Process for preparing polyalkyl silicone microsphere in the presence of interfacial agent
A technology of polyalkylsiloxane and alkylsiloxane, which is applied in the field of preparation of polyalkylsiloxane microspheres, can solve the problems of narrow range, wide particle size distribution, complex post-treatment methods, etc., and achieve enhanced resistance Abrasion, wide application, effect of changing slip
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Embodiment 1
[0024] Take 180ml of distilled water, measure its conductivity as 0.954μs / cm, and adjust its conductivity to 9.25μs / cm with dilute hydrochloric acid. Take 30ml of methyltrimethoxysilane and put it into a four-necked flask equipped with stirring, condenser and thermometer. At 25°C, slowly add the prepared distilled water into the flask, and heat up to 35°C for 5 hours of hydrolysis. Lower the temperature of the hydrolyzate to 18°C, add TW85 at a concentration of 1.28mmol / L (based on the volume of the hydrolyzate), stir to disperse it in the reaction system, then add 0.4% dilute ammonia water dropwise to the hydrolyzate, and quickly Stir until the pH value reaches 8.2, let stand at room temperature for 4 hours, pour off the upper aqueous solution, filter the product with suction, wash, and bake at 120°C for 12 hours to obtain 11.0 g of polyalkylsiloxane microspheres with a yield of 94.0%. Diameter 1.0 μm.
Embodiment 2
[0026] Take 180ml of distilled water, measure its conductivity as 0.808μs / cm, and adjust its conductivity to 9.25μs / cm with dilute hydrochloric acid. Take 30ml of methyltrimethoxysilane and put it into a four-necked flask equipped with stirring, condenser and thermometer. At 25°C, slowly add the prepared distilled water into the flask, and heat up to 35°C for 5 hours of hydrolysis. Lower the temperature of the hydrolyzate to 18°C, add OP13 at a concentration of 0.147mmol / L (calculated by the volume of the hydrolyzate), stir to disperse it in the reaction system, then add 0.4% dilute ammonia water dropwise to the hydrolyzate, and quickly Stir until the pH value reaches 8.2, let stand at room temperature for 4 hours, pour off the upper aqueous solution, filter the product with suction, wash, and dry at 120°C for 12 hours to obtain 11.5 g of polyalkylsiloxane microspheres with a yield of 97.8%. Diameter 8.0μm.
Embodiment 3
[0028] Take 180ml of distilled water, measure its conductivity as 0.861μs / cm, and adjust its conductivity to 9.25μs / cm with dilute hydrochloric acid. Take 30ml of methyltrimethoxysilane and put it into a four-necked flask equipped with stirring, condenser and thermometer. At 25°C, slowly add the prepared distilled water into the flask, and heat up to 35°C for 5 hours of hydrolysis. Lower the temperature of the hydrolyzate to 18°C, add sodium dodecyl sulfate (SDS) at a concentration of 3.960mmol / L (based on the volume of the hydrolyzate), stir to disperse it in the reaction system, and then drop it into the hydrolyzate Add 0.4% dilute ammonia water, stir rapidly until the pH value reaches 8.2, let stand at room temperature for 4 hours, pour off the upper aqueous solution, filter the product with suction, wash, and bake at 120°C for 12 hours to obtain polyalkylsiloxane microspheres 11.1 g, yield 94.8%, particle size 3.0 μm.
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