Preparation method of organic siloxane microspheres with narrow particle size distribution and richly organized surfaces

A technology for organizing siloxanes and siloxanes, which is applied in the field of preparation of surface-rich organosiloxane microspheres with narrow particle size distribution, and can solve the problems of simple post-treatment process, wide distribution, and harsh synthesis reaction conditions. The problem is to achieve the effect of less demanding reaction conditions, easy industrial production, and improved physical and chemical properties

Inactive Publication Date: 2014-04-23
韦兴祥 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the United States patent (US5801262), anionic surfactants, polymer stabilizers, hydroxide bases and hydration are combined by dispersion polymerization to form the first aqueous mixed solution, and silane monomers are added to form the second Mix the solution, then stir and react within a certain temperature range, and then obtain narrowly distributed polysiloxane microspheres through post-treatment processes such as suction filtration; in Japanese patent (JP2000186148), the silane monomer is first used under acidic conditions Polysiloxane microspheres were prepared by hydrolyzing and then polymerizing under alkaline conditions. This method is carried out in two steps, and the requirements for controlling the reaction conditions are relatively high, but the post-treatment process is simple; in the Chinese patent (CN101676023), the One or more mixtures of trialkoxysilanes are added to the mixed solution of water and alcohol, and then polymerized under alkaline conditions to prepare silicone microspheres. The obtained microspheres have a good spherical shape but a wide distribution
In the Chinese patent (CN102604100), deionized water and a basic catalyst are first added to the trialkoxysilane, stirred and hydrolyzed under nitrogen, and then centrifuged to remove unreacted monomers, and then a basic catalyst is added to the obtained product to carry out Polycondensation reaction, and then suction filtration, washing, and drying to obtain monodisperse micron-sized polyorganosilicon microspheres. At the same time, organic-inorganic hybrid material microspheres are synthesized by using siloxane monomers containing different alkyl groups. After this method The treatment process is simple, but the synthesis reaction conditions are harsh and the operation steps are cumbersome
However, in the preparation methods of the above various siloxane microspheres, only the preparation of the microspheres, the particle size distribution and other direct issues are involved, but little attention is paid to the non-polar organicization of the surface of the microspheres.

Method used

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  • Preparation method of organic siloxane microspheres with narrow particle size distribution and richly organized surfaces
  • Preparation method of organic siloxane microspheres with narrow particle size distribution and richly organized surfaces
  • Preparation method of organic siloxane microspheres with narrow particle size distribution and richly organized surfaces

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) In a reactor equipped with a stirrer and a thermometer, add 55 grams of deionized water, 0.54 grams of sodium dodecylbenzenesulfonate, and 0.045 grams of polyvinylpyrrolidone, and then at a constant temperature of 25 degrees Celsius, Stir at a speed of 350rpm for 20 minutes to obtain a dispersion;

[0031] (2) Add 18 grams of methyltrimethoxysilane into the reactor, stir at a constant temperature of 25 degrees Celsius for 30 minutes, then add 0.2 grams of ammonia solution with a mass fraction of 10%, and stir at a speed of 350 rpm for 2.5 Hour, obtain methylsiloxane microsphere mixed solution;

[0032] (3) After adjusting the pH value of the methylsiloxane microsphere mixture to 9.0, add 0.3 g of hexamethyldisiloxane to the reactor, and stir and react at 350 rpm for 3 hours to obtain surface-rich methylation Methylsiloxane microsphere dispersion;

[0033] (4) Use a centrifuge at 4000rpm for 15 minutes to obtain the product, wash it with deionized water, and then d...

Embodiment 2

[0035] The difference between this example and Example 1 is that in step (3), 0.5 g of dimethylvinylmethoxysilane is added to the reactor, and the reaction is stirred at 350 rpm for 3 hours to obtain the surface methyl-rich vinyl methoxysilane Silicone microsphere dispersion liquid; after step (4), 5.3 grams of surface-rich methyl vinylated methylsiloxane microspheres are obtained, with a particle size of 1 to 5 microns.

Embodiment 3

[0037] (1) In a reactor equipped with a stirrer and a thermometer, add 65 grams of deionized water, 0.47 grams of dodecylbenzenesulfonic acid sodium salt, and 0.048 grams of polyvinylpyrrolidone, and then at a constant temperature of 28 degrees Celsius, Stir at a speed of 350rpm for 25 minutes to obtain a dispersion;

[0038](2) Add 22 grams of methyltrimethoxysilane into the reactor, stir at a constant temperature of 24 degrees Celsius for 30 minutes, then add 0.25 grams of ammonia solution with a mass fraction of 10%, and stir at a speed of 350 rpm for reaction 3 Hour, obtain methylsiloxane microsphere mixed solution;

[0039] (3) After adjusting the pH value of the methylsiloxane microsphere mixture to 8.5, add 0.6 g of hexamethyldisilazane to the reactor, and stir and react at 350 rpm for 2.5 hours to obtain surface-rich methylation Methylsiloxane microsphere dispersion;

[0040] (4) Use a centrifuge at 4000rpm for 15 minutes to obtain the product, wash it with deionized...

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Abstract

The invention discloses a preparation method of organic siloxane microspheres with narrow particle size distribution and richly organized surfaces. The preparation method comprises the steps of (1) adding an anionic surfactant and a polymer stabilizer into deionized water, and mechanically stirring to prepare a dispersion liquid; (2) adding a siloxane monomer into the dispersion liquid, mechanically stirring for a certain period of time under a constant-temperature condition, and then adding a basic catalyst to initiate a reaction for a certain period of time to prepare a siloxane microsphere mixed liquid; (3) adjusting the pH value of the microsphere mixed liquid to a certain range, adding a silane monomer rich in organic groups, and stirring to react for a certain period of time to ensure that the silane monomer rich in organic groups is grafted to the siloxane microspheres through the reaction; and (4) centrifuging the reaction product to obtain a solid, and washing and drying to obtain the organic siloxane microspheres with narrow particle size distribution and richly organized surfaces. The preparation method disclosed by the invention is simple, is low in reaction condition requirement and low in preparation cost, and the prepared organic siloxane microspheres is narrow in particle size distribution and low in surface polarity.

Description

technical field [0001] The invention relates to the fine chemical industry field of organosilicon materials, in particular to a method for preparing organosiloxane microspheres with narrow particle size distribution surface and rich organosiloxane. Background technique [0002] Organosiloxane microspheres are semi-inorganic and semi-organic micron-sized spherical particles with silicon-oxygen bonds, silicon-carbon bonds, and carbon-hydrogen bonds. They have excellent high and low temperature resistance, weather resistance, wear resistance, hydrophobicity, and electrical Insulation properties, special optical properties, chemical inertness, physiological inertness, non-toxic, odorless and harmless, etc., which are widely used in the processing and modification of polymer materials such as plastics, rubber, coatings, etc., and can improve the heat resistance, cold resistance, and It can also be used in ink modification, cosmetic smoothness, bioengineering, chemical separation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/18C08G77/20C08G77/28C08G77/06C08G77/388
Inventor 韦兴祥欧阳昌伟
Owner 韦兴祥
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