Method capable of realizing volume production and used for preparing micron order single-dispersibility polysiloxane microspheres

A technology of polyorganosiloxane and monodispersity, which is applied in the field of preparing micron-sized monodisperse polyorganosiloxane microspheres that are easy to mass-produce, and can solve the problem that is not conducive to mass production of micron-sized polyorganosiloxane microspheres. Problems such as complex selection and design of balls and equipment, harsh reaction conditions, etc., to achieve the effect of truly controllable particle size, mass production, and less harsh reaction conditions

Active Publication Date: 2016-09-21
贵州正业龙腾新材料开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions required by the above method are harsh, the steps are cumbersome, and the equipment selection and design are complicated, which is not conducive to the implementation of mass production of micron-sized polyorganosiloxane microspheres.

Method used

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  • Method capable of realizing volume production and used for preparing micron order single-dispersibility polysiloxane microspheres
  • Method capable of realizing volume production and used for preparing micron order single-dispersibility polysiloxane microspheres
  • Method capable of realizing volume production and used for preparing micron order single-dispersibility polysiloxane microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Step ①, add 400g of deionized water and 2g of KOH solid powder into the reactor equipped with a stirrer, the temperature is 15°C at room temperature, the stirring speed is 250rpm, the time is 15min, and the pH value is 10.65.

[0033] In step ②, add 8.8 g of methyltrimethoxysilane monomer solution to the basic catalyst solution in step ① to prepare a seed solution, the temperature is 15° C. at room temperature, the stirring speed is 300 rpm, and the time is 20 min.

[0034] In step ③, add 56g of methyltrimethoxysilane monomer solution to the seed solution obtained in step ② to carry out polycondensation reaction. The temperature is 15°C at room temperature, the stirring speed is 250rpm, and the time is 30min. The obtained product is filtered and washed with deionized water , and dried at 150°C for 8h to obtain 29.45g of micron-sized monodisperse organosiloxane microspheres with an average particle size of 2.15μm, such as figure 2 shown.

Embodiment 2

[0036] The difference between this embodiment and embodiment 1 is:

[0037] Step ② Add 6 g of methyltrimethoxysilane monomer solution to prepare a seed solution. The temperature is 21° C. at room temperature, the stirring speed is 350 rpm, and the time is 20 minutes.

[0038] Step ③Add 75g of methyltrimethoxysilane monomer solution to carry out polycondensation reaction. The temperature is 21°C at room temperature, the stirring speed is 300rpm, and the time is 30min. The obtained product is filtered, washed with deionized water, and dried at 150°C for 8h to obtain micron single Dispersion grade silicone microspheres 36.8g, average particle size 2.5μm, such as image 3 shown.

Embodiment 3

[0040] Step ①, add 380g of deionized water and 4g of NaOH solid powder into the reactor equipped with a stirrer, the temperature is 22°C at room temperature, the stirring speed is 380rpm, the time is 18min, and the pH value is 12.55.

[0041] In step ②, add 9.4 g of phenyltrimethoxysilane monomer solution to the basic catalyst solution in step ① to prepare a seed solution. The temperature is 22° C. at room temperature, the stirring speed is 350 rpm, and the time is 25 minutes.

[0042] In step ③, add 48g of phenyltrimethoxysilane monomer solution to the seed solution obtained in step ② for polycondensation reaction. The temperature is 22°C at room temperature, the stirring speed is 300rpm, and the time is 40min. The obtained product is filtered and washed with deionized water , dried at 180°C for 6h to obtain 36.2g of micron-sized monodisperse organosiloxane microspheres with an average particle size of 1.67μm, as Figure 5 shown.

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Abstract

The invention discloses a method capable of realizing volume production and used for preparing micron order single-dispersibility polysiloxane microspheres. The method comprises the following steps of (1) preparing a basic catalyst solution; (2) adding trialkoxysilane monomers into the basic catalyst solution (1) to prepare a seed solution; (3) then adding trialkoxysilane monomers into the seed solution obtained in the step (2) to perform a polycondensation reaction; performing filtering, washing and drying to obtain a finished product. The operation can be performed under the conditions of normal temperature, normal pressure and no atmosphere protection; the synthesis steps are simple; the operation is easy; synthesis equipment does not have special requirements; the volume production can be easily realized. No organic solvents polluting the environment are used in the reaction process; no dispersing agents, swellers, stabilizing agents, emulgators or the like are used; the types of reaction polymerization raw materials are few; the product purity is high; the yield is high; the cost is low; the size of the particle diameter of the microspheres can be effectively regulated through controlling the concentration of an initial seed solution; the distribution of the particle diameter of the obtained microspheres is uniform; the high-degree monodispersity is shown; the surface is regular; the degree of sphericity is high.

Description

technical field [0001] The invention relates to a method for preparing micron-scale monodisperse polyorganosiloxane microspheres that are easy to mass-produce, in particular to a micron-scale monodisperse polyorganosiloxane microsphere with controllable particle size, high purity, and easy mass production. Siloxane microspheres and methods for their preparation. Background technique [0002] Polyorganosiloxane microspheres are semi-organic and semi-inorganic polyorganosilsesquioxane hollow spherical microspheres with a three-dimensional cross-linked molecular structure and insoluble and infusible properties. Therefore, polyorganosiloxane microspheres have excellent heat resistance, optical properties, and dispersion properties. They are used as light-diffusing additives in transparent plastic materials such as PC, PMMA, and PS, thereby endowing the base material with high haze and high light transmittance. It has excellent light diffusion characteristics and has been widely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/20C08G77/18B01J13/14
CPCB01J13/14C08G77/06C08G77/18C08G77/20
Inventor 沈志平袁江文欧阳昌伟王翔代礼彬杨军高跃生聂矗夏锐倪凯凯梁烛秦欣
Owner 贵州正业龙腾新材料开发有限公司
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