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A kind of polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fiber

A technology of fatty acid ester and phenyl silicone oil, which is applied in the fields of carbon fiber, fiber treatment, textiles and papermaking, etc. It can solve the problems of affecting the overall performance of carbon fiber, prone to microscopic phase separation, and deterioration of carbon fiber mechanical properties.

Active Publication Date: 2022-05-27
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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  • A kind of polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fiber
  • A kind of polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fiber
  • A kind of polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low-silicon oil agent for carbon fiber

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, 23.65g octamethyltrisiloxane, 20mL dry toluene, Then add 1.00g potassium hydroxide alkali glue and 9.00g tetramethylammonium hydroxide alkali glue as catalysts, heat up to 110 ℃ under nitrogen protection, stir the reaction for 10h, the reaction is over, wash with water to remove the catalyst, the organic phase is dried, heated to At 140° C., the solvent and low boilers were distilled off under reduced pressure to obtain colorless and transparent phenyl silicone oil with a yield of 95%.

Embodiment 2

[0035] In a 250 mL three-necked flask with a thermometer and mechanical stirring, add 50.00 g of phenyl modified silicone oil synthesized in Example 1, 20.00 mL of toluene, 2.40 g of acid clay, and 2.40 g of high-hydrogen silicone oil (with a hydrogen content of 1.67%). , the viscosity is 300mPa s), N 2 The temperature was raised to 100°C under protection, the reaction was stirred for 10 hours, the catalyst was removed by filtration, and the solvent and low boilers were removed by distillation 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 with a thermometer, mechanical stirring and a water separator, add 55.90g n-octanoic acid, 30g trimethylolpropane monoallyl ether, 30mL toluene, 1g p-toluenesulfonic acid, 0.7g polymerization inhibitor BHT, heated to 110 °C for dehydration reaction for 6 h, stopped heating, cooled to room temperature, washed with water to remove the catalyst, distilled under reduced pressure to remove the solvent, and obtained light yellow trimethylolpropane monoallyl ether dioctanoate with a yield of 94.5 %.

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Abstract

A polyol fatty acid ester / phenyl / polyether co-modified silicone oil, a preparation method, and a special low-silicone oil agent for carbon fiber prepared from the co-modified silicone oil as the main component to meet the production requirements of carbon fiber, belonging to the carbon fiber oil preparation technology field. The present invention starts from octaphenylcyclotetrasiloxane, octamethylcyclotetrasiloxane, and hydrogen-containing silicone oil, prepares phenyl hydrogen-containing silicone oil through anionic ring-opening polymerization, and then introduces heat resistance through hydrosilylation A good polyol fatty acid ester further reduces the silicon content, introduces a polyether segment to improve the hydrophilicity of the silicone oil, and obtains a polyol fatty acid ester / phenyl / polyether co-modified silicone oil. The special low-silicone oil agent for carbon fiber is an emulsion composed of the main component and water, the mass percentage of the main component is 1-40%; the main component is co-modified by polyol fatty acid ester / phenyl / polyether Composed of silicone oil, emulsifier, antioxidant, antistatic agent, 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 in particular relates to a polyol fatty acid ester / phenyl / polyether co-modified silicone oil, a preparation method and a carbon fiber production requirement prepared by using the co-modified silicone oil as the main component Low silicone oil 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 civil fields such as sports equipment, textile machinery, transportation machinery, construction engineering, and automotive materials. [0003] In the production of carbon fiber, the f...

Claims

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Application Information

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Patent Type & Authority Patents(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