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Preparation method of heptafluoroisobutyronitrile

A technology for heptafluoroisobutyronitrile and heptafluoroisobutyramide is applied in the field of preparation of perfluoroisobutyronitrile, can solve the problems of low yield, unfavorable industrial scale up, high cost, and achieves high reaction yield and easy industrial production , the effect of mild reaction conditions

Pending Publication Date: 2020-06-30
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In this method, perfluoroisobutyramide is dehydrated to prepare heptafluoroisobutyronitrile step. If a general dehydrating agent is used, the yield will be low and the cost of waste treatment will be high. If an expensive dehydrating agent is used, although it can solve the problem of low yield problem, but the cost is too high, which is not conducive to industrial scale-up

Method used

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  • Preparation method of heptafluoroisobutyronitrile
  • Preparation method of heptafluoroisobutyronitrile
  • Preparation method of heptafluoroisobutyronitrile

Examples

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Embodiment 1

[0038] The volume of the reaction kettle is 10L, equipped with stirring, thermometer and condenser, and connected with gas cooling and absorption device. Add 3.00 kg of methyl tert-butyl ether, 2.10 kg of p-toluenesulfonyl chloride, and 2.13 kg of heptafluoroisobutyramide into the reaction kettle, and cool down to -10°C after the addition. Then start to add 1.2 kg of triethylamine dropwise, control the reaction temperature at -10 to 0°C, and keep the temperature at -10°C for 2.0 hours after the dropwise addition. After the reaction, the temperature was raised to 30° C. and kept for 4.0 hours. During the process, the gas escaped from the system was cooled to make it liquefied, and a total of 1.92 kg of heptafluoroisobutyronitrile was obtained with a purity of 99.6% and a yield of 98.1%.

Embodiment 2

[0040] The volume of the reaction kettle is 10L, equipped with stirring, thermometer and condenser, and connected with gas cooling and absorption device. Add 3.00 kg of methyl tert-butyl ether, 2.10 kg of p-toluenesulfonyl chloride, and 2.13 kg of heptafluoroisobutyramide into the reaction kettle, and cool down to -10°C after the addition. Then start to add 1.1 kg of aniline dropwise, control the reaction temperature at -10 to 0°C, and keep the temperature at -10°C for 2.0 hours after the dropwise addition. After the reaction, the temperature was raised to 30° C. and kept for 4.0 hours. During the process, the gas escaped from the system was cooled and liquefied to obtain 1.77 kg of heptafluoroisobutyronitrile with a purity of 99.2% and a yield of 90.4%.

Embodiment 3

[0042] The volume of the reaction kettle is 10L, equipped with stirring, thermometer and condenser, and connected with gas cooling and absorption device. Add 3.00 kg of methyl tert-butyl ether, 2.10 kg of p-toluenesulfonyl chloride, and 2.13 kg of heptafluoroisobutyramide into the reaction kettle, and cool down to -10°C after the addition. Then start to add 1.0 kg of cyclohexylamine dropwise, control the reaction temperature at -10 to 0°C, and keep the temperature at -10°C for 2.0 hours after the dropwise addition. After the reaction, the temperature was raised to 30° C. and kept for 4.0 hours. During the process, the gas escaped from the system was cooled and liquefied to obtain 1.83 kg of heptafluoroisobutyronitrile with a purity of 99.6% and a yield of 93.7%.

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Abstract

The invention discloses a method for preparing heptafluoroisobutyronitrile. According to the method, heptafluoroisobutyronitrile is prepared by taking p-toluenesulfonyl chloride and heptafluoroisobutyramide as raw materials. The preparation method provided by the invention has the advantages of high yield, low cost, basically no three wastes, mild operation conditions and suitability for industrial production.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing nitrile, in particular to a preparation method of perfluoroisobutyronitrile. Background technique [0002] Heptafluoroisobutyronitrile is a potential insulating gas, and its preparation method is reported to have two preparation routes. [0003] The first preparation route uses nitrogen-containing heterocycles as starting materials, and generates heptafluoroisobutyronitrile after the nitrogen-containing heterocycles are ring-opened by high-energy means such as light irradiation or thermal cracking. For example, document J.CHEM.SOC.PERKIN TRANS.1, 1990:983-987 has reported the method that adopts the photochemical method to synthesize heptafluoroisobutyronitrile as raw material with fluoro-1,2,3-triazine compounds , the reaction equation is as follows: [0004] [0005] This method has high cost of raw materials, low reaction yield, harsh reaction conditions, and is not suitable fo...

Claims

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Application Information

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IPC IPC(8): C07C255/10C07C253/20C07C309/73C07C303/28
CPCC07C253/20C07C303/28C07C309/73C07C255/10
Inventor 蒋强倪航李华张洁明王飞
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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