Unlock instant, AI-driven research and patent intelligence for your innovation.

A polyol ester/polyether co-modified silicone oil and special oil for carbon fiber

A polyol ester, co-modification technology, applied in the direction of carbon fiber, etc., can solve the problems of affecting the overall performance of carbon fiber, poor hydrophilicity of ester-modified silicone oil, and impact of carbon fiber performance.

Active Publication Date: 2017-06-20
JILIN UNIV
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The oils used for carbon fiber manufacturing are mainly divided into silicon-based oils and organic non-silicon oils. Among them, non-silicon oils have poor heat resistance and less dosage. At present, silicon-based oils are still dominant. This type of oil Silicone oils are usually made of modified silicone oils such as amino, epoxy, and polyether as the main raw material, and are water-based emulsions formed with the participation of emulsifiers and other additives. Compared with non-silicon oils, the heat resistance of silicone oils is significantly improved. , but people have gradually discovered that silicon-based oils cannot be completely decomposed and volatilized during the entire heating and carbonization process, and the residual silicon is very easy to form trace amounts of SiC and SiO x and Si 3 N 4 , so that the performance of carbon fiber is affected
In recent years, the low-silicon type oil agent added with heat-resistant organic ester compounds has attracted people's attention. Most of the technology adopts the method of physical blending and re-emulsification of silicone oil and organic ester, but the problem of this process is that the ester The local compatibility between the silicone compound and silicone oil is poor, resulting in microscopic phase separation, so that the oil emulsion formed by the two cannot be evenly attached to the surface of the carbon fiber precursor fiber bundle, and ultimately affects the overall performance of the carbon fiber. We are in the patent (Application No. 201310566072.8, Yang Qingbiao, Li Yaoxian, Wang Lige, Guo Jing, Wang Xiuling, A Polyol Ester Modified Silicone Oil, Preparation Method and Carbon Fiber Special Oil) Invented a carbon fiber special oil preparation method with polyol ester modified silicone oil as the key component , in this patent, the organic ester with good heat resistance is grafted to the side chain of silicone oil, which can avoid the microscopic phase separation problem caused by physical blending, and a series of oil formulations can be formed by precisely adjusting the composition of the emulsifier, but due to The hydrophilicity of ester-modified silicone oil is relatively poor, and the requirements for the formula are relatively strict. Even a small change will affect the stability of the oil emulsion, which is not conducive to the local adjustment of the oil formula according to the production needs in the industry.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A polyol ester/polyether co-modified silicone oil and special oil for carbon fiber
  • A polyol ester/polyether co-modified silicone oil and special oil for carbon fiber
  • A polyol ester/polyether co-modified silicone oil and special oil for carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 36.38g of trimethylolpropane monoallyl ether, 100mL of toluene, and 73.17mL of triethylamine into a 500mL three-neck flask with mechanical stirring, slowly add 85.7mL of octanoyl chloride dropwise under ice-water bath with stirring and cooling, and the dropwise addition ends After that, continue to stir for 6.0h to make the reaction complete. After the reaction is finished, filter off the generated triethylamine hydrochloride, and use 40mL of 5.0% NaHCO 3 The aqueous solution was washed once until neutral, and then the solvent was distilled off under reduced pressure to obtain light yellow trimethylolpropane monoallyl ether dicaprylate with a yield of 92%.

Embodiment 2-3

[0025] 30g trimethylolpropane monoallyl ether dicaprylate synthesized in Example 1, a small amount of toluene and 2.044g catalyst (the isopropanol solution of 5.0% chloroplatinic acid by mass percentage) are added with mechanical stirring, spherical In a 250mL three-necked flask with a condenser tube and a constant pressure dropping funnel, after passing nitrogen gas into it and activating at 30°C for 1.0h, put 10.88g of low-hydrogen silicone oil (hydrogen content: 0.4, viscosity: about 200mPa·s, self-made according to literature, literature For: Ma Fengguo, Liu Chunxia, ​​Shen Wenling, Research on Preparation of Low Hydrogen Silicone Oil by Telomerization of High Hydrogen Silicone Oil, Organic Silicon Materials, 2010, 24, 356-359) diluted with toluene to 50% of the original mass, added to constant pressure drops In the liquid funnel, start the stirrer, raise the temperature to 100°C under the protection of nitrogen, drop the diluted low-hydrogen silicone oil into the three-nec...

Embodiment 4-5

[0028] Trimethylolpropane monoallyl ether dicaprylate modified silicone oil was synthesized according to the method in Example 2.

[0029] Add the long-chain polyether AEM-8 containing C=C double bond and catalyst (5.0% by mass percentage of isopropanol solution of chloroplatinic acid) into a 500mL three-necked flask with mechanical stirring, spherical condenser and constant pressure dropping funnel Nitrogen gas was passed through, activated at 30°C for 1.0h, and the temperature was raised to 100°C under the protection of nitrogen, and then slowly added trimethylolpropane monoallyl ether dicaprylate modified silicone oil solution dropwise within 1.5h, dropwise Continue to react for 5.0 hours after the addition is completed. After the reaction is completed, the solvent and low boilers are evaporated under reduced pressure to obtain a transparent and viscous trimethylolpropane monoallyl ether dicaprylate / polyether (AEM-8) co-modified non-toxic silicone oil, the product yield is ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
viscosityaaaaaaaaaa
viscosityaaaaaaaaaa
viscosityaaaaaaaaaa
Login to View More

Abstract

The invention provides polyol ester / polyether co-modified silicone oil and a special oil agent for carbon fiber, which takes the polyol ester / polyether co-modified silicone oil as a main component, and belongs to the technical field of chemical fibers. According to the invention, a polyether segment is introduced to polyol ester modified silicone oil to obtain the polyol ester / polyether co-modified silicone oil with very good emulsifying capability. The synthesized polyol ester / polyether co-modified silicone oil has good emulsifying property and can form stable-property waterborne emulsion together with various surfactants. The special oil agent for carbon fibers, disclosed by the invention, is not limited specially when in use. The special oil agent for carbon fibers is diluted with deionized water into 1.0-3.0wt% emulsion according to a common method; then, densified carbon fiber precursors are soaked in the diluted emulsion in an oiling tank and then are dried, coiled, pre-oxidized and carbonized, something like that; and thus carbon fibers are obtained finally.

Description

technical field [0001] The invention belongs to the technical field of chemical fibers, and in particular relates to a polyol ester / polyether co-modified silicone oil and a special oil agent for carbon fibers prepared from the polyol ester / polyether co-modified silicone oil as the main component. Background technique [0002] Carbon fiber has excellent properties such as high strength, low density, high temperature resistance, and corrosion resistance, and is widely used in aerospace, national defense, military, and construction vehicles. At present, when carbon fiber is produced industrially, most of the process routes are to pre-oxidize the raw silk through an oxidation furnace, and then perform high-temperature carbonization and graphitization on the pre-oxidized silk. During this process, a large amount of tar is produced with complex exothermic reactions. It is easy to cause the adhesion of fiber bundles, and defects, wool and broken filaments will be generated during t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G77/38D06M15/647D06M15/643D06M101/40
Inventor 杨清彪边坤李耀先宋岩郭靖
Owner JILIN UNIV