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A method of preparing trifluorochloroethene through gas-phase catalytic dehydrochlorination

A technology for dehydrochlorination of chlorotrifluoroethylene, which is applied in the direction of dehydrohalogenation preparation, catalyst activation/preparation, chemical instruments and methods, etc., and can solve the problems of low conversion rate, low efficiency and high equipment requirements of trifluorotrichloroethane , to achieve significant social and economic benefits, simple and efficient preparation, and easy industrialization

Active Publication Date: 2017-04-19
福州绿航环保技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions of this method are relatively mild (80~110 ℃), and the operation method is relatively simple and mature, but there are also the following disadvantages: almost all are intermittent operations, the production equipment is huge, and the efficiency is low; the actual amount of zinc powder used is much larger than that of Theoretical amount (usually 113 to 115 times the theoretical amount); a large amount of methanol or ethanol solvent must be consumed; the amount of by-product zinc chloride is large and difficult to handle, resulting in environmental pollution; a small amount of by-product trifluoroethylene, difluoroethylene, Chlorodifluoroethylene, etc. are difficult to collect and separate; the production cost is high
The disadvantage is that the conversion rate of trifluorotrichloroethane is too low, so that the energy consumption of the process is high, and the reaction conditions have higher requirements than catalytic hydrogenation
Catalyst active components use expensive palladium chloride and platinum chloride, the cost is high
Due to the presence of H in the system 2 , Cl 2 etc., the equipment requirements are high, and it is difficult to prolong the service life of the catalyst

Method used

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Examples

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Effect test

preparation example Construction

[0024] 2. The method for preparing chlorotrifluoroethylene provided by the present invention adopts relatively cheap activated carbon as a catalyst, and the cost is low, and the preparation is simple and efficient.

[0025] 3. The method for preparing chlorotrifluoroethylene provided by the present invention overcomes the disadvantages of long operation period and low yield per unit volume of the existing process, and achieves the goals of high yield, few steps and easy industrialization. The invention can realize the production of high-purity chlorotrifluoroethylene through the selection of reactants and the control of reaction conditions.

[0026] Further, vaporize 1,2-dichloro-1,1,2-trifluoroethane with N 2 After entrainment and dilution, enter the reactor to react with nitrogen-containing activated carbon catalyst, in molar ratio, N 2 : 1,2-dichloro-1,1,2-trifluoroethane=1:1~9.

[0027] The nitrogen-containing activated carbon catalyst used in the method of the present i...

Embodiment 1

[0039] Prepare 4.0mol / L HNO 3 Solution 50mL, then weigh the specific surface area to be 810m 2 Put 12g of coconut shell activated carbon per g into a round bottom flask, pour the prepared nitric acid into it, reflux in a water bath at 60°C for 5 hours, then wash it with distilled water for 8 hours at the same temperature, place the coconut shell activated carbon in a vacuum oven, Dry at 110°C for 6 hours and take it out.

[0040] Then the treated activated carbon was used as a catalyst to catalyze the dehydrochlorination of 1,2-dichloro-1,1,2-trifluoroethane to prepare chlorotrifluoroethylene. The reaction is carried out in a plug-flow tubular reactor. The reaction tube of the tubular reactor adopts a Ni tube with an inner diameter of 12mm and a length of 50cm, and is placed in a tube furnace to heat up. In order to prevent the condensation of the material, all reactions are connected The pipeline is made of stainless steel pipe, and the temperature is kept at about 80°C wit...

Embodiment 2

[0042] Prepare 2.0mol / L HNO 3 Solution 50mL, then weigh the specific surface area as 650m 2 Put 12g of coconut shell activated carbon per gram into a round bottom flask, pour the prepared nitric acid into it, reflux in a water bath at 90°C for 3 hours, then wash with distilled water for 8 hours at the same temperature, place the coconut shell activated carbon in a vacuum oven, Dry at 110°C for 6h and take it out.

[0043] Dissolve 2 g of aniline in a hydrochloric acid solution with a concentration of 1.0 mol / L, stir magnetically to disperse the aniline evenly, then add the above-mentioned activated carbon into the solution, and continue stirring for 1 h. Dissolve ammonium persulfate in hydrochloric acid solution with a concentration of 1.0 mol / L, and cool the solution to 0°C in an ice-water mixed bath. The activated carbon-containing aniline solution (ie, mixed solution A) was cooled to 0°C, and at the same time, the ammonium persulfate solution (ie, mixed solution B) was sl...

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Abstract

The invention relates to a method of preparing trifluorochloroethene through gas-phase catalytic dehydrochlorination. 1,2-dichloro-1,1,2-trifluoroethane after being vaporized reacts with existence of a nitrogen-containing activated carbon catalyst under atmospheric pressure at 400-650 DEG C, and a reaction product is collected and subjected to quenching, washing with water, drying, compression and rectification purification to obtain a high-purity trifluorochloroethene product. The nitrogen-containing activated carbon catalyst is activated carbon modified with aniline, and is prepared by activated carbon pretreatment, modification with aniline and auxiliary agent loading. The activated carbon which is cheap is adopted as the catalyst, and is low in cost, simple, convenient and efficient in preparation and good in catalytic performance. The method has advantages of a simple process, easily available raw materials, easy industrialization and environment protection.

Description

technical field [0001] The invention belongs to the technical field of fluorochloroalkene preparation, and specifically relates to a method for preparing chlorotrifluoroethylene by gas-phase catalytic dehydrochlorination. Background technique [0002] Chlorotrifluoroethylene is one of the important monomers for the synthesis of fluorine-containing materials. Through its homopolymerization or copolymerization, a series of fluororesins, fluororubbers, fluorine coatings and chlorofluorocarbon lubricating oils can be prepared. Because these fluorine-containing materials have excellent chemical inertness and high and low temperature resistance, they have attracted widespread attention. [0003] The reductive dechlorination method of trifluorotrichloroethane metal zinc powder is a commonly used method for the preparation of chlorotrifluoroethylene in industry. Utilizing the dechlorination function of Zn, one molecule of zinc must be consumed for every two chlorine atoms removed f...

Claims

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Application Information

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IPC IPC(8): C07C17/25C07C21/18B01J27/24B01J35/10B01J37/08
CPCC07C17/25B01J27/24B01J37/082B01J35/617C07C21/18
Inventor 陈岩飞王聪海肖晓明
Owner 福州绿航环保技术服务有限公司
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