Method for preparing C11 perfluoroketone

A technology of perfluoroketone and perfluoropropionyl fluoride, which is applied in the field of preparing C11 perfluoroketone, can solve problems such as difficulties and increased production costs, and achieve the effects of short reaction time, fast reaction speed and convenient purification

Inactive Publication Date: 2017-05-10
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As shown in the patent CN201511028330.2, hexafluoropropylene oxide (HFPO) dimer is an important organic fluorine intermediate, which can be used to synthesize important organic fluorine products such as perfluoro-n-propyl vinyl ether and surfactants , but in the process of synthesizing HFPO dimer, a large amount of HFPO trimer is usually produced. This by-product has high toxicity, but the harmless treatment of it by conventional waste treatment will cause a substantial increase in production costs , so it is best to be able to recycle it and develop high value-added derivative products. This recycling process is a relatively difficult link in the entire production process. At present, there is no mature and feasible solution at home and abroad.

Method used

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  • Method for preparing C11 perfluoroketone
  • Method for preparing C11 perfluoroketone

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Experimental program
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Effect test

Embodiment 1

[0013] Embodiment 1, a method for preparing C11 perfluoroketone, the specific steps of the preparation method are as follows: 144g of hexafluoropropylene oxide trimer, potassium carbonate (44g) and diglyme (260mL) were added to 1L In the reaction kettle, stirred and reacted at 0°C for 2 hours, then introduced PPF (62g), raised the temperature to 95°C, stirred and reacted for 2 hours, observed that the reaction pressure did not change, lowered the temperature, opened the reaction kettle, separated the lower layer liquid and distilled to obtain The yield of product C11 perfluoroketone (149g) was 86%.

Embodiment 2

[0014] Embodiment 2, a kind of method for preparing C11 perfluoroketone, the concrete steps of preparation method are as follows: Hexafluoropropylene oxide trimer (1000g), cesium carbonate (687g) and acetonitrile (2.6L) are added in 10L reactor , stirred and reacted at 0°C for 2 hours, then introduced PPF (417g), raised the temperature to 115°C, stirred and reacted for 3 hours, observed that the reaction pressure did not change, lowered the temperature, opened the reaction kettle, separated the lower layer and distilled to obtain the product C11 Fluoroketone (1069g), yield 89%.

[0015] The invention simplifies the environmental protection treatment process, the raw materials are easy to obtain, the reaction yield is improved, the operation is simple, the purification is easy, and the scale-up production can be carried out. Hexafluoropropylene oxide trimer, perfluoropropionyl fluoride (PPF) As the starting reactant, the final product is obtained through one-step reaction, the ...

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Abstract

The invention discloses a method for preparing C11 perfluoroketone. The preparation method comprises the following specific steps: adding a hexafluoropropylene oxide trimer, a reaction solvent and basic salts into a reaction kettle, and carrying out stirring reaction at the temperature of 0DEG C for 1 to 2 hours; then introducing perfluorodipropionyl peroxides, raising the temperature to 75 to 155DEG C, and carrying out stirring reaction for 1 to 8 hours; cooling after reaction pressure has no change, opening the reaction kettle, separating out subnatant and distilling to obtain a product C11 perfluoroketone. According to the method disclosed by the invention, an environment-friendly treatment process is simplified, raw materials are easily obtained, the reaction yield is increased, simple operation and easiness in purification are realized, and enlarged production can be performed; the hexafluoropropylene oxide trimer, the perfluorodipropionyl peroxides and the basic salts are used as initial reactants; the initial reactants are subjected to one-step reaction to obtain a finished product; the reaction temperature is lower, the reaction speed is high, and the reaction yield is higher, so that the enlargement of the compound is easily realized.

Description

technical field [0001] The invention relates to the field of fluorine-containing fine chemicals, in particular to a method for preparing C11 perfluoroketone. 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 and corrosion resistance. It is an important cleaning agent and can be widely used in the manufacture and cleaning of cutting-edge instruments and equipment . [0003] The preparation method of C11 perfluoroketone usually adopts hexafluoropropylene oxide dimer and perfluoron-propyl vinyl ether as starting raw materials, and under suitable reaction conditions, potassium fluoride or cesium fluoride is used as catalyst to catalyze After one step reaction, C11 perfluoroketone is obtained. As shown in the patent CN201511028330.2, hexafluoropropylene oxide (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/175C07C45/45
CPCC07C45/455C07C49/175
Inventor 张志君徐雅硕王博肖鑫冀汝南于颖
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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