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A kind of preparation method of perfluoro-2-methyl-3-pentanone

A technology of methyl and pentanone, applied in the field of preparation of perfluoro-2-methyl-3-pentanone, can solve the problems of low production efficiency, high cost, environmental pollution, etc., achieve low cost, few reaction steps, Simple effect of product separation and purification

Active Publication Date: 2017-08-01
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

[0007] The existing technologies for preparing perfluoro-2-methyl-3-pentanone from perfluoro-2-methyl-2-pentene through epoxidation and isomerization inevitably require a large amount of acetonitrile Toxic solvents such as corrosive and irritating NaClO and other oxidants have the disadvantages of low production efficiency, high cost, and environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] One-step Catalytic Oxidation of Perfluoro-2-methyl-2-pentene to Perfluoro-2-methyl-3-pentanone by Supporting KF and RbF on Activated Carbon

[0034] (i) Pretreatment of activated carbon support

[0035] Prepare 4.6 mol / L of HNO 3 solution 50 mL, then weighed 10 g of coconut shell activated carbon and put it into a round bottom flask, poured the prepared nitric acid into it, refluxed it in a water bath at 90°C for 5 hours, then washed it with distilled water for 8 hours at the same temperature, and put 10 g of coconut shell activated carbon Place in a vacuum oven, dry at 110°C for 6 h, and take it out;

[0036] (ii) Catalyst preparation by isometric impregnation method

[0037] Add 12 mL of the prepared mixture containing 1 g of potassium fluoride and 0.5 g of rubidium fluoride dropwise onto activated carbon under stirring, let it stand for 24 h, dry at 110 °C for 8 h, and then roast at 550 °C for 3 h in a nitrogen atmosphere to obtain the catalyst RbF-KF / AC;

[0038...

Embodiment 2

[0041] One-step Catalytic Oxidation of Perfluoro-2-methyl-2-pentene to Perfluoro-2-methyl-3-pentanone by Supporting KF and RbF on Activated Carbon

[0042] The implementation steps are the same as in Example 1, except that the catalytic reaction temperature in step (iii) is changed to 250°C, and the reaction pressure is 0.7MPa. After the reaction, the gas is received by condensation and measured and analyzed. The conversion rate of -pentene was 76.7%, and the selectivity of perfluoro-2-methyl-3-pentanone was 59.1%.

Embodiment 3

[0044] La 2 o 3 Preparation of Perfluoro-2-methyl-3-pentanone by Promoted RbF-KF / AC Catalyst

[0045] (i) Catalyst preparation

[0046] First prepare the RbF-KF / AC catalyst according to Example 1, weigh 1.06g of lanthanum nitrate, dissolve it in 12mL of distilled water, add the lanthanum nitrate solution dropwise to the Rb-KF / AC catalyst under stirring, and dry at 110°C for 8h , and then calcined at 550°C for 3h in a nitrogen atmosphere to obtain La 2 o 3 -RbF-KF / AC catalyst;

[0047] (ii) Catalytic reaction

[0048] The catalytic reaction process is the same as step (iii) of Example 1. The results show that the conversion rate of perfluoro-2-methyl-2-pentene is 78.5%, and the selectivity of perfluoro-2-methyl-3-pentanone is 81.1% %.

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Abstract

The invention discloses a preparation method of perfluoro-2-methyl-3-pentanone. According to the method, perfluoro-2-methyl-2-amylene is used as a raw material to be subjected to gas-phase reaction with a certain amount of oxidative gas such as oxygen or air in a fixed bed reactor under the catalyst existence condition; the perfluoro-2-methyl-3-pentanone is directly prepared through one-step or two-step gas-phase reaction, wherein the two-step gas-phase reaction mainly includes perfluoro-2-methyl-2-amylene epoxidation reaction and epoxidation compound gas-phase isomerization reaction. By using the technology, the fixed bed reactor process is used for continuously performing the gas-phase reaction; solvents are not needed in the production process; the cost is greatly reduced; the environment pollution problem is solved; the process safety is improved; meanwhile, the problems of separation of solvents from products, recovery treatment of solvents and catalysts and the like are also avoided. Therefore the preparation method has the characteristics that the cost is low, the preparation is convenient, technical parameters of the catalyst reaction process can be easily controlled, the product separation and purification are simple, the preparation method is very suitable for industrial production and the like.

Description

technical field [0001] The present invention relates to a preparation method of perfluoro-2-methyl-3-pentanone, in particular to a method of combining perfluoro-2-methyl-2-pentene and oxygen and other oxidizing gases under the condition of the presence of a catalyst The preparation method of producing perfluoro-2-methyl-3-pentanone by reaction. Background technique [0002] With the elimination of halon fire extinguishing agents, the main fire extinguishing agents of the new generation mainly include HFC-227ea, FIC-1311, HFC-125, HFC-236 and perfluoro-2-methyl-3-pentanone. Among them, the best environmental protection performance is perfluoro-2-methyl-3-pentanone (the ODP value for ozone layer destruction is 0, and the greenhouse effect GWP value is only 1) and trifluoroiodomethane. However, the cost of trifluoroiodomethane is relatively high (iodine is relatively expensive), and it is difficult to promote it in the market at present. As a halon substitute, perfluoro-2-met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/167C07C45/34C07C45/58
CPCC07C45/34C07C45/58C07D301/08C07C49/167
Inventor 韩文锋王志昆习苗唐浩东
Owner 浙江诺亚氟化工有限公司
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