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Preparation method of monodispersity micron-sized polysilicon microspheres

A polyorganosilicon and monodispersity technology, which is applied in the field of monodisperse micron-scale polyorganosilicon microspheres and its preparation, can solve the problem that the particle size of the organosilicon microspheres is difficult to be monodispersed and the coverage rate of organic functional groups is low. , the post-processing is cumbersome and other problems, to achieve the effect of good particle size uniformity, fewer types of raw materials, and easy control of the reaction

Active Publication Date: 2012-07-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two methods are cumbersome, not only can not make the organic functional groups evenly covered on the silicon, but also the coverage is very low
Some of the above-mentioned preparation methods need to use emulsifiers, some need to use alcohol, the raw materials are more complicated, and the post-treatment is cumbersome. It is difficult to realize the monodispersity of particle size of silicone microspheres, and the coverage rate of organic functional groups on silicon is low and the distribution is uneven

Method used

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  • Preparation method of monodispersity micron-sized polysilicon microspheres
  • Preparation method of monodispersity micron-sized polysilicon microspheres
  • Preparation method of monodispersity micron-sized polysilicon microspheres

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Embodiment 1

[0028] (1) In a reactor equipped with a stirrer, a thermometer, a reflux condenser, and a nitrogen device, add 80ml of deionized water and 15ml of vinyltrimethoxysilane, and then add 0.008ml of a mass percent concentration of 28% ammonia solution, the reaction temperature is 30°C, the stirring speed is 300rpm, and the reaction time is 6h.

[0029] (2) Centrifuge the mixed system of step (1) on a centrifugal sedimentation machine to filter out unreacted monomers at a speed of 5000 rpm for 20 minutes.

[0030] (3) Add 0.5 ml of ammonia solution with a mass percent concentration of 28% to the reaction system obtained in step (2), the reaction temperature is 30° C., the stirring speed is 500 pm, and the time is 1 h. The resulting product was filtered, washed with water and ethanol, and dried at 100 °C for 15 h to obtain 7.6 g of monodisperse micron-sized silicone microspheres with an average particle size of 1.6 μm, such as figure 1 shown.

Embodiment 2

[0032] The difference between this embodiment and embodiment 1 is:

[0033] Step (1) dripping 0.03ml of the mass percentage concentration of 28% ammonia solution, the reaction time is 8h, step (3) adding 0.7ml of the mass percentage concentration of 28% ammonia solution, the reaction time is 4h, to obtain a monodisperse 7.4 g of micron-sized silicone microspheres, with an average particle size of 1.4 μm.

Embodiment 3

[0035] The difference between this embodiment and embodiment 1 is:

[0036] Step (1) Add 5ml of vinyltrimethoxysilane, the reaction temperature is 40°C, the speed of the mixed system in the step (2) is 4000rpm on the centrifugal sedimentation machine, the time is 15min, and the step (3) adds 0.3ml of mass percentage Aqueous ammonia solution with a concentration of 28% and a reaction time of 3 hours to obtain 2.5 g of monodisperse micron-sized silicone microspheres with an average particle size of 2 μm.

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Abstract

The invention discloses a preparation method of monodispersity micron-sized polysilicon microspheres which comprises the following steps: (1) adding deionized water and a basic catalyst in trialkoxysilane, and stirring in a nitrogen condition for hydrolysis; (2) centrifugally separating and filtering a mixed system in step (1) to remove unreacted monomers; and (3) adding the basic catalyst in a reaction system obtained from the step (2) for polycondensation, filtering, washing and drying to obtain the monodispersity micron-sized polysilicon microspheres. According to the method, the reaction temperature is low, the reaction can be conducted at room temperature, the synthesis steps are simple; the method does not use organic solvents which pollute the environment or emulsifiers in the reaction process, is simple in post treatment, less in types of raw materials, high in yield, and low in preparation cost, and can effectively adjust the grain size range of the microspheres to realize controllable sizes; and the obtained silicon microspheres are good in grain size uniformity and high in monodispersity, and has extremely good sphericity.

Description

technical field [0001] The invention relates to a monodisperse micron-order organosilicon microsphere, in particular to a size-controllable monodisperse micron-order polyorganosilicon microsphere and a preparation method thereof. Background technique [0002] Polyorganosiloxane microspheres have excellent physical and chemical properties such as high and low temperature resistance, weather resistance, flame retardancy, abrasion resistance, hydrophobicity, electrical insulation, and physiological inertia. , coatings, cosmetics, light diffusion light guide plates and other fields, thereby improving heat resistance, flame retardancy, oxidation resistance, scratch resistance, light diffusion, etc. [0003] In the preparation of monodisperse micron-sized silicone microspheres, some people have done research. Mary et al. (US5801262) obtained the first batch of emulsions by mixing anionic surfactants, stabilizers, alkaline hydroxide aqueous solution, water, etc. together by emulsi...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/20C08G77/28
Inventor 马文石张冬桥段宇
Owner SOUTH CHINA UNIV OF TECH
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