N,N-bis(trimethylsilyl)allylamine and preparation method thereof

A technology of trimethylsilyl and allylamine, applied in the field of N, can solve the problems of corrosion of production equipment, high reaction cost and high price, and achieve the effects of prolonging service life, high conversion rate of raw materials and reducing reaction cost

Inactive Publication Date: 2017-05-31
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] a. Use trimethylchlorosilane and allylamine as raw materials to react to generate hydrogen chloride and N, N-bis(trimethylsilyl)allylamine. Because hydrogen chloride has strong acidity, it will corrode production equipment and pollute environment, triethylamine needs to be used for neutralization to generate triethylamine hydrochloride, which is mixed with N,N-bis(trimethylsilyl)allylamine, it is difficult to separate and purify, and it is difficult to obtain High target product N,N-bis(trimethylsilyl)all

Method used

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  • N,N-bis(trimethylsilyl)allylamine and preparation method thereof
  • N,N-bis(trimethylsilyl)allylamine and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0043] Install a stirrer, a constant pressure dropping funnel, a reflux condenser and a thermometer on the four-necked flask, control the temperature in the four-necked flask at 10°C, feed nitrogen into the flask until the bottle is full of nitrogen, and dissolve 28.5g of allylamine Add 1.2g of trifluoromethanesulfonic acid into the flask, add 96.6g of hexamethyldisilazane into the constant pressure dropping funnel, start stirring, and after stirring for 10min, dropwise drop hexamethyldisilazane into the flask, The dropping time is 30 minutes, and after the dropping, the temperature is raised to 100° C. and kept for 4 hours.

[0044] Then cool down to room temperature, at a temperature of 80 ° C, under reduced pressure distillation under the condition of 58mmHg to obtain 82.1gN, N-bis(trimethylsilyl)allylamine product, the calculated yield of the product is 81% , The purity of N,N-bis(trimethylsilyl)allylamine was 99.0%.

Embodiment 2

[0046] Install a stirrer, a constant pressure dropping funnel, a reflux condenser and a thermometer on the four-necked flask, control the temperature in the four-necked flask at 28°C, feed nitrogen into the flask until the bottle is full of nitrogen, and dissolve 28.5g of allylamine Add 1.2g of concentrated sulfuric acid into the flask, add 96.6g of hexamethyldisilazane into the constant pressure dropping funnel, start stirring, and after stirring for 10 minutes, add hexamethyldisilazane dropwise into the flask at a constant speed, and the dropping time After 30 minutes, the temperature was raised to 110°C and kept for 5 hours after dropping.

[0047] Cool down to room temperature then, be 85 ℃ in temperature, underpressure distillation under the condition of 65mmHg obtain 81.7gN, N-bis(trimethylsilyl)allylamine product, calculate the yield of product and be 80.2% , The purity of N,N-bis(trimethylsilyl)allylamine was 98.6%.

Embodiment 3

[0049]Install a stirrer, a constant pressure dropping funnel, a reflux condenser and a thermometer on the four-necked flask, control the temperature in the four-necked flask at 28°C, feed nitrogen into the flask until the bottle is full of nitrogen, and dissolve 28.5g of allylamine and 1.2 titanium tetrachloride were added to the flask, 96.6g of hexamethyldisilazane was added to the constant pressure dropping funnel, and stirring was started. After stirring for 10 minutes, hexamethyldisilazane was added dropwise to the flask at a constant speed, and The time is 40 minutes, and after the dripping is completed, the temperature is raised to 110° C. and kept for 5.5 hours.

[0050] Cool down to room temperature then, be 85 ℃ in temperature, underpressure distillation obtain 81.2g N under the condition of pressure 65mmHg, N-bis(trimethylsilyl) allyl amine product, the yield that calculates product is 80.14% , The purity of N,N-bis(trimethylsilyl)allylamine was 98.7%.

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Abstract

The invention discloses N,N-bis(trimethylsilyl)allylamine and a preparation method thereof, and relates to the field of organic polymer materials. The preparation method comprises the following steps of at the temperature lower than 30 DEG C, adding a catalyst and 1 parts of allylamine into a reaction kettle in parts by mass, and uniformly stirring, wherein the catalyst is lewis acid; B, adding 1.1 to 1.3 parts of hexamethyl-disilazane into the reaction kettle, heating to 90 to 110 DEG C, and conducting heat preservation for 4 to 6h, so as to obtain a crude product of N,N-bis(trimethylsilyl)allylamine. The preparation method has the advantages that the yield rate and the product purity are increased, the product cost is reduced, and the friendly effect on equipment and environment is good.

Description

technical field [0001] The invention relates to the field of organic polymer materials, in particular to N,N-bis(trimethylsilyl)allylamine and a preparation method thereof. Background technique [0002] Polyimide (Polyimide, PI) is a class of polymers containing imide rings in the main chain. It has good heat resistance and insulation properties. It is widely used in aerospace, electronic and electrical fields, and is also extended to adhesive , Filtration separation and other fields, these fields put forward higher requirements for the performance of polyimide. [0003] In order to improve the performance of polyimide, fluorine-containing monomers are usually used to participate in the reaction. However, the price of fluorine-containing monomers is relatively expensive, resulting in high synthesis costs. For this reason, silicones have been developed for modifying polyimides. Imide, so that it has better solubility, adhesion, high and low temperature resistance and process...

Claims

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Application Information

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IPC IPC(8): C07F7/10C07F7/20
CPCC07F7/10C07F7/20
Inventor 冯琼华肖俊平梁成凯王智威
Owner 湖北新蓝天新材料股份有限公司
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