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Method and device for continuously preparing heptafluoroisobutyramide

A technology of heptafluoroisobutyramide and heptafluoroisobutyryl, which is applied in the field of preparation of heptafluoroisobutyramide, can solve the problems of complex post-processing, difficult process, high price, etc., and achieve easy industrial production and shorten the process flow , The effect of high production efficiency

Pending Publication Date: 2020-05-29
昊华气体有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Among the above methods, the raw material of acyl fluoride in method (1) is highly toxic, and its rectification and purification have high requirements for the safety of equipment and operation, and the process route has many steps and complicated post-treatment, so the overall process is relatively difficult
The perfluorinated compound raw material that selects in the organic synthesis method in the method (2) is expensive; Take acid fluoride as the preparation method of intermediate, need to use complex catalysis or catalytic cracking system, increased the difficulty of technology, and the use of metal catalyst is not enough Economical and environmentally friendly; at the same time, this type of method also includes the problem of rectification and purification of heptafluoroisobutyryl fluoride after cracking, and the process is difficult

Method used

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  • Method and device for continuously preparing heptafluoroisobutyramide
  • Method and device for continuously preparing heptafluoroisobutyramide

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Such as figure 1 Shown, a kind of device that the method for continuously preparing heptafluoroisobutyramide uses comprises electrolytic kettle (1), condensation reflux device (2), catcher (3), spray tower (4), still ( 5), distillation condenser (6); the electrolytic kettle (1) is connected to the condensing reflux (2), the top of the trap (3) is connected to the top of the condensing reflux (2), and the bottom of the trap (3) is connected to the spray The bottom of the tower (4), and the top of the spray tower (4) are connected to the distillation kettle (5), and the spray tower (4) realizes material circulation through a delivery pump, and a distillation condenser (6) is connected to the distillation kettle (5); The vacuum system is externally connected to the device (6); the trap (3), the spray tower (4), and the distillation condenser (6) all have vent pipelines leading to the acid mist purification tower; two traps are connected in parallel.

[0028] Use isobutyri...

Embodiment 2

[0030] Use isobutyric anhydride and hydrogen fluoride as raw materials, control the electrolysis voltage to 4.0-8.0V, and the current density to 5-50mA / cm 2 , electrolysis under steady flow conditions. During the electrolysis process, the condensing temperature is controlled at 10-15°C, and the trap temperature is -15--10°C. After the heptafluoroisobutyryl fluoride in the trap reaches a predetermined weight, the trap is switched to ensure the normal operation of the electrolysis; The temperature in the washing tower is 35-45°C, add an amine methanol solution with a concentration of 10mol / L, and start the circular spraying; control the flow rate of heptafluoroisobutyryl fluoride to enter the spray tower at a flow rate of 100-250g / min, After the addition of isobutyryl fluoride, stop spraying; transfer the reaction solution to a vacuum distillation kettle, under stirring, control the temperature of the kettle to 50°C, vacuum degree of 0.09MPa, remove the solvent by distillation u...

Embodiment 3

[0032] Use isobutyric anhydride and hydrogen fluoride as raw materials, control the electrolysis voltage to 4.0-8.0V, and the current density to 5-50mA / cm 2 , electrolysis under steady flow conditions. During the electrolysis process, the condensation temperature is controlled at -80~-60°C, and the trap temperature is -150~-192°C. After the heptafluoroisobutyryl fluoride in the trap reaches the predetermined weight, switch the trap to ensure the normal operation of the electrolysis ;Control the temperature in the washing tower to 0-35°C, add amine-methanol solution with a concentration of 3mol / L, and start the circular spraying; control the flow rate of acyl fluoride to enter the spray tower at a flow rate of 400-500g / min, and wait for the addition of acyl fluoride to be completed , stop spraying; transfer the reaction solution to a vacuum distillation kettle, under stirring, control the temperature of the kettle at 60°C, vacuum degree 0.085MPa, remove the solvent by distillat...

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Abstract

The invention discloses a method and device for continuously preparing heptafluoroisobutyrylamide. The method comprises the steps: carrying out electrolytic fluorination on isobutyric anhydride, carrying out condensation reflux on electrolytic gas to remove hydrogen fluoride, and freezing to collect heptafluoroisobutyryl fluoride; carrying out a reaction on heptafluoroisobutyryl fluoride with an ammonia methanol solution in a spray tower, carrying out reduced pressure distillation after the reaction is finished to obtain a heptafluoroisobutyrylamide crude product, and recrystallizing to obtainthe heptafluoroisobutyrylamide product. The device comprises an electrolysis kettle (1), a reflux condenser (2), a catcher (3), a spray tower (4), a distillation kettle (5) and a distillation condenser (6). The method and the device are simple in process, high in equipment efficiency and easy for industrial production.

Description

technical field [0001] The invention relates to a preparation method and device of heptafluoroisobutyramide. Background technique [0002] Heptafluoroisobutyramide is a key precursor compound for the preparation of new insulating and environmentally friendly gas perfluoroisobutyronitrile. The existing reported synthesis methods are as follows: [0003] (1) Electrolytic synthesis method, the patent document US 2015 / 0083979A1 reported that using acid anhydride as the starting material, electrolytic fluorination to obtain perfluoroisobutyryl fluoride, after separation and purification by rectification, esterification reaction with methanol to obtain perfluoroisobutyryl fluoride Methyl butyrate, and then react with ammonia methanol solution to prepare perfluoroisobutyronitrile heptafluoroisobutyramide. [0004] [0005] (2) Organic synthesis method, organic synthesis method is divided into the following types: [0006] Patent document CN108424375A uses hexafluoropropylene a...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C231/24C07C233/05C25B3/08C25B3/28
CPCC07C231/02C07C231/24C25B3/28C07C233/05
Inventor 牛鹏飞任章顺汪建春黄晓磊张金彪牛学坤袁胜芳
Owner 昊华气体有限公司
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