Continuous production process of perfluor-2-methyl-3-pentanone

A technology of methyl and pentanone, which is applied in the chemical industry, sustainable manufacturing/processing, organic chemistry, etc., and can solve problems such as complex processes

Active Publication Date: 2018-04-06
SHANGHAI AIMO JINSHAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The characteristic of this reaction is that starting from the readily available commercial raw material hexafluoropropylene dimer, the yield is relatively high. Howev...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] Preparation of hexafluoropropylene dimer: add KF / tetramethylethylenediamine / acetonitrile into the reaction kettle at a mass ratio of 1 / 2 / 100, stir at 40°C for one hour, then transfer to the catalyst solution storage tank for use. The hexafluoropropylene steel cylinder and catalyst solution storage tank are connected with the continuous reactor through a delivery pump. The catalyst solution is pumped in at 20 kg / hour, and hexafluoropropylene gas is fed in, the reaction time is controlled at 30-70 seconds, and the temperature is controlled at 25°C. Adjust the pressure of the hexafluoropropylene inlet to 0.1-0.3MPa; the outlet is connected to the phase separation kettle, the catalyst solution in the upper layer enters the catalyst storage tank for the reaction cycle, the lower layer is the crude product of hexafluoropropylene dimer, and the pure product is obtained by rectification , yield 32%.

Embodiment 2

[0092] Preparation of hexafluoropropylene dimer: add KF / tetrabutylammonium fluoride / acetonitrile into the reaction kettle at a mass ratio of 1 / 4.5 / 100, stir at 40°C for one hour, then transfer to the catalyst solution storage tank for use. The hexafluoropropylene steel cylinder and catalyst solution storage tank are connected with the continuous reactor through a delivery pump. The catalyst solution is pumped in at 20 kg / hour, and hexafluoropropylene gas is fed in, the reaction time is controlled at 30-70 seconds, and the temperature is controlled at 25°C. Adjust the pressure of the hexafluoropropylene inlet to 0.1-0.3MPa; the outlet is connected to the phase separation kettle, the catalyst solution in the upper layer enters the catalyst storage tank for the reaction cycle, the lower layer is the crude product of hexafluoropropylene dimer, and the pure product is obtained by rectification , yield 45%.

Embodiment 3

[0094] Preparation of hexafluoropropylene dimer: add KF / 18-crown ether-6 / acetonitrile into the reaction kettle at a mass ratio of 1 / 4.6 / 100, stir at 40°C for one hour, then transfer to the catalyst solution storage tank for use. The hexafluoropropylene steel cylinder and catalyst solution storage tank are connected with the continuous reactor through a delivery pump. The catalyst solution is pumped in at 20 kg / hour, and hexafluoropropylene gas is fed in, the reaction time is controlled at 30-70 seconds, and the temperature is controlled at 25°C. Adjust the pressure of the hexafluoropropylene inlet to 0.1-0.3MPa; the outlet is connected to the phase separation kettle, the catalyst solution in the upper layer enters the catalyst storage tank for the reaction cycle, the lower layer is the crude product of hexafluoropropylene dimer, and the pure product is obtained by rectification , The yield was 76%.

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PUM

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Abstract

The invention provides a continuous production process of perfluor-2-methyl-3-pentanone. The method specifically comprises the step of carrying out contact with reactants successively by taking hexafluoropropylene as a raw material to obtain a product, wherein the contact means that different materials in a reactor coexist with a time shorter than or equal to 600s. The continuous production process provided by the invention has the advantages of being cheap and easily available in raw material, simple to operate, high in degree of automation, high in synthetic yield, few in byproduct, short inreaction time and the like.

Description

technical field [0001] The invention relates to the field of perfluoro-2-methyl-3-pentanone production, specifically, the invention provides a continuous flow of perfluoro-2-methyl-3-pentanone using hexafluoropropylene gas as raw material Production Process. Background technique [0002] Perfluoro-2-methyl-3-pentanone is a perfluorohexanone halogenated hydrocarbon fire extinguishing agent named Novec1230 introduced by 3M Company of the United States to replace the halon fire extinguishing agent. It is a colorless liquid under normal pressure, which is convenient for storage and transportation; it is easy to gasify and has a high heat capacity, resulting in a low fire extinguishing concentration and excellent fire extinguishing performance; at the same time, it is a green environmental protection material, and the harm to the environment and humans is close to zero; and It has good insulation, has little impact on related sensitive and valuable equipment and materials, has n...

Claims

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Application Information

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IPC IPC(8): C07C45/58C07C49/167
CPCC07C17/281C07C17/358C07C45/58C07D301/03C07D301/12C07D303/48C07C49/167C07C21/18Y02P20/10
Inventor 姜标詹乐武邢萍陈君
Owner SHANGHAI AIMO JINSHAN PHARM CO LTD
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