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Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof

An amino-modified and aminopropyl-modified technology, applied in the direction of silicon organic compounds, carbon fibers, fiber processing, etc., can solve the problems of high-performance carbon fiber damage, broken wires, sticking rollers, etc., and achieve the effect of improving heat resistance

Active Publication Date: 2016-02-03
新元化学(山东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two major problems with the current silicon-containing oil agent. One is that the amino silicone oil will cross-link and stick to the roller after the production line runs for a long time. The phenomenon of embrittlement and fracture will damage the surface of carbon fiber, especially for high-performance carbon fiber, and even broken wires will occur

Method used

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  • Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof
  • Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof
  • Compound for improving heat resistance of amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A compound A that improves the heat resistance of amino-modified silicone oil carbon fiber oil has a structure shown in formula (I):

[0036]

[0037] In formula (I), z=2-5.

[0038] Preparation method: Mix 88.8g of hexamethylcyclotrisiloxane and 160.8g of tetramethyldisiloxane, stir evenly, lower the temperature to 0°C, add 0.1g of catalyst trifluoromethanesulfonic acid, react for 0.5h, medium And to neutral, vacuum distillation, pressure 1.33kPa, take 115 ℃ ~ 120 ℃ fraction, obtain decamethyldihydropentasiloxane; 71.2g of the above-mentioned ultra-short chain hydrogen-containing silicone oil, 45.6g of allyl glycidol Ether was mixed with 0.08g of Carl's Platinum catalyst, heated to 85°C, reacted for 3h, and unreacted raw materials were removed by distillation under reduced pressure to obtain compound A (z=3).

[0039] figure 1 For the infrared spectrogram of the compound A that this embodiment makes, wherein 792.28cm -1 , 839.14, 1249.94cm -1 for Si-CH 3 Absorp...

Embodiment 2

[0041] Mix 88.8g of hexamethylcyclotrisiloxane and 107.2g of tetramethyldisiloxane, stir evenly, lower the temperature to 10°C, add 0.1g of catalyst trifluoromethanesulfonic acid, react for 2h, neutralize to neutral, Vacuum distillation, pressure 1.33kPa, take 105 ℃ ~ 135 ℃ fraction to obtain ultra-short-chain hydrogen-containing silicone oil; mix 89g of the above-mentioned ultra-short-chain hydrogen-containing silicone oil, 45.6g allyl glycidyl ether and 0.08g platinum catalyst, and heat up to 85°C, react for 3 hours, and distill off unreacted raw materials under reduced pressure to obtain A, which is a mixture of z=2~5.

Embodiment 3

[0043] Side chain aminopropyl modified silicone oil has the structure shown in formula (II):

[0044]

[0045] (II), x=80~160, y=1~3.

[0046] Preparation method: 890g octamethylcyclotetrasiloxane, 24.9g aminopropylmethyldiethoxysilane, 4.9g deionized water, 16.2g hexamethyldisiloxane and 0.09g tetramethylhydroxide Ammonium is added to the reactor, and N 2 , stir, heat up to 80°C to 90°C for 2 hours, then reduce the pressure to 66.7kPa, raise the temperature to 100°C to 110°C for 4 hours, return to normal pressure, raise the temperature to 170°C for 1 hour to decompose the catalyst, and finally reduce the pressure to 133Pa Raise the temperature to 175°C to 180°C to remove small molecular substances, and obtain a side chain aminopropyl modified silicone oil with a kinematic viscosity of 200cp, an ammonia value of 0.16mmol / g, and a volatile component of 3.43%.

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Abstract

The invention relates to a compound for improving the heat resistance of an amino-modified silicone oil carbon fiber oil formulation and preparation and application thereof. The compound has the structure shown in a formula (I). The compound is added into the oil formulation to be used by compounding with side chain aminopropyl-modified silicone oil with the kinematic viscosity of 80 cp-300 cp and the amino value of 0.15 mmol / g-0.20 mmol / g, the heat resistance of the oil formulation is greatly improved, and the problems of glue solidifying and roll sticking of the modified silicon oil formulation and modified silicon oil formulation embrittling and fracturing which occur in pre-oxidizing at 350 DEG C are solved.

Description

technical field [0001] The invention relates to a compound for improving the heat resistance of an amino-modified silicone oil carbon fiber oil agent and its preparation and application, belonging to the technical field of oil agents. Background technique [0002] Carbon fiber is a key material supporting strategic emerging industries, and is widely used in national defense, aerospace, wind power, building reinforcement, sporting goods and other fields. [0003] Carbon fiber oil is an essential and important additive in the production process of carbon fiber. It can effectively protect and lubricate carbon fiber in the stages of spinning, pre-oxidation and low-temperature carbonization. It can be said that without high-quality oil, high-quality carbon fiber cannot be produced. . At present, the production technology of carbon fiber oil is mainly mastered by Japanese companies, and domestic technology is relatively backward. [0004] Modified silicone oils have attracted wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/513D06M15/643D06M15/53D06M13/463C07F7/08C08G77/26D06M101/40
Inventor 田志钢解乐福解承钢杨燕张殿松
Owner 新元化学(山东)股份有限公司
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