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Method for synthesizing C11 perfluoro-ketone

A technology of perfluoroketone and potassium fluoride, which is applied in the field of synthesizing C11 perfluoroketone, can solve the problems of low yield, high reaction temperature, and long reaction time, and achieve high reaction yield, simple operation, and fast reaction speed Effect

Inactive Publication Date: 2016-04-20
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] This method has a high reaction temperature and a long reaction time, and waste solids and waste gas are generated. The solids are corrosive to equipment and the yield is low.

Method used

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  • Method for synthesizing C11 perfluoro-ketone
  • Method for synthesizing C11 perfluoro-ketone

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A method for synthesizing C11 perfluoroketone: Perfluoro-n-propyl vinyl ether (PPVE) 106g, hexafluoropropylene oxide dimer 144g, cesium fluoride 12g and diethylene glycol dimethyl ether 260mL are added to In a 1L reactor, raise the temperature to 95°C, stir and react for 2 hours, observe that the reaction pressure does not change, lower the temperature, open the reactor, separate the lower layer liquid and obtain 205g of product C11 perfluoroketone by conventional distillation with a yield of 86%.

[0025] Among them, the method for synthesizing perfluoro-n-propyl vinyl ether can be: using hexafluoropropylene oxide as a raw material to carry out self-dimerization (the actual reaction is two steps, and perfluoro-n-propyl vinyl ether is first isomerized to generate CF 3 CF 2 CFO, which can undergo a telomerization reaction with hexafluoropropylene oxide in one step, and the two-step reaction can be combined in the same reactor) to generate an acyl fluoride intermediate, w...

Embodiment 2

[0028] On the basis of Example 1, carry out scale-up production test: with perfluoro-n-propyl vinyl ether (PPVE) 1kg, hexafluoropropylene oxide dimer 1.5kg, cesium fluoride 120g and diglyme Add 2.6L into a 10L reactor, raise the temperature to 95°C, stir and react for 2 hours, observe that the reaction pressure does not change, lower the temperature, open the reactor, separate the lower layer liquid and distill to obtain the product C11 perfluoroketone 1.95kg, the yield is 87 %.

[0029] Facts have proved that using the method for synthesizing C11 perfluoroketones of the present invention, the product yield is greater than 80%, and the raw materials are easy to prepare, the reaction yield is improved, the operation is simple, easy to purify, and can be scaled up for production. Social value and economic value.

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Abstract

The invention discloses a method for synthesizing C11 perfluoro-ketone. The method is characterized by taking a hexafluoropropylene oxide (HFPO) dimer and perfluoro-n-propyl vinyl ether (PPVE) as starting materials, taking potassium fluoride or cesium fluoride as a catalyst under suitable reaction conditions and obtaining C11 perfluoro-ketone through one-step reaction under the condition of catalysis. The method for synthesizing C11 perfluoro-ketone has the beneficial effects that by utilizing the method, the product yield is more than 80%; the raw materials are easy to prepare, the reaction yield is increased, and the method is easy to operate, is easy in purification, can be used for carrying out large scale production and has high social and economic values; researches find that the final product is obtained through one-step reaction by using the HFPO dimer and PPVE as starting reactants; the reaction temperature is lower, the reaction speed is high and the reaction yield is higher, so that large scale production of the compound is easy to achieve.

Description

technical field [0001] The invention relates to a method for synthesizing C11 perfluoroketone, belonging to fluorine-containing fine chemicals. Background technique [0002] High boiling C11 perfluoroketone (1,1,1,2,4,5,5,5-octafluoro-2,4-bis(1,1,2,2,3,3,3-heptafluoropropane Oxygen) 3-pentanone) is an important cleaning agent, which has the characteristics of high boiling point, low volatility, heat resistance, corrosion resistance, etc., and can be used in the manufacture and cleaning of cutting-edge instruments and equipment. [0003] Through research, it is found that the only method for synthesizing the C11 perfluoroketone is US Patent No. 4136121, and the method has disadvantages such as difficult raw material preparation, long reaction time, low reaction yield, etc., so that there are very few manufacturers of this perfluoroketone, and the price is expensive. Seriously hinder the application of this product. [0004] So far, there is only one method for synthesizing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/175
Inventor 张志君赵兴华徐雅硕王博肖山
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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