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Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fibers

A technology of fatty acid ester and phenyl silicone oil, which is applied in the field of special low-silicone oil agent for carbon fiber, preparation, and polyol fatty acid ester/phenyl/polyether co-modified silicone oil. Problems such as uniform adhesion and affecting the overall performance of carbon fiber

Active Publication Date: 2021-05-11
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the perspective of raw materials, carbon fibers are mainly divided into two types: silicon-based oils and organic silicone-free oils. At present, high-performance carbon fibers mostly use silicon-based oils. This type of oil has excellent thermal stability and applicability that cannot be achieved by other compounds, but In the process of use, it is easy to produce trace SiC, SiOx and other silicides, and the ash content of carbon fiber is relatively large, which affects the performance of carbon fiber
In view of the silicon residue problem caused by the use of silicone-based oils alone, people have been trying to find organic silicone-free oils that can completely replace silicone-based oils in recent years. Currently, polyoxyethylene advanced aliphatic alkyl ethers, neopentyl alcohol derivatives Although non-siloxane compounds based on carbon fiber do not produce silicides during the preparation of carbon fibers, they have poor heat resistance and tend to produce hairs and broken filaments in the pre-oxidation and carbonization stages, which makes the mechanical properties of carbon fibers Therefore, the development of carbon fiber oil agent focuses on reducing the silicon content appropriately without affecting the fiber performance, and adding non-silicon organic compounds with good heat resistance to silicone oil to form a low-silicon oil agent
[0004] Among the low-silicon oils, modified silicone oils, emulsifiers and heat-resistant organic ester compounds (such as pentaerythritol fatty acid esters, trimethylolpropane fatty acid esters, pyromellitic acid fatty alcohol esters, etc.) The method of preparing oil emulsion by direct mixing, and then turning to emulsification, but the problem of this process is: the local compatibility between the added heat-resistant organic ester compound and silicone oil is poor, and microscopic phase separation is easy to occur, so that the oil can not be evenly attached. On the surface of the carbon fiber precursor fiber bundle (precursor), it affects the overall performance of the carbon fiber

Method used

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  • Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fibers
  • Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fibers
  • Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fibers

Examples

Experimental program
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Effect test

Embodiment 1

[0033] In a 500mL three-necked flask with a thermometer and mechanical stirring, add 59.64g octaphenylcyclotetrasiloxane, 117.16g octamethylcyclotetrasiloxane and 23.65g octamethyltrisiloxane, 20mL dry toluene, Then add 1.00g of potassium hydroxide alkali gel and 9.00g of tetramethylammonium hydroxide alkali gel as a catalyst, raise the temperature to 110°C under the protection of nitrogen, stir and react for 10h, after the reaction is completed, remove the catalyst by washing with water, and heat the organic phase to At 140°C, the solvent and low boilers were distilled off under reduced pressure to obtain a colorless and transparent phenyl silicone oil with a yield of 95%.

Embodiment 2

[0035] In a 250mL three-necked flask with a thermometer and mechanical stirring, add 50.00g of phenyl-modified silicone oil, 20.00mL of toluene, 2.40g of acid clay, 2.40g of high hydrogen-containing silicone oil (the hydrogen content is 1.67%) synthesized in Example 1 , viscosity is 300mPa·s), N 2 Under protection, the temperature was raised to 100°C, the reaction was stirred for 10 h, the catalyst was removed by filtration, and the solvent and low boilers were distilled off under reduced pressure to obtain a colorless, transparent and viscous phenyl hydrogen-containing silicone oil with a yield of 95%.

Embodiment 3

[0037] In a 250mL three-necked flask equipped with a thermometer, mechanical stirring and a water separator, add 55.90g of n-octanoic acid, 30g of trimethylolpropane monoallyl ether, 30mL of toluene, 1g of p-toluenesulfonic acid, and 0.7g of inhibitor BHT, heated to 110°C for dehydration reaction for 6 hours, stopped heating, cooled to room temperature, washed with water to remove the catalyst, and distilled off the solvent under reduced pressure to obtain light yellow trimethylolpropane monoallyl ether dicaprylate with a yield of 94.5 %.

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Abstract

The invention discloses polyol fatty acid ester / phenyl / polyether co-modified silicone oil, a preparation method and a special low-silicon oil agent for carbon fibers which is prepared by taking the co-modified silicone oil as a main component and meets the production requirements of the carbon fibers, and belongs to the technical field of preparation of oil agents for the carbon fibers. By starting from octaphenylcyclotetrasiloxane, octamethylcyclotetrasiloxane and hydrogen-containing silicone oil, phenyl hydrogen-containing silicone oil is prepared through an anionic ring-opening polymerization reaction, then polyol fatty acid ester with good heat resistance is introduced through a hydrosilylation reaction to further reduce the silicon content, a polyether chain segment is introduced to improve the hydrophilicity of the silicone oil, and thus, the polyol fatty acid ester / phenyl / polyether co-modified silicone oil is obtained. The special low-silicon oil agent for carbon fibers is an emulsion composed of a main component and water, wherein the mass percentage of the main component is 1-40%. The main component is composed of the polyol fatty acid ester / phenyl / polyether co-modified silicone oil, an emulsifier, an antioxidant, an anti-static agent, a heat-resistant ester compound and non-ester modified silicone oil.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber oil preparation, and specifically relates to a polyol fatty acid ester / phenyl / polyether co-modified silicone oil, a preparation method, and a carbon fiber oil that meets the production requirements of carbon fibers prepared by using the co-modified silicone oil as the main component. Special low silicon oil agent for carbon fiber. Background technique [0002] Carbon fiber has excellent properties such as light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, and thermal conductivity. It is an indispensable new material in aerospace and other fields. With the expansion of production scale , and its application fields have gradually expanded to civilian fields such as sports equipment, textile machinery, transportation machinery, construction engineering, and automotive materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46D06M15/647D06M15/65D06M15/53D06M13/463D06M13/292D06M101/40
CPCC08G77/46D06M15/647D06M15/65D06M15/53D06M13/463D06M13/292D06M2101/40
Inventor 杨清彪屈德辉宋岩李耀先
Owner JILIN UNIV