonate.

[0027] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 3.5:4.5. Example

[0028] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 74% polysiloxane polymer, 1% cross-linking agent, 7% surfactant, 16% water and 2% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0029] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 24:18:34.

[0030] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 14:16:24.

[0031] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 4:6:5.

[0032] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 3:4:4.0.

[0033] The surfactant is an alkyl sulfonate.

[0034] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 4.0:5.0. Example

[0035] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 75% of polysiloxane polymer, 1% of cross-linking agent, 8% of surfactant, 15% of water and 1% of emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0036] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 26:20:36.

[0037] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 16:18:26.

[0038] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 5:7:6.

[0039] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 4:5:4.5.

[0040] The surfactant is an alkyl sulfonate.

[0041] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 4.5:5.5. Example

[0042] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 76% polysiloxane polymer, 1% cross-linking agent, 9% surfactant, 10% water and 4% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0043] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 28:22:38.

[0044] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 18:20:28.

[0045] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 6:8:7.

[0046] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 5:6:5.0.

[0047] The surfactant is an alkyl sulfonate.

[0048] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 5.0:6.0. Example

[0049] A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 77% polysiloxane polymer, 1% cross-linking agent, 10% surfactant, 7% water and 5% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0050] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 30:24:40.

[0051] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 20:22:30.

[0052] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 7:9:8.

[0053] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 6:7:5.5.

[0054] The surfactant is an alkyl sulfonate.

[0055] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 5.5:6.5.

[0056] Comparative Example 1: A method for preparing an organosilicon emulsion, comprising: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: 80% polysiloxane polymer, 1% cross-linking agent, 14% surfactant, 3% water and 2% emulsifier are mixed and reacted, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

[0057] The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 30:22:50.

[0058] The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 20:24:30.

[0059] The metal catalysts are platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 10:14:15.

[0060] The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 7:8:6.

[0061] The surfactant is an alkyl sulfonate.

[0062] The cross-linking agents are dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 6:9.

[0063] test: Experiment 1: Lubricity Test Obtaining a sample friction coefficient of a sample plate, where the sample plate is made of a material that does not react with the silicone emulsion; The surface of the sample plate is evenly coated with silicone emulsion with a thickness of 1 mm. The ambient temperature is maintained at 20 degrees Celsius. The friction coefficient of the sample plate after coating is obtained every one minute. The test is repeated 10 times, and the average value is taken as the target friction coefficient. The target friction coefficient is compared with the sample friction coefficient to obtain the friction coefficient change ratio; The friction coefficient is obtained as follows: The sample plate is fixed horizontally, and an object with a mass of 1 kg is placed on the surface of the sample plate. The maximum pulling force of the horizontally dragged object is obtained, and the maximum pulling force is divided by the weight of the object to obtain the friction coefficient. In general, silicone emulsion has a more obvious effect on the overall change of friction coefficient, and can adjust the lubrication degree to the range required by the body. Moreover, as the ratio changes, the friction coefficient can be fine-tuned within a smaller range. Therefore, the appropriate ratio can be selected for practical application based on the impact of the friction coefficient on the use effect.

[0064] Experiment 2: Viscosity Test Place the silicone emulsion at room temperature or 25°C for 2-3 hours; Open the lid of the silicone emulsion container and stir with a spatula for 1 to 2 minutes; Place the silicone emulsion container into a constant temperature bath; The rotation speed was adjusted between 2-20RPM, the temperature was set at 25°C, and after the rotation was completed, the viscosity of the silicone emulsion was measured; From this experiment, we can know that the prepared silicone emulsion has good viscosity. When used, it can improve its ability to adhere to the skin surface. Combined with its lubricity, it is easier to spread evenly on the skin surface when used. At the same time, due to its viscosity, it is not easy to evaporate and can lock moisture in the skin, thereby ensuring the effectiveness of cosmetics.

[0065] In summary, the advantages of the present invention are: by controlling the composition ratio of the polysiloxane polymer, surfactant, cross-linking agent and emulsifier, the lubricity and viscosity of the generated silicone emulsion can be controlled within a range that makes the body feel more comfortable, so that when used in cosmetics, the use experience of the cosmetics can be improved. At the same time, by controlling the composition ratio, the unnecessary products remaining in the reaction are reduced, and by setting a metal catalyst, the reaction speed can be further promoted and the preparation efficiency can be improved.

[0066] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions only describe the principles of the present invention. The present invention may be subject to various changes and improvements without departing from the spirit and scope of the present invention. These changes and improvements fall within the scope of the present invention. The scope of protection claimed by the present invention is defined by the attached claims and their equivalents.

Claims

1. A method for preparing an organosilicon emulsion, characterized in that: include: Step 1: obtaining a polysiloxane polymer, obtaining an organosilicon material capable of reacting with the polysiloxane polymer to extend the chain, and a metal catalyst for the chain extension reaction; Step 2: Mix 70-80% polysiloxane polymer, 1% crosslinking agent, 1%-14% surfactant, 0.5%-20% water and 0.1%-10% emulsifier for reaction, wherein the percentages are calculated by weight; Step 3: While the preparation process is ongoing, the polyorganosiloxane is premixed with the crosslinking agent, the mixture of the polysiloxane polymer and the crosslinking agent, the surfactant, water and the emulsifier are added at a uniform speed, the temperature is controlled at 60° C. to 80° C., and mixed with the surfactant and water to obtain an organic silica gel; Step 4: Stirring at a shear rate lower than 1000 rpm, when the viscosity of the organic silica gel reaches a range of 0.02-1000 Pa·s and remains stable, an organic silicone emulsion is obtained.

2. The method for preparing an organosilicon emulsion according to claim 1, characterized in that: The polysiloxane polymer is composed of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane, and the mass ratio of methyltrichlorosilane, dimethyldichlorosilane and phenyltrichlorosilane is 20-30:14-22:30-50.

3. The method for preparing an organosilicon emulsion according to claim 2, characterized in that: The organic silicon material is trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane, and the mass ratio of trimethylolpropane, triethoxysilane and dihydroxy polydimethylsiloxane is 10-20:12-24:20-30.

4. The method for preparing an organosilicon emulsion according to claim 3, characterized in that: The metal catalyst is platinum, palladium and rhodium, and the mass ratio of platinum, palladium and rhodium is 2-10:4-14:3-15.

5. The method for preparing an organosilicon emulsion according to claim 3, characterized in that: The emulsifiers are lecithin, vegetable gum and gelatin, and the mass ratio of lecithin, vegetable gum and gelatin is 1-7:2-8:3-6.

6. The method for preparing an organosilicon emulsion according to claim 4, characterized in that: The surfactant is an alkyl sulfonate.

7. The method for preparing an organosilicon emulsion according to claim 5, characterized in that: The cross-linking agent is dicumyl peroxide and benzoyl peroxide, and the mass ratio of dicumyl peroxide to benzoyl peroxide is 3-6:4-9.

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