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A kind of polycarbosilane containing highly active crosslinkable group and its preparation method

A technology of polycarbosilane and cross-linking group, which is applied in the field of preparation of silicon carbide ceramic precursors, can solve the problems of residue, difficult to remove catalyst, long reaction time, etc. Effect

Active Publication Date: 2022-03-08
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the content of acryloyloxy group in the product is controllable, the reaction time is longer when there is no catalyst, and the catalyst is difficult to remove when the catalyst is included, and there are residues of monomers that have not participated in the reaction.

Method used

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  • A kind of polycarbosilane containing highly active crosslinkable group and its preparation method
  • A kind of polycarbosilane containing highly active crosslinkable group and its preparation method
  • A kind of polycarbosilane containing highly active crosslinkable group and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Referring to the literature (J.Eur.Ceram.Soc., 2017; 37(10):3263–3270), the synthetic structural unit is mainly -SiH 2 -CH 2 - Liquid polycarbosilane. In an ice-water bath, add 4.4g of liquid polycarbosilane and 60ml of dry dehydrated n-heptane into the flask, and then 2 and concentrated HCl quantitatively produced Cl 2 (0.01mol) passed through saturated brine, concentrated sulfuric acid, and anhydrous calcium chloride successively, and then passed into a flask to stir and react for 30 minutes.

[0049] (2) Under an ice-water bath, add hydroxyethyl acrylate (0.01 mol) and triethylamine (0.025 mol), stir and react for 10 minutes, then centrifuge at high speed to remove the ammonium salt. Then add 5ml of acetonitrile, stir and centrifuge, remove the acetonitrile solution with a separatory funnel, then add 5ml of acetonitrile, stir and centrifuge, then remove the acetonitrile solution with a separatory funnel, the obtained n-heptane solution is concentrated under re...

Embodiment 2

[0055] Under an ice-water bath, 4.4 g of the liquid polycarbosilane synthesized in Example 1, 60 ml of dehydrated n-heptane and thionyl chloride (0.01 mol) were added into the flask. After stirring and reacting for 20 minutes, hydroxyethyl acrylate (0.01 mol) and triethylamine (0.025 mol) were added in an ice-water bath, and after stirring and reacting for 10 minutes, the ammonium salt was removed by high-speed centrifugation. Then add 5ml of acetonitrile, stir and centrifuge, remove the acetonitrile solution with a separatory funnel, then add 5ml of acetonitrile, stir and centrifuge, then remove the acetonitrile solution with a separatory funnel, the obtained n-heptane solution is concentrated under reduced pressure at room temperature to obtain Based liquid polycarbosilane.

[0056] According to NMR, in the structure of the obtained liquid polycarbosilane containing acryloyloxy group, the molar content of structural units containing acryloyloxy group was 9%. Take 1 g of the...

Embodiment 3

[0058] Under an ice-water bath, 4.4 g of the liquid polycarbosilane synthesized in Example 1, 60 ml of dehydrated benzene and thionyl chloride (0.006 mol) were added into the flask. After stirring and reacting for 5 minutes, hydroxypropyl methacrylate (0.008 mol) and triethylamine (0.015 mol) were added under an ice-water bath, and after stirring and reacting for 5 minutes, the ammonium salt was removed by high-speed centrifugation. Benzene and unreacted triethylamine were distilled off under reduced pressure. Subsequently, add 80ml of cyclohexane and 5ml of acetonitrile, centrifuge after stirring, remove the acetonitrile solution with a separatory funnel, then add 5ml of acetonitrile, centrifuge after stirring, then remove the acetonitrile solution with a separatory funnel, and depressurize the obtained cyclohexane solution at room temperature Concentrate to obtain liquid polycarbosilane containing methacryloxy groups.

[0059] According to NMR, in the structure of the obtai...

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Abstract

The invention discloses a preparation method of polycarbosilane containing highly active crosslinkable groups, which comprises the following steps: mixing polycarbosilane, a halogenating agent and a solvent, and then carrying out a halogenation reaction to obtain partially halogenated polycarbosilane; The obtained polycarbosilane, the acid absorber and the compound containing the highly active crosslinkable group are mixed, stirred and reacted, and then separated and treated to obtain the polycarbosilane containing the highly active crosslinkable group. The invention also discloses the polycarbosilane containing highly active crosslinkable groups prepared by the above preparation method. The preparation method has low reaction temperature, short time and few side reactions, and high-purity products can be obtained through subsequent centrifugation, concentration and purification. The invention also regulates the amount of crosslinking groups introduced by controlling the degree of halogenation, thereby improving the heat curing or light curing rate of the prepared polycarbosilane, and enabling the product to have a higher ceramic yield.

Description

technical field [0001] The invention relates to the field of ceramics, in particular to a method for preparing a silicon carbide ceramic precursor. Background technique [0002] Silicon carbide (SiC) ceramics have excellent comprehensive properties such as high temperature resistance, wear resistance, corrosion resistance, radiation resistance, oxidation resistance, small thermal expansion rate and high thermal conductivity. The field has important application value, but because of its extremely high thermal stability and strength, SiC ceramics are difficult to form and process. Therefore, at present, the preparation of ceramic materials mainly adopts the traditional powder molding method, which needs to go through many processes such as micropowder preparation, molding, sintering, processing, etc., and there are high preparation temperatures, and it is difficult to obtain uniform chemical composition and microstructure. Finishing, high brittleness of ceramic products and o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C04B35/565
CPCC08G77/60C04B35/571C04B2235/483
Inventor 裴学良陈江善何流黄庆黄政仁柴之芳
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI