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Preparation process of perfluoro-2-methyl-3-pentanone

A preparation technology, methyl technology, applied in the field of preparation technology of perfluoro-2-methyl-3-pentanone, to achieve the effect of high efficiency of reaction equipment, easy operation and low equipment requirements

Active Publication Date: 2014-05-14
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this method is that hexafluoropropylene and perfluoropropionyl fluoride are needed as two organic fluorine compound raw materials, especially perfluoropropionyl fluoride is not yet available in commercial products, and supporting production is required

Method used

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  • Preparation process of perfluoro-2-methyl-3-pentanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Synthesis of perfluoro-2-methyl-2,3-epoxypentane by continuous liquid phase epoxidation

[0038] Follow these steps:

[0039] a. Prefabricate 164.7kg of newly prepared sodium hypochlorite solution with an available chlorine content of 16.98%, add 19.7L of acetonitrile, mix well to make a sodium hypochlorite-acetonitrile solution, and weigh 98.6kg (0.329kmol) of 97.4% perfluoro-2- Methyl-2-pentene, the perfluoro-2-methyl-2-pentene of the present invention is obtained by telomerization and isomerization of hexafluoropropylene by a known method;

[0040] b. After measuring the sodium hypochlorite-acetonitrile solution and perfluoro-2-methyl-2-pentene according to the ratio with a metering pump, cool them to about -10°C through the second heat exchanger and the first heat exchanger respectively After that, it is continuously sent to the mixer for mixing;

[0041] c. The mixed reaction materials in the mixer are continuously sent into a pipeline-type liquid phas...

Embodiment 2

[0047] The continuous liquid phase epoxidation method synthesizes perfluoro-2-methyl-2,3-epoxypentane according to the following steps:

[0048] The method operation identical with embodiment 1, difference is that sodium hypochlorite quality is 163.3kg, and available chlorine content is 17.11%, and acetonitrile consumption is 19.7L, and perfluoro-2-methyl-2-pentene consumption is 98.6kg (0.329 kmol) content is 98.21%, and the reaction temperature is 0°C.

[0049] Results: The quality of the crude epoxide was 99.2kg (0.314kmol), the content was 97.83%, and the yield was 95.14%.

Embodiment 3

[0051] The continuous liquid phase epoxidation method synthesizes perfluoro-2-methyl-2,3-epoxypentane according to the following steps:

[0052] The same method operation as in Example 1, the difference is that the quality of sodium hypochlorite is 164.6kg, the available chlorine content is 18.03%, the amount of diethylene glycol dimethyl ether is 22.6L, perfluoro-2-methyl-2-pentene The dosage is 113.3kg (0.329kmol) and the content is 98.21%.

[0053] Results: The quality of the crude epoxide was 114.2kg (0.356kmol), the content was 97.62%, and the yield was 95.12%.

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Abstract

The invention discloses a preparation process of perfluoro-2-methyl-3-pentanone, belonging to the technical field of preparation methods of perfluoroketone compounds in the field of organofluorine chemistry. The perfluoro-2-methyl-3-pentanone is obtained by performing an epoxidation reaction and a catalytic isomerization reaction on perfluoro-2-methyl-pentene serving as a raw material in sequence. The preparation process comprises the following steps: I, in a continuous liquid phase epoxidation reaction, mixing a corresponding proportion of aprotic polar solvent into a sodium hypochlorite solution to promote the reaction, increase the raw material conversion ratio and increase the reaction rate at least by 2-3 percent, wherein the step is characterized by easiness and convenience in operation, low equipment requirement and high reaction equipment efficiency; II, performing a continuous gas phase catalytic reaction, wherein the application of a solvent is effectively avoided, the cost and environmental pollution are lowered, the problems of the need of separating the solvent from a product in post-treatment, difficulty in recycling and treating the solvent and a catalyst, and the like are solved, and the product can be refined and purified more easily. The preparation process has the advantages of high process automation degree, easiness and convenience in operation, high product purity and high reaction equipment efficiency, and is suitable for industrial application.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of perfluoroketones in the field of organic fluorine chemistry, and in particular relates to a preparation process of perfluoro-2-methyl-3-pentanone. Background technique [0002] Perfluoro-2-methyl-3-pentanone (Perfluoro-2-methyl-3-pentanone), also known as FK-5-1-12, is a perfluoroketone compound with a boiling point of 49°C and a normal temperature and pressure Below is a colorless liquid. It has the characteristics of low boiling point, high volatility, low toxicity, non-combustibility, easy storage and transportation, excellent use performance and good environmental protection performance. As a fire extinguishing agent, it has the characteristics of easy vaporization, strong heat absorption capacity and excellent fire extinguishing performance. It is a clean substitute for halon fire extinguishing agent; and because of its good insulation performance, it is not classified as dang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/167C07C45/58C07D303/48C07D301/03
CPCC07C45/58C07D301/03C07D303/48C07C49/167
Inventor 张元塔周孝瑞张招福鲁迪陶杨
Owner 浙江诺亚氟化工有限公司
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