Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Radiative reduction and curing method of liquid polycarbosilane

A polycarbosilane, liquid technology, applied in the field of polymers, can solve the problems of incomplete hydrogenation and reduction of liquid polycarbosilane, reduce the ceramicization rate of liquid polycarbosilane, and no methyl chloride reduction treatment, etc., to achieve easy industrialization Production, high reproducibility, avoidance of altered effects

Active Publication Date: 2019-08-02
HUBEI UNIV OF SCI & TECH
View PDF3 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods also deviate the silicon-carbon ratio of the cured polymer from 1:1, and introduce a certain amount of free carbon and SiO in the final ceramic product. 2 Such impurities seriously affect the performance of the product
[0005] (2) The hydrogenation reduction reaction of liquid polycarbosilane was not complete during the preparation process, and part of the methyl chloride could not be completely reduced
It can be seen that although the hydrogenation reduction of methyl chloride is not complete, it will not affect the composition of the final product, but it will also reduce the ceramicization rate of the liquid polycarbosilane prepared by the Grignard coupling method.
In the reported studies on the pyrolytic ceramicization of liquid polycarbosilane, no further reduction treatment of methyl chloride has been found, and an effective way to completely remove the methyl chloride contained in liquid polycarbosilane has not yet been found.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Radiative reduction and curing method of liquid polycarbosilane
  • Radiative reduction and curing method of liquid polycarbosilane
  • Radiative reduction and curing method of liquid polycarbosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] At room temperature, in a water-free and oxygen-free glove box with an argon atmosphere, pipette 3ml of liquid polycarbosilane into a petri dish with a diameter of 60mm. The liquid polycarbosilane used is prepared by Grignard coupling-hydrogenation reduction method , the molecular chain contains chloromethyl groups, and the molar ratio of chlorine atoms to carbon atoms is 0.06:1. After the petri dish filled with liquid polycarbosilane is packaged in a PE bag, it is irradiated with high-energy electron beams in the air, and the radiation dose rate is 30kGy / circle, the radiation dose is 240-600kGy. After irradiation, put the sample in a constant temperature box at -20-60°C and let it stand for 1-72 hours to obtain solid polycarbosilane with completely reduced methyl chloride.

[0032] attached figure 1 It is the H NMR spectrum of liquid polycarbosilane at different radiation doses, as shown in the attached figure 1 It can be seen that with the gradual increase of the ra...

Embodiment 2

[0036] At room temperature, in a water-free and oxygen-free glove box with an argon atmosphere, pipette 3ml of liquid polycarbosilane into a petri dish with a diameter of 60mm. The liquid polycarbosilane used is prepared by Grignard coupling-hydrogenation reduction method , the molecular chain contains chloromethyl groups, and the molar ratio of chlorine atoms to carbon atoms is 0.08:1. After the petri dish filled with liquid polycarbosilane is packaged in PE bags, high-energy electron beams are irradiated in the air, and the radiation dose rate is 30kGy / circle, the radiation dose is 180-360kGy. After irradiation, place the sample in a constant temperature box at -20-60°C and let it stand for 1-72 hours to obtain solid polycarbosilane in which methyl chloride has been incompletely reduced.

[0037] The polycarbosilane obtained after radiation curing is placed in a corundum crucible, and under the protection of argon, is calcined in a high-temperature tube furnace to 1100°C res...

Embodiment 3

[0039] At room temperature, in the air, use a pipette gun to pipette 3ml of liquid polycarbosilane into a petri dish with a diameter of 60mm. The liquid polycarbosilane used is prepared by Grignard coupling-hydrogenation reduction method. The molecular chain contains chloromethyl, and The molar ratio of chlorine to carbon is 0.03:1. After covering the petri dish filled with liquid polycarbosilane with PE plastic wrap, high-energy electron beams are used to irradiate in the air. The radiation dose rate is 30kGy / circle, and the radiation dose is 240-300kGy. After irradiation, put the sample in a thermostat at -20-60°C and let it stand for 1-72 hours to obtain a solid polycarbosilane in which methyl chloride is completely reduced and oxygen participates in curing.

[0040] The polycarbosilane obtained after radiation curing is placed in a corundum crucible, and under the protection of argon, is calcined in a high-temperature tube furnace to 1300°C respectively to obtain SiC powder...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a radiative reduction and curing method for liquid polycarbosilane, and belongs to the field of macromolecules and the field of inorganic non-metallic ceramics. An electron beamradiation technology is applied to reduction and curing of liquid polycarbosilane, liquid polycarbosilane containing chloromethyl groups is subjected to a radiation chemical reaction under radiationof electron beams, and cross-linking curing of liquid polycarbosilane is realized while chlorine atoms are reduced by hydrogen. The method can be directly applied to a liquid polycarbosilane dipping pyrolysis method for preparing a silicon carbide ceramic material, unsaturated bonds are not required to be introduced into liquid polycarbensilane molecular chains, or a cross-linking agent, a catalyst and an initiating agent are added to a liquid polycarbensilane precursor, curing of liquid polycarbensilane can be realized, so that not only is change of a silicon-carbon ratio of the polymer precursor in a curing process avoided, but also introduction of heteroatoms such as platinum, oxygen and nitrogen are avoided, and the method has the advantages of being simple to operate, easy to controland capable of realizing large-scale production and the like.

Description

technical field [0001] The invention belongs to the field of macromolecules and the technical field of inorganic non-metallic ceramics, and relates to a method for radiation reduction and solidification of liquid polycarbosilane. Background technique [0002] Silicon carbide (SiC) is an advanced ceramic material that has received widespread attention. It has the characteristics of high strength, low density, high temperature resistance, oxidation resistance, and good compatibility with metals. and other fields have broad application prospects. Among the SiC ceramic preparation methods that have been developed, the polymer impregnation pyrolysis method (PIP) is the most suitable method for the preparation of SiC films, SiC continuous fibers, SiC-based composites and bonded / sintered larger SiC due to the characteristics of polymers that are easy to shape and process. The most efficient method for monolithic artifacts. This method puts forward the following requirements for t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08J3/28C08J3/24C08L83/16C04B35/571C04B35/622
CPCC08J3/28C08J3/24C08G77/60C04B35/571C04B35/622C08J2383/16
Inventor 刘小玲朱晓明余积许云书曹余良谢聪王军涛舒婷胡鹏姬柳迪
Owner HUBEI UNIV OF SCI & TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products