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Method for continuous production of hexafluoroacetone

A technology of hexafluoroacetone and hexafluoropropylene, which is applied in the field of continuous production of hexafluoroacetone, can solve the problems of difficult control of the reaction process, low conversion rate and selectivity, and influence on product quality, so as to avoid overheating, improve selectivity and The effect of conversion rate and excellent mass transfer effect

Active Publication Date: 2022-03-29
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to make up for the existing one-step method for preparing hexafluoroacetone, which has low conversion rate and selectivity, affects product quality, low catalyst activity, complicated preparation process, and difficult control of the reaction process, and provides a continuous production of hexafluoroacetone. Method, the process utilizes the circulation loop reactor, the mixing effect of gas, liquid and solid, adopts the selection of suitable solvent and catalyst to improve the conversion rate of hexafluoropropylene oxidation and the selectivity of hexafluoroacetone, and at the same time reduces the temperature of reaction, realizing the ideal Effect

Method used

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  • Method for continuous production of hexafluoroacetone

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Effect test

Embodiment 1

[0038] AlCl 3Prepare a suspension with hydrofluoroether at a mass ratio of 1:50, heat the suspension through a heat exchanger to a reaction temperature of 60°C, pump it into a circulating loop reactor, and mix oxygen and hexafluoropropylene at a mass ratio of 5:1 Configure the mixed gas, pass the mixed gas into the reactor through the compressor, the mass ratio of the mixed gas and the catalyst suspension is 1:30, the reaction temperature is controlled at 50°C, the injection speed of the Venturi mixer is 70m / s, and the reaction stays The time is 5 minutes, the gas part is extracted, and the finished product of hexafluoroacetone is obtained after low-temperature rectification. The reaction conversion rate and selectivity are respectively 98.20% and 99.45% through gas chromatography detection. After 5 cycles of the reaction solution, the reaction conversion rate and selectivity sex were 97.02%, 98.86%.

Embodiment 2

[0040] AlCl 3 , KF and hydrofluoroether to prepare a suspension according to the mass ratio of 1:1:100, heat the suspension through a heat exchanger to a reaction temperature of 60°C, pump it into a circulating loop reactor, and mix oxygen and hexafluoropropylene by mass The mixed gas is configured at a ratio of 3:1, and the mixed gas is fed into the reactor through the compressor. The mass ratio of the mixed gas and the catalyst suspension is 1:20, the reaction temperature is controlled at 60°C, and the injection speed of the Venturi mixer is 70m / s, the reaction residence time is 3min, the gas part is taken out, and the finished product of hexafluoroacetone is obtained after low-temperature rectification. The reaction conversion rate and selectivity are respectively 98.90% and 99.03% through gas chromatography detection. After 8 cycles of the reaction solution, the reaction The conversion and selectivity were 97.38% and 98.93%, respectively.

Embodiment 3

[0042] AlCl 3 , AgI and fluorocarbon according to the mass ratio of 1:1:300 to prepare a suspension, heat the suspension through a heat exchanger to a reaction temperature of 60°C, pump it into the circulation loop reactor, and mix oxygen and hexafluoropropylene according to the mass ratio The mixed gas is configured at 1:1, and the mixed gas is fed into the reactor through the compressor. The mass ratio of the mixed gas and the catalyst suspension is 1:10, the reaction temperature is controlled at 60°C, and the injection speed of the Venturi mixer is 50m / s , the reaction residence time is 5min, the gas part is produced, and the finished product of hexafluoroacetone is obtained after low-temperature rectification. The reaction conversion rate and selectivity are respectively 98.63% and 99.52% through gas chromatography detection. After 6 cycles of the reaction solution, the reaction conversion The rate and selectivity were 97.68% and 99.03%, respectively.

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Abstract

The invention belongs to the field of synthesis of fluorine-containing fine chemicals, and in particular relates to a method for continuously producing hexafluoroacetone. The method uses oxygen and hexafluoropropylene as raw materials, selects a suitable organic solvent, and uses a circulation loop reactor to carry out a liquid phase oxidation reaction in the presence of a catalyst, the catalyst being AlCl 3 , CrCl 3 , AgI, KF, AlF 3 、Cr 2 o 3 One or two of them, and the organic solvent is one of HFE, fluorocarbon, HFP oligomer or perfluoropolyether oil. The method improves the mass transfer effect of the heterogeneous reaction, realizes the one-step preparation of hexafluoroacetone from hexafluoropropylene, improves the conversion rate and selectivity of the conversion of hexafluoropropylene into hexafluoroacetone, and avoids the reaction caused by the exothermic reaction. The phenomenon of rapid temperature rise improves the safety of catalytic oxidation reaction. It is a new process with fast reaction rate, environmental friendliness and easy industrialization.

Description

technical field [0001] The invention belongs to the field of synthesis of fluorine-containing fine chemicals, and in particular relates to a method for continuously producing hexafluoroacetone. Background technique [0002] Hexafluoroacetone (hexafluoroacetone, referred to as HFA), structural formula CF 3 COCF 3 , is an important organic fluorine raw material, widely used in the fields of medicine, pesticides and synthetic materials, especially as a raw material for special polymer materials, has extraordinary value, for example, hexafluoroisopropanol synthesized by hydrogenation reduction, is a A safe high-grade solvent and a monomer for high-performance fluoroelastomers. Bisphenol AF prepared from hexafluoroacetone is an important fluororubber crosslinking agent. In addition, companies such as DuPont in the United States and Daikin in Japan have synthesized many valuable chemical products through hexafluoroacetone: 6FDA, a fluorine-containing polyimide monomer widely us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/34C07C49/167
CPCC07C45/34C07C49/167
Inventor 王磊刘添王汉利
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL