Polycarbosilane containing high-activity cross-linking groups and preparation method thereof

A technology of polycarbosilane and cross-linking groups, which is applied in the field of preparation of silicon carbide ceramic precursors, can solve the problems of long reaction time, residue, and difficult removal of catalysts, and achieve short reaction time, short time and few side reactions Effect

Active Publication Date: 2019-09-06
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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  • Polycarbosilane containing high-activity cross-linking groups and preparation method thereof
  • Polycarbosilane containing high-activity cross-linking groups and preparation method thereof
  • Polycarbosilane containing high-activity cross-linking groups and preparation method thereof

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 high-activity cross-linking groups. The method comprises the following steps that after polycarbosilane, halogenated reagentsand solvents are mixed, a halogenation reaction is performed, and partially-halogenated polycarbosilane is obtained; the obtained polycarbosilane, an acid absorbent and a compound containing high-activity cross-linking groups are mixed and then stirred, and the polycarbosilane containing high-activity cross-linking groups is obtained through separation. The invention further discloses the polycarbosilane containing high-activity cross-linking groups prepared through the preparation method. The preparation method is low in reaction temperature and short in time, and adopts few side reactions,and the product with high purity can be obtained through centrifuging, concentrating and purifying in the follow-up steps. The introducing amount of cross-linking groups can be controlled by controlling the halogenation degree, the thermosetting or photo setting speed of the obtained polycarbosilane is increased, and the product can have the high 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 Applications(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
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