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

Inactive Publication Date: 2006-10-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the post-processing method is complicated, and the generated microspheres need to be filtered with a mesh sieve to ensure a narrow particle size distribution.
[0007] The main de

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The disclosed preparation method for polyalkylpolysiloxane microsphere comprises: hydrolyzing alkylpolysiloxane to produce alkylsilanol; adding surfactant and then ammonia, and polycondenzing for the product with wide size range (0.1-10 mum) and high yield (>94%).

Description

technical field [0001] The invention relates to a method for preparing polyalkylsiloxane microspheres, in particular to a new method for preparing polyalkylsiloxane microspheres with controllable particle size by using a surfactant. technical background [0002] Silicone resin microspheres are neither soluble in organic solvents nor melted, and their surface has excellent water drainage and lubricity. Compared with inorganic powders, the obtained spherical polysiloxane particles not only have a smaller specific gravity, but also have excellent durability. Thermal and excellent dispersibility and not easy to coalesce. Physical and chemical properties such as high hardness, high melting point, and wear resistance; physiological properties such as smoothness, non-toxic and tasteless, and optical properties such as transparency and gloss make it widely used in rubber and plastic industries, cosmetics, coatings, pigments, optical products, etc. . [0003] The reported particle ...

Claims

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Application Information

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IPC IPC(8): C08G77/06
Inventor 辛忠杨阳
Owner EAST CHINA UNIV OF SCI & TECH
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