Preparation method of hexafluoropropylene oxide

A technology of hexafluoropropylene oxide and hexafluoropropylene, which is applied in the field of gas-phase oxidation to prepare hexafluoropropylene oxide, can solve the problems of high reaction temperature, low conversion rate, and inaccessibility, and achieve low reaction temperature and fast reaction speed , the effect of less solvent consumption

Inactive Publication Date: 2015-04-29
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high reaction temperature, high energy consumption, low conversion rate, and when there is no copper, the catalytic oxidation will not obtain the target product HFPO

Method used

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  • Preparation method of hexafluoropropylene oxide
  • Preparation method of hexafluoropropylene oxide
  • Preparation method of hexafluoropropylene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] will (HFPO) x Add it to a 1L dry autoclave, seal the autoclave and evacuate it with a vacuum pump for 30 minutes to remove impurity gases. Then inject HFP into the reactor, and maintain the stirring speed at 350rpm. Raise the temperature of the stirred tank body to 90°C~160°C, maintain it for 0.5h~1h until the temperature is stable, and then add oxygen, the oxygen partial pressure ΔP O2 =0.2MPa. After reacting for a certain period of time, the HFP conversion rate and the selectivity of the target product HFPO were detected, and the results are listed in Table 1.

Embodiment 2-8

[0030] Change (HFPO) x Type and consumption, HFP and oxygen consumption, reaction temperature, reaction time etc., all the other are identical with embodiment 1. After reacting for a certain period of time, the HFP conversion rate and the selectivity of the target product HFPO were detected, and the results are listed in Table 1.

[0031] (HFPO) used in Examples 7-8 x Among them, the mass content ratio of dimers, trimers, tetramers and pentamers is about 1:3:3:1.

[0032] Table 1

[0033]

[0034] As can be seen from Table 1, using (HFPO) x When used as a solvent for HFP epoxidation, the epoxidation reaction can proceed stably, and the conversion rate of HFP in a single oxygen (0.2MPa) reaction is between 9.2% and 38.4% (relative to HFP. Due to the constant oxygen flow, the conversion rate Depending on the amount of HFP added), the selectivity of the target product HFPO is located at 69.9%-73.3%. Show (HFPO) x It is an ideal reaction solvent.

Embodiment 9

[0036] will (HFPO) 2 Add it to a 1L dry autoclave, seal the autoclave and evacuate it with a vacuum pump for 30 minutes to remove impurity gases. Then, 100 g of HFP was injected into the reactor, and the stirring speed was maintained at 350 rpm. Raise the temperature of the stirred tank to 130°C and maintain it for 0.5h to 1h until the temperature is stable, then add oxygen in 6 times, each time the oxygen partial pressure ΔP O2 =0.2MPa. After reacting for a certain period of time, the conversion rate of HFP and the selectivity of the target product HFPO were detected after each addition of oxygen.

[0037] The total reaction time of this reaction was 5.16h, the final conversion rate of HFP reached 100%, and the selectivity of the target product HFPO was 72.1%.

[0038] Table 2

[0039] Oxygen addition times

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Abstract

The invention provides a preparation method of hexafluoropropylene oxide. The preparation method comprises the step of carrying out gas phase oxidation on hexafluoropropylene and oxygen by utilizing CF3CF2CF2O[CF(CF3)CF2O][n-1]CF(CF3)COF as a reaction solvent, so as to prepare hexafluoropropylene oxide, wherein n is an integer from 1 to 5. According to the preparation method provided by the invention, an oxidative burst problem can be solved, the high selectivity of an epoxidation reaction is maintained, the reaction can be continuously and stably carried out, and therefore, the high-yield hexafluoropropylene oxide is obtained.

Description

technical field [0001] The invention relates to a production method of hexafluoropropylene oxide, in particular to a method for preparing hexafluoropropylene oxide by gas phase oxidation. Background technique [0002] Hexafluoropropylene oxide (HFPO for short) is an important basic raw material for fluorine chemical industry. React with various nucleophiles. Hexafluoropropylene oxide can be used to produce important organic fluorine products such as hexafluoroacetone and hexafluoroisopropanol, and can also be used to prepare perfluorinated ion exchange membranes (or resins) and important monomers of perfluoropolyether. Used in the preparation of the pharmaceutical anesthetic sevoflurane. [0003] The preparation of hexafluoropropylene oxide includes gas-phase oxidation and liquid-phase oxidation, among which the liquid-phase oxidation method has industrial application value. [0004] The liquid-phase oxidation method is to disperse HFP and oxygen in a suitable solvent by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/06
CPCC07D303/48C07D301/08
Inventor 黄挺秀魏作君韩国庆徐卫国方小青陈先进汪梨超任其龙陈丰秋杨亦文
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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