Poly(methylsilane-carbosilane) and preparation method thereof

A technology of methylsilane and carbosilane, which is applied in the field of polysilane and its preparation, can solve problems such as introduction obstacles, achieve the effects of improved safety, improved curing molding process, and high ceramic yield

Active Publication Date: 2013-07-24
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the past PMS and its modification process, in order to completely react the Si-Cl bond, an excessive amount of sodium metal was often used. The introduction of carbon-carbon unsaturated bonds brings certain obstacles

Method used

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  • Poly(methylsilane-carbosilane) and preparation method thereof
  • Poly(methylsilane-carbosilane) and preparation method thereof
  • Poly(methylsilane-carbosilane) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Install a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, and a gas guiding device on a dry 3L three-neck round bottom flask, and then vacuumize and replace with nitrogen three times. Under the protection of nitrogen, add 750ml of newly distilled xylene, 50ml of dioxane and 3.53mol (0.9 times of Si-Cl equivalent) Na cut into small pieces into the three-necked flask, and add formazan to the constant pressure dropping funnel. Dichlorosilane (1.825mol)-chloromethylmethyldichlorosilane (0.09175mol) monomer mixture. After the device is heated up to Na melting, adjust and stir to prepare sodium sand, add the monomer mixture dropwise (3-4 hours), after the dropwise addition is completed, continue to react at 115°C for 4 hours, stop stirring, cool naturally, and then transfer and filter to obtain Si-Cl polymer solution, distill off the solvent and add 500ml tetrahydrofuran for the next step of Grignard coupling reaction.

[0034] During the Grignar...

Embodiment 2

[0037] Install a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, and a gas guiding device on a dry 3L three-necked round bottom flask, and then vacuumize and replace nitrogen three times. Under nitrogen protection, add 750ml of freshly distilled xylene, 50ml of tetrahydrofuran and 4.0mol of Na cut into small pieces into a three-necked flask, and add methyldichlorosilane (1.825mol)-chloromethyl A mixture of methyldichlorosilane (0.1825mol) and freshly distilled xylene. After the device is heated up to Na melting, start stirring to prepare sodium sand, add monomer solution dropwise, and then react at 110-120°C for 5 hours to obtain an intermediate polymer containing Si-Cl bonds. After adding 200ml of dry tetrahydrofuran, add 440mL of 1.0mol / L ViMgBr tetrahydrofuran solution dropwise into the above reaction system, react at 60°C for 6 hours, stop stirring, and cool naturally. Then mix the hydrochloric acid-ice-water mixture of excess 100ml, 3mol / L hy...

Embodiment 3

[0039] Install a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, and a gas guiding device on a dry 2L three-necked round-bottomed flask, and then vacuumize and replace nitrogen three times, then add 300ml of newly distilled xylene-di Hexane mixed solution and 35.32g (1.53mol) of Na cut into small pieces, add methyldichlorosilane (0.73mol)-chloromethylmethyldichlorosilane (0.0365mol)- A mixture of chloromethyldimethylsilyl chloride (0.073mol) and freshly distilled xylene. Heat up the device, adjust the stirring until the Na melts, prepare sodium sand, add the monomer mixture dropwise, after the dropwise addition, keep the temperature at 100-120°C, react for 8 hours, stop stirring, cool naturally, then transfer and filter, inert Distilled under atmosphere, the resulting concentrated intermediate polymer was used in the Grignard reaction.

[0040] During the Grignard reaction, 1.0 mol / L ViMgBr THF solution (5%-15% excess) was added dropwise to the TH...

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Abstract

The invention discloses poly(methylsilane-carbosilane) and a preparation method thereof. The structural formula of the poly(methylsilane-carbosilane) copolymer is shown in formula I which is shown in the specification, wherein x=0-0.2, y=0.03-0.2, z=0-0.25, n=10-30, R1 represents Me, Ph or C2-C8 aromatic hydrocarbon or alkane, R2 represents Me or H, and Y represents a group containing C-C unsaturated bond. The preparation method of the poly(methylsilane-carbosilane) comprises the following steps of: in an organic solvent, carrying out a Wurtz type condensation polymerization reaction on a chlorosilane monomer mixture and insufficient alkali metal to synthesize Si-Cl bond-containing intermediate polymer; and then obtaining liquid methylsilane-carbosilane copolymer containing a C-C unsaturated bond through a grignard coupling reaction. The poly(methylsilane-carbosilane) disclosed by the invention can be served as a silicon carbide ceramic precursor, has the advantages of high ceramic yield, good storage stability and adjustability in structure composition, and can be applied to precursors of ceramic coatings and block body materials, and impregnants of composite materials.

Description

technical field [0001] The invention relates to a poly(methylsilane-carbosilane) and a preparation method thereof. Background technique [0002] The silicon carbide polymer ceramic precursor is the key raw material for the preparation of silicon carbide fibers, as the matrix resin for the preparation of silicon carbide-based composite materials by the PIP method, and for the preparation of silicon carbide-based high-temperature resistant bonding, connection, and composite ceramics. Among the many silicon carbide precursors researched and developed at home and abroad, the most mature technology and widely used is Kumada, which is produced by polydimethylsilane (PDMS) through high temperature cracking (about 470°C) invented by Yajima. Rearrangement of the resulting polycarbosilane (PCS). Among them, PDMS is obtained by reductive coupling polycondensation of dimethyldichlorosilane in xylene solvent by excessive molten metal sodium; while the cracking of PDMS requires high temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/24
Inventor 李永明王秀军徐彩虹曾凡
Owner INST OF CHEM CHINESE ACAD OF SCI
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