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Preparation method for liquid hyperbranched polycarbosilane containing acryloyloxy group

An acryloxy, polycarbosilane technology, which is applied in the field of preparation of liquid hyperbranched polycarbosilane, can solve the problems of high content of unsaturated double bonds, difficult to control, and low yield of LHBPCS ceramicization, and achieves a simple preparation process. , The effect of improving the ceramic yield and shortening the reaction time

Active Publication Date: 2017-03-01
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

However, in this method, the content of unsaturated double bonds is high and difficult to control, so that the ceramization yield of LHBPCS substituted with unsaturated double bonds is low.

Method used

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  • Preparation method for liquid hyperbranched polycarbosilane containing acryloyloxy group
  • Preparation method for liquid hyperbranched polycarbosilane containing acryloyloxy group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Synthesis of LHBPCS: Add 500ml THF solvent, 40.84g magnesium powder and two iodine simple substances into the reaction kettle, then add 264.84g Cl 3 SiCH 2 Cl, where magnesium and Cl 3 SiCH 2 The molar ratio of Cl is 1.05:1. After the dropwise addition, react at 60°C for 12h; then add 41.37g lithium aluminum hydride for reduction at 60°C. After the reduction, add 68.54g, 4mol / L hydrochloric acid to quench the remaining Magnesium powder and lithium aluminum hydride, and finally filtered, pickled, washed with water, and vacuum distilled to obtain LHBPCS containing Si-H bonds.

[0025] Concrete reaction process is shown in the following formula:

[0026]

[0027] (2) Weigh 33g of LHBPCS prepared in step (1) (Si-H molar content is 1.5mol) and place it in a 2L four-necked flask consisting of a stirrer, a constant pressure dropping funnel, a reflux condenser, and a nitrogen pipe. In the middle; fill the reaction system with nitrogen through the nitrogen pipe, get r...

Embodiment 2

[0034] (1) Synthesis of LHBPCS: Add 500ml THF solvent, 40.84g magnesium powder and two iodine simple substances into the reaction kettle, then add 264.84g Cl 3 SiCH 2 Cl, where magnesium and Cl 3 SiCH 2 The molar ratio of Cl is 1.05:1. After the dropwise addition, react at 60°C for 12h, then add 41.37g lithium aluminum hydride for reduction for 12h, the temperature is 60°C, after the reduction, add 68.54g, 4mol / L hydrochloric acid to quench the remaining Magnesium powder and lithium aluminum hydride, and finally filtered, pickled, washed with water, and vacuum distilled to obtain LHBPCS containing Si-H bonds.

[0035] (2) Weigh 22g of LHBPCS prepared in step (1) (Si-H molar content is 1mol) and place it in a 2L four-necked flask consisting of a stirrer, a constant pressure dropping funnel, a reflux condenser, and a nitrogen pipe. , then add 300ml THF solution to the four-necked flask, fully stir and mix; fill the reaction system with nitrogen through the nitrogen tube, and ...

Embodiment 3

[0040] (1) Synthesis of LHBPCS: Add 500ml THF solvent, 40.84g magnesium powder and two iodine simple substances into the reaction kettle, then add 264.84g Cl 3 SiCH 2 Cl, where magnesium and Cl 3 SiCH 2 The molar ratio of Cl is 1.05:1. After the dropwise addition, react at 60°C for 12h, then add 41.37g lithium aluminum hydride for reduction for 12h, the temperature is 60°C, after the reduction, add 68.54g, 4mol / L hydrochloric acid to quench the remaining Magnesium powder and lithium aluminum hydride, and finally filtered, pickled, washed with water, and vacuum distilled to obtain LHBPCS containing Si-H bonds.

[0041] (2) Weigh 22g of LHBPCS prepared in step (1) (Si-H molar content is 1mol) and place it in a 2L four-necked flask consisting of a stirrer, a constant pressure dropping funnel, a reflux condenser, and a nitrogen pipe. , and then add 300ml THF solution to the four-necked flask, fully stir and mix; fill the reaction system with nitrogen through the nitrogen tube, ...

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Abstract

The invention provides a preparation method for liquid hyperbranched polycarbosilane containing an acryloyloxy group. The liquid hyperbranched polycarbosilane containing the acryloyloxy group is prepared from liquid hyperbranched polycarbosilane containing a Si-H bond and an acryloyloxy compound containing a hydroxyl or mercapto group through a reaction without a catalyst or under the catalysis of halide of metallic Zn, Al, B, Sn, Cr, Co or Pd, oxide of alkali metal, hydroxide of alkali metal or organic base. The preparation method is simple and the content of the acryloyloxy group in the product can be controlled, so the ceramic yield of the product is improved.

Description

technical field [0001] The invention relates to a preparation method of liquid hyperbranched polycarbosilane, in particular to a preparation method of liquid hyperbranched polycarbosilane containing acryloyloxy groups. Background technique [0002] Silicon carbide ceramics have the characteristics of superhardness, wear resistance, high strength, corrosion resistance, high temperature resistance, and oxidation resistance, and are widely used in key fields such as aerospace and military. Liquid hyperbranched polycarbosilane (LHBPCS) is an excellent SiC ceramic-based precursor due to its good fluidity, self-crosslinking, high ceramic yield, and pyrolysis products close to the stoichiometric ratio of SiC. [0003] There have been researches on photocuring 3D printing of LHBPCS and then sintering to prepare SiC ceramic devices (Eckel ZC, ZhouCY, Martin JH, Jacobsen AJ, Carter WB, Schaedler TA. Additive manufacturing of polymer-derived ceramics[J].Science, 2016, 351(6268):58-62)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/565
CPCC04B35/571C08G77/60
Inventor 季鹏何流裴学良黄庆
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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