Preparation method of cationic amino modified epoxy silicone oil and compounding and application of polyacrylonitrile carbon fiber precursor oil agent

A technology of epoxy silicone oil and amino modification, which is applied in fiber type, fiber treatment, textile and paper making, etc., and can solve the problems of good storage stability of emulsion

Active Publication Date: 2019-08-13
吉林乾仁新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the difficulty of implementing existing patents and the technical problems in the production process of polyacrylonitrile carbon fiber precursors, the present invention researches and develops self-assembling and self-emulsifying cationic amino-modified epoxy silicone oil. On the one hand, no emulsifier is needed, and the size of the emulsion can be adjusted. On the other hand, modified silicone oil emulsion has good storage stability

Method used

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  • Preparation method of cationic amino modified epoxy silicone oil and compounding and application of polyacrylonitrile carbon fiber precursor oil agent
  • Preparation method of cationic amino modified epoxy silicone oil and compounding and application of polyacrylonitrile carbon fiber precursor oil agent
  • Preparation method of cationic amino modified epoxy silicone oil and compounding and application of polyacrylonitrile carbon fiber precursor oil agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Use 50g of N-methylpyrrolidone (NMP) to mix 30.78g of octadecylamine and 12.69g of polyetheramine (molecular weight: 1000), install the sealing and condensing device, and then pass in nitrogen gas, set the temperature at 50°C, and wait until the temperature reaches 50°C ℃ and stabilized for ten minutes, add the water separator, set the temperature to 80 ℃, after the temperature is constant, add 81.53g of epoxy silicone oil, slowly raise the temperature to 110 ℃, react for 2.5 hours, cool down to room temperature, add Add 6.85g of glacial acetic acid to emulsify with 215g of water. The cationic amino-modified epoxy silicone oil emulsion has a molecular weight of 5000, a particle size of 622.59nm, and a silicone oil content of 32%. The emulsion was stored at room temperature for 6 months or 3000 rpm / centrifuge for 30 minutes without precipitation.

Embodiment 2

[0086] Use 50g of N-methylpyrrolidone (NMP) to mix 28.66g of octadecylamine and 11.82g of polyetheramine (molecular weight: 1000). After installing the sealing and condensing device, nitrogen gas is introduced, and the temperature is set at 50°C until the temperature reaches 50°C. ℃ and stabilized for ten minutes, add the water separator, set the temperature to 80 ℃, after the temperature is constant, add 84.52g of epoxy silicone oil, slowly raise the temperature to 110 ℃, react for 2.5 hours, cool down to room temperature, add Add 6.38g of glacial acetic acid to emulsify with 215g of water. The cationic amino-modified epoxy silicone oil emulsion has a molecular weight of 10,000, a particle size of 193.97nm, and a silicone oil content of 32%. The emulsion was stored at room temperature for 6 months or 3000 rpm / centrifuge for 30 minutes without precipitation.

Embodiment 3

[0088] Use 50g of N-methylpyrrolidone (NMP) to mix 27.60g of octadecylamine and 11.38g of polyetheramine (molecular weight: 1000). After installing the sealing and condensing device, nitrogen gas is introduced, and the temperature is set at 50°C until the temperature reaches 50°C. ℃ and stabilized for ten minutes, add the water separator, set the temperature to 80 ℃, after the temperature is constant, add 86.02g of epoxy silicone oil, slowly raise the temperature to 110 ℃, react for 2.5 hours, cool down to room temperature, add Add 6.14g of glacial acetic acid to emulsify with 215g of water. The cationic amino-modified epoxy silicone oil emulsion has a molecular weight of 20,000, a particle size of 173.42nm, and a silicone oil content of 32%. The emulsion was stored at room temperature for 6 months or 3000 rpm / centrifuge for 30 minutes without precipitation.

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Abstract

The invention relates to a preparation method of self-assembled self-emulsified water-based cationic amino modified epoxy silicone oil and compounding and application of polyacrylonitrile carbon fiberprecursor oil. A certain amount of hydrophilic M1 and hydrophobic primary amine (R-NH2) or a secondary diamine (R1NH-R-NHR1) are put into a reaction kettle, heating is executed to 50-80 DEG C for melting or dissolving, then a certain amount of epoxy resin and a certain amount of epoxy silicone oil are added, reaction occurs for 2-6 hours under a nitrogen atmosphere at 90-115 DEG C, cooling is executed to room temperature to obtain amino modified epoxy silicone oil (AMOA), and a salt forming agent is added into a reaction kettle for neutralization; and after even stirring, a certain amount ofwater is added for emulsification to obtain a self-assembled self-emulsified aqueous cationic amino modified epoxy silicone oil emulsion. AMOA is compounded with one or more of auxiliary silicone oilsAMS1, AMS2 and AMS3, other additives and deionized water are added, and polyacrylonitrile carbon fiber protofilament oil agent is prepared under stirring. The oil agent is applied to a polyacrylonitrile carbon fiber production line.

Description

technical field [0001] The invention relates to a key component of a polyacrylonitrile carbon fiber raw silk oil agent, a preparation method of cationic amino-modified epoxy silicone oil and its compounding with auxiliary silicone oil, in particular to a self-assembled self-emulsifying amphiphilic cationic The preparation technology of amino-modified epoxy silicone oil and the compounding method of polyacrylonitrile carbon fiber precursor oil agent and its application in the production of polyacrylonitrile carbon fiber precursor. Background technique [0002] In the background description of US Patent US20170284016A1, it is mentioned that the oil agents are mainly epoxy-modified silicone oil, amine-modified silicone oil, polyether-modified silicone oil and their compounding. The role of the oil agent is to protect the polyacrylonitrile carbon fiber precursors from pre-oxidation and carbonization in an inert gas atmosphere at 200-400 ° C. When the temperature reaches 1000 ° C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46D06M15/647D06M15/65D06M101/28
CPCC08G77/46D06M15/647D06M15/652D06M2101/28
Inventor 杨春才
Owner 吉林乾仁新材料有限公司
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