A kind of preparation method of low volatile spherical silicone resin micropowder

A low-volatile, spherical silicon technology, applied in the field of polymer material preparation, can solve the problems of increased volatile content, inconvenient application, easy moisture absorption, etc., and achieves the effect of less energy consumption and concise process.

Active Publication Date: 2019-06-28
CHANGSHU CHANGJI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The ring-shaped silicone resin micropowders prepared by the preparation methods in the prior art, including the above-mentioned patents, all have the following disadvantages: because a certain amount of hydroxyl groups remain in the product (ie, spherical silicone resin micropowders), the volatile matter is relatively low. High (1-2%) or volatile content is not easy to reach a low level such as below 1%, and it is easy to absorb moisture and cause volatile content to increase, which brings inconvenience to application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 10.0kg of ordinary spherical silicone resin micropowder and 1.0kg of hexamethyldisilazane into a fully dry stainless steel rotary reactor, close the reactor, set the rotation speed at 8 rpm, and react at 50°C for 6 hours. Then cool the material to normal temperature, press filter with nitrogen, and after no filtrate flows out, the filter cake is rotary evaporated at 60°C / -0.093MPa for 2.5 hours to obtain the product of the present invention. .

Embodiment 2

[0022] In a fully dry stainless steel rotary reactor, put in 10.0kg of ordinary spherical silicone resin powder, 15.0kg of N, O-bis(trimethylsilyl)acetamide, close the reactor, set the speed at 12 rpm, and React at 50°C for 3 hours. Then cool the material to normal temperature, press filter with nitrogen, and after no filtrate flows out, the filter cake is rotary evaporated at 60°C / -0.095MPa for 3 hours to obtain the product of the present invention. .

Embodiment 3

[0024] In a fully dry stainless steel rotary reactor, put 10.0kg of ordinary spherical silicone resin powder and 30.0kg of tris(trimethylsilyl)phosphate, close the reactor, set the speed at 9 rpm, and react at 20°C for 1 Hour. Then the material was pressure filtered with nitrogen, and after no filtrate flowed out, the filter cake was rotary evaporated at 90°C / -0.095MPa for 3.5 hours to obtain the product of the present invention.

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PUM

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Abstract

The invention relates to a preparation method of low volatile component spherical silicon resin micro-powder and belongs to the technical field of high molecular material preparation. The preparation method comprises the following steps of: inputting spherical silicon resin micro-powder and a silanized raw material into a reaction container provided with a stirring device and a heating device to heat in the heating device and react in the stirring device in the stirring state, and controlling the reaction temperature and the reaction time; after the reaction, cooling the temperature to normal temperature and performing press filtering; and evaporating a filter cake obtained by press filtering at reduced pressure, and controlling the reduced pressure, the pressure-reducing temperature and the evaporating time to obtain the low volatile component spherical silicon resin micro-powder, wherein when the silanized raw material is cured at the normal temperature, a solvent is added into the reaction container and the filter cake after press filtering is washed by the solvent. The preparation method provided by the invention has the technical effects that as the process course is concise, industrial amplified production requirements can be met; and as the spherical silicon resin micro-powder reacts with the silanized raw material in the reaction container, the volatile components of the low volatile component spherical silicon resin micro-powder can be reduced to 0.52-0.78%, and the energy consumption is small.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to a method for preparing low-volatile spherical silicone resin micropowder. Background technique [0002] Inorganic-organic hybrid materials (referred to as hybrid materials) not only have the rigidity, dimensional stability and thermal stability of the inorganic phase, but also have the toughness and ease of processing of the organic phase, so in recent years, they have been widely used in physics, chemistry, materials and so on. Science, biomedicine and other fields have aroused great interest of scientific and technological workers. Among many hybrid materials, silicone resin micropowder has become a typical representative of inorganic-organic hybrid materials due to its excellent comprehensive performance and wide application value. [0003] Spherical silicone resin powder is a new type of silicone product newly developed in recent years. It is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/12C08L83/04
CPCC08J3/12C08J2383/04
Inventor 傅人俊曲大伟胡永明
Owner CHANGSHU CHANGJI CHEM
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