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A kind of method for preparing perfluoroisopropyl ethyl ketone

A technology of perfluoroisopropyl ethyl ketone and perfluoropropene, which is applied in the field of fluorine-containing fine chemical synthesis and preparation of perfluoroisopropyl ethyl ketone, which can solve the problems of difficult to obtain raw materials, difficult to realize industrialization, and difficult separation , to achieve mild temperature and pressure conditions, conducive to industrial production, and the effect of simple and easy method

Active Publication Date: 2020-01-10
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The document describes that this method produces more dimers of hexafluoropropylene and perfluoro-3-hexanone, and it is difficult to realize industrialization because the boiling point is close to the separation.
[0012] Zapevalov et al. (Zhurnal Organicheskoi Khimii; vol.22; nb.1; (1986); p.93-99) use perfluorohexane isomerization to obtain perfluoroisopropyl ethyl ketone. High yield, but the perfluoroepoxide itself is difficult to obtain, so the method is very limited
[0013] Rogovik et al. (Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation); vol.39; nb.9.1.; (1990); p.1870-1876;) used a fluorine-containing sulfonic acid through Decompose to obtain perfluoroisopropyl ethyl ketone, the conversion rate of this method is 16%, the yield is 76%, and its raw material is difficult to obtain, so this method is also very limited
[0014] In addition, there are synthetic routes such as the reaction method of perfluorocarboxylate and perfluoroacid anhydride (see patent documents US5466877, US4136121 for details), but there are disadvantages such as difficult availability of reaction raw materials and high cost, and it is difficult to realize industrial production

Method used

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  • A kind of method for preparing perfluoroisopropyl ethyl ketone
  • A kind of method for preparing perfluoroisopropyl ethyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A 125W UV lamp (wavelength of 254nm) irradiation device with a power of 125W is installed on a pressure-resistant jacketed steel reactor with a volume of 2000ml, and the reactor is equipped with a stirring device.

[0031] Strictly dry the reactor, replace the air in the reaction vessel with nitrogen, add 600g of perfluoropropylene HFP, 8g of potassium fluoride and 800g of diglyme to the reactor, raise the temperature and keep the temperature in the reaction vessel at 50°C;

[0032] Turn on the ultraviolet irradiation with a wavelength of 254nm, intermittently feed a total of 40g of oxygen and keep the pressure in the reaction vessel at 1MPa, and fully react for 5 hours;

[0033] The product obtained by the reaction was allowed to stand and separate layers, and the liquid in the lower layer was taken out, and after being washed with alkali and water, 286 g of the product was obtained.

[0034] Detected by gas chromatography, the content of perfluoroisopropyl ethyl keto...

Embodiment 2

[0036] Compared with Example 1, the only difference is: 16g of potassium fluoride is used, and the reaction temperature is 60°C.

Embodiment 3

[0038] Compared with Example 1, the only difference is that 20g of potassium fluoride is used, and the reaction temperature is 70°C.

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Abstract

The invention relates to a method for preparing perfluoro-isopropyl ethyl ketone. The method comprises the step: with perfluoropropylene and oxygen as raw materials and fluoride salt as a catalyst, under the ultraviolet irradiation condition, reacting to obtain perfluoro-isopropyl ethyl ketone. According to the method provided by the invention, a product can be obtained by a one-step reaction, sothat the method is simple, convenient and practicable; and the method is easily available in raw materials, low in cost, few in side reaction and mild in reaction condition, so that the method is beneficial for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to fluorine-containing fine chemical synthesis, and in particular to a method for preparing perfluoroisopropyl ethyl ketone. Background technique [0002] Perfluoroisopropyl ethyl ketone, that is, perfluoro-2-methyl-3-pentanone, has the structural formula: [0003] [0004] It is a colorless transparent liquid at normal temperature and pressure, with a boiling point of 49°C and a freezing point of -108°C. It has a density of 1.6g / mL at 25°C under 1 atmosphere and is immiscible with water. [0005] As a halogenated hydrocarbon, perfluoroisopropyl ethyl ketone has excellent flame retardant properties and also performs well in environmental protection. It meets the requirements of human society for sustainable development and has broad development prospects. [0006] Magnesium alloys are very easy to oxidize and burn during smelting and processing. In order to solve this problem,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/00C07C49/167
CPCC07C45/00C07C49/167
Inventor 张鸣刘波杨旭仓李俊玲李斌陈炯
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD