Preparation method of cyano-alkyl and aryl co-modified polysiloxane

A technology of cyanohydrocarbyl silane and polysiloxane, which is applied in the field of chemical additives, can solve the problems of single structure of silicone oil, low heat resistance, and inability to completely inhibit the bonding between fibers, so as to reduce surface defects and static electricity Cumulative, prevents the effect of hot-melt adhesion

Active Publication Date: 2016-02-24
GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the carbon fiber precursor treated with the oil agent made of heat-resistant resin alone has poor bundling properties and is not suitable for high-speed preparation of carbon fibers.
The emulsion prepared by mixing heat-resistant resin and silicone oil, due to the difference in compatibility between silicone oil and ester compounds, the emulsion cannot form a uniform and stable protective film on the surface of the carbon fiber precursor fiber, and cannot obtain stable carbon fiber
Polyol ester / polyether co-modified silicone oil is emulsified, because the compound with three ester groups is difficult to ensure the bundling of the precursor fiber in the pre-oxidation stage, and the polyol ester / polyether co-modified silicone oil Due to its low heat resistance, it cannot completely inhibit the inter-fiber bonding in the stages of pre-oxidation and low-temperature carbonization
[0011] Moreover, the structure of existing silicone oil agents is relatively simple, and it is rare to see silicone oil agents co-modified by two groups

Method used

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  • Preparation method of cyano-alkyl and aryl co-modified polysiloxane
  • Preparation method of cyano-alkyl and aryl co-modified polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Cyanoalkyl aryl co-modified polysiloxane B1 is prepared by the following steps: add 8.00 grams of cyanoethylsilane hydrolyzate obtained by hydrolyzing cyanoethylmethyldimethoxysilane into a reaction flask in a nitrogen atmosphere, 8.60 grams of phenylmethyldimethoxysilane, 79.40 grams of octamethylcyclotetrasiloxane, adding 0.01 grams of sodium hydroxide as a catalyst, and 4.00 grams of hexamethyldisiloxane as an end-capping agent, at 130 ° C The reaction was carried out under stirring condition, and the reaction time was 2 hours.

Embodiment 2

[0062] Cyanoalkyl aryl co-modified polysiloxane B2 is prepared by the following steps: add 8.00 grams of cyanoethylsilane hydrolyzate obtained by hydrolyzing cyanoethylmethyldimethoxysilane into a reaction flask in a nitrogen atmosphere, 8.60 grams of phenylmethyldimethoxysilane, 79.40 grams of octamethylcyclotetrasiloxane, adding 0.01 grams of sodium hydroxide as a catalyst, 0.30 grams of hexamethyldisiloxane as a capping agent, at 100 ° C The reaction was carried out under stirring condition, and the reaction time was 5 hours.

Embodiment 3

[0064] Cyanoalkyl aryl co-modified polysiloxane B3 is prepared by the following steps: add 4.80 grams of cyanoethylsilane hydrolyzate obtained by hydrolysis of cyanoethylmethyldimethoxysilane into a reaction flask in a nitrogen atmosphere, 5.16 grams of phenylmethyldimethoxysilane, 86.04 grams of octamethylcyclotetrasiloxane, add 0.01 grams of sodium hydroxide as a catalyst, and 4.00 grams of hexamethyldisiloxane as a capping agent, at 90 ° C The reaction was carried out under stirring condition, and the reaction time was 8 hours.

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Abstract

The invention provides a preparation method of cyano-alkyl and aryl co-modified polysiloxane. The method includes the following steps that cyano-alkyl silane is hydrolyzed, cyano-alkyl silane hydrolyzate is obtained, an alkali catalyst and an end-capping agent are added into the cyano-alkyl silane hydrolyzate, an aryl coupling agent and cyclosiloxane under protection of inert gas, and reaction is performed at 80-130 DEG C; the cyano-alkyl and aryl co-modified polysiloxane is prepared; the content of cyano-alkyl in the cyano-alkyl and aryl co-modified polysiloxane is 0.05-5 mmol/g, and the content of aryl in the cyano-alkyl and aryl co-modified polysiloxane is 0.1-3 mmol/g, and viscosity is 50-10,000 cST. The cyano-alkyl and aryl co-modified polysiloxane prepared through the method can serve as auxiliaries for producing high-performance carbon fibers. Particularly, the cyano-alkyl and aryl co-modified polysiloxane can serve as silicon oil agents for producing carbon fibers and can effectively moisten the surfaces of the fibers, reduce friction between the fibers and friction between the fibers and a guide roller, reduce surface defects and electrostatic accumulation caused by friction, and effectively prevent hot-melting adhesion of precursor fibers at the pre-oxidization stage and at the low-temperature carbonization stage.

Description

technical field [0001] The invention belongs to the field of chemical additives, and in particular relates to a preparation method of cyanocarbon-based and aryl-group co-modified polysiloxane, the cyanocarbon-based and aryl-group co-modified polysiloxane prepared by the method and applications thereof. Background technique [0002] Carbon fiber is a military-civilian industrial material with unique properties. It has better specific strength and specific modulus than metal and plastic. Composite materials produced with carbon fiber have been widely used in aerospace, aviation, sports equipment, and power blades. , pressure vessels, automobiles and other fields. In aerospace, cable and other fields, the requirements for the strength and modulus of carbon fibers are increasing day by day, and at the same time, the requirements for the stabilization of carbon fiber production are also getting higher and higher. [0003] Now the most common method for industrial production of c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26C08G77/06C08G77/08D06M15/643D06M101/40
CPCC08G77/06C08G77/08C08G77/26D06M15/643D06M2101/40
Inventor 黄振宏武振刚林汉国黄辛
Owner GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD
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