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Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture

A technology of trifluoroacetyl chloride and trifluoroethane, which is applied in the field of compound preparation, can solve problems such as difficult realization and harsh reactor requirements, and achieve the effects of improving production efficiency, shortening time, and reducing equipment investment and energy consumption.

Active Publication Date: 2010-06-23
福建舜跃科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

US5296640, has described to prepare trifluoroacetyl chloride by oxidizing HCFC-123 under supercritical state, have by-product hydrofluoric acid and TFAA to produce in the reaction, add that the high temperature and high pressure under supercritical state are harsh to reactor, industrially relatively Difficult to achieve

Method used

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  • Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture
  • Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture
  • Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture

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Embodiment 1

[0020] Add 5L of trifluoroethane chlorination mixture into 10L enamel kettle, the mixture is composed of: 90% trifluorochloroethane, 9% trifluorodichloroethane and 1% trifluorotrichloroethane, inside the reactor A 2kW mercury lamp is installed. Continuously feed oxygen and chlorine under stirring, flow rate is 500ml / min and 400ml / min respectively, turn on mercury lamp after 15 minutes, carry out photochemical oxidation reaction by mercury lamp radiation, react at 0.09Mpa, material bubble point temperature (about 5°C). The reactants are continuously discharged from the gas phase outlet on the upper part of the reactor in the form of gas phase, and the liquid level in the reactor is kept constant by continuously adding trifluoroethane chlorination mixture through the dropping funnel, and the supplementary speed is determined by the reaction rate; the continuously discharged reactants include reaction Vaporized trifluoroethane chlorination mixture, product trifluoroacetyl chlori...

Embodiment 2

[0024] The difference of embodiment 2 reaction and embodiment 1 is that the chlorination mixture among the embodiment 2 consists of: 9% trifluorochloroethane, 90% trifluorodichloroethane and 1% trifluorotrichloroethane, The flow rate of chlorine gas is 250ml / min, and the reaction is carried out at 0.31MPa and the bubble point temperature of the material in the reactor (about 60°C). Other conditions were the same as in Experiment 1, except for trifluoroethane chlorination mixture, oxygen, chlorine and hydrogen chloride gas, trifluoroacetyl chloride accounted for 91% of the gas phase products, and a total of 10.3 mol of trifluoroacetyl chloride was generated. The content of trifluorotrichloroethane in the bottom liquid is 7.14%.

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Abstract

The invention discloses a method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture, which comprises the following steps: 1) adding trifluoroethane chlorinated mixture into a reactor, continuously introducing oxygen and chlorine under stirring, irradiating with a mercury lamp for photochemical oxidation, continuously discharging reactants in the form of gas phase from the upper part of the reactor, and continuously supplementing the trifluoroethane chlorinated mixture to maintain the level in the reactor constant; and 2) condensing the gasified trifluoroethane chlorinated mixture in the reactor through a condensation and separation tower and making the condensed trifluoroethane chlorinated mixture return to the reactor to continuously react, discharging the product trifluoro acetyl chloride from the top of the condensation and separation tower and collecting the trifluoro acetyl chloride after compression and condensation. Compared with the existing preparation method, the invention has the advantages that: the trifluoroethane chlorinated mixture can be directly used for preparation of the trifluoro acetyl chloride without separation, the processis advanced and reasonable, the synthesis route is simplified, the time is reduced, the production efficiency is greatly enhanced, and the equipment investment and energy consumption are reduced.

Description

technical field [0001] The present invention relates to a compound preparation method, in particular to a method for preparing trifluoroacetyl chloride from a trifluoroethane chlorination mixture. Background technique [0002] The acid chloride group in trifluoroacetyl chloride can easily react with amines and alcohols to generate amides and esters respectively. It is an important raw material for the synthesis of pesticides and medicines. [0003] Several methods have been disclosed which can be used to prepare trifluoroacetyl chloride. Literature (Haszeldine R.N., Nyman F., "Oxidation of polyhalogeno-compounds.Part II.Photolysis and photochemical oxidation of some chlorofluoroethanes", J.Chem.Soc., 1959, 387-396) introduced the method of oxidizing trifluorodichloroethylene Alkanes and trifluoro-chloroethane to prepare trifluoroacetyl chloride, they have high requirements on the purity of raw materials, and the industrial production cost is high. US3883407 describes the p...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/58
Inventor 赵建明韩箴贤崔觉剑
Owner 福建舜跃科技股份有限公司
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