Method for preparing trifluoroacetyl chloride

A technology of trifluoroacetyl chloride and chlorine gas, applied in the preparation of acyl halide, organic chemistry and other directions, can solve the problems of poor selectivity, unsafe, difficult separation, etc., and achieve the effect of avoiding corrosion

Active Publication Date: 2010-06-16
福建舜跃科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

US5241113 describes the preparation of TFAC by utilizing activated carbon to catalyze the oxidation of HCFC-123, the higher reaction temperature causes the carbon-carbon bond in some raw materials to break, and the selectivity is poor
US5041647, has described to prepare TFAC by oxidizing HCFC-123, but must use water as catalyzer, also quite harsh to the requirement of stirring in order to prevent local overheating in the reactor, can be accompanied by trifluoroacetic acid (TFAA) when the existence of water generates TFAC ), the separation between TFAC, TFAA and water is also difficult
US5259938 describes the preparation of TFAC by liquid-phase oxidation of HCFC-123, which improv

Method used

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  • Method for preparing trifluoroacetyl chloride
  • Method for preparing trifluoroacetyl chloride

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Experimental program
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Effect test

Embodiment 1

[0028] Add 1L of HCFC-123 into a 1L special three-neck glass flask, and place a set of shading plates below the gas-liquid phase interface. The shading plates are similar to the louver structure, allowing the gas to pass through but preventing the light under the liquid from penetrating into the gas phase space. The middle interface on the top of the flask is the mercury lamp placement port, and the 500w mercury lamp, quartz cold hydrazine, and quartz sleeve are placed in sequence from the inside to the outside, and the sleeve and the interface are sealed. Oxygen and chlorine are fed continuously under magnetic stirring, the flow rate is 75ml / min and 15ml / min respectively, after 15 minutes, the mercury lamp is turned on, and the photochemical oxidation reaction is carried out through the radiation of the mercury lamp, and the reaction is carried out at normal temperature and pressure. The reactant is continuously discharged from the gas phase outlet on the upper part of the rea...

Embodiment 2

[0032] The difference of embodiment 2 reaction and experiment 1 is that no shading plate is added below the gas-liquid phase interface of embodiment 2, and other conditions are the same as experiment 1, and TFAC accounts for 90% except raw material, oxygen, chlorine and hydrogen chloride gas in the gas phase product, altogether 0.94 mol TFAC was produced. The content of HCFC-123 in the bottom solution is 93.14%, and the by-product CFC-113a is 6.81%. Glass corrosion was found at the gas-liquid phase interface of the reactor, the gas phase part, and the condensation return pipe.

Embodiment 3

[0034] The difference between reaction and experiment 1 in embodiment 3 is that the flow of chlorine gas in embodiment 3 is adjusted to 0 after the mercury lamp is turned on, and other conditions are the same as in experiment 1. In the gas phase product, TFAC accounts for 99% except raw materials, oxygen, chlorine and hydrogen chloride gas. %, a total of 0.64mol TFAC was produced. The content of HCFC-123 in the bottom liquid is 98.59%, and the by-product CFC-113a is 1.27%. No corrosion was found in the glass of the reactor, condenser, etc.

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Abstract

The invention discloses a method for preparing trifluoroacetyl chloride (TFAC), comprising the following steps: 1) HCFC-123 is added into a reactor, oxygen and chlorine are continuously introduced while stirring, photochemical oxidation reaction is carried out through mercury lamp radiation, the reactant is continuously exhausted from the upper part of the reactor in the form of gas phase, and the liquid level in the reactor keeps constant by continuously supplementing HCFC-123; and 2) the vaporized HCFC-123 in the reaction is condensed by a condenser installed above the reactor and flows back into the reactor to continue participating in the reaction, the product TFAC is exhausted from the top of the condenser and is collected after compression and condensation, the by-product hydrogen chloride is absorbed by water washing and the unreacted chlorine is processed by alkali washing absorption. In the method, the reactor is required to have gas phase space, a shading component is arranged below the gas-liquid phase interface and the mercury lamp is totally immersed below the shading component, thus effectively preventing the generated TFAC from radiolytic decomposition by the mercury lamp in the gas phase space and avoiding the decomposition products from corroding the glass reactor and the lamp tube.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of trifluoroacetyl chloride. Background technique [0002] The acid chloride group in TFAC can easily react with amines and alcohols to form 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 TFAC. US3883407, has described and is less than 0.1% HCFC-123 preparation TFAC by ultraviolet lamp radiation vapor phase oxidation, this reaction needs just can carry out under certain temperature and pressure, and thinks that this reaction is not suitable for carrying out in liquid phase, because The hydrofluoric acid produced by the side reaction will corrode the UV lamp. US5241113 describes the preparation of TFAC by using activated carbon to catalyze the oxidation of HCFC-123. The higher reaction temperature causes the carbon-car...

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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