Fluorination catalyst, and preparation method and use thereof

A fluorination catalyst, catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the difficulty of increasing the complexity and repeatability of the impregnation method, Fluorination catalysts have problems such as low operating temperature and harsh operating temperature requirements to achieve the effects of inhibiting carbon deposition, improving catalytic activity, and large pore volume.

Active Publication Date: 2015-09-16
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN1192995C has reported a kind of fluorination catalyst, adopts impregnation method to Cr(NO 3 ) 3 Loaded on activated carbon, obtained by drying, roasting, and hydrogen fluoride activation, at 330 ° C, it is used to catalyze the fluorine-chlorine exchange reaction between 1,2-dichlorohexafluorocyclopentene and hydrogen fluoride to prepare 1-chloroheptafluorocyclopentene. The catalytic activity is very low, the conversion rate is only 26%, and the selectivity is 91%
In addition, the fluorination catalyst is prepared by an impregnation method. Since the impregnation method includes a complex adsorption process of the active components and a redistribution process of the active components during drying, these processes increase the process complexity and the difficulty of repeatability of the impregnation method, and Activated carbon-supported catalysts have strict requirements on the operating temperature, generally not exceeding 300 ° C, if the temperature is too high, such as 330 ° C and above, it is easy to collapse the pore structure of the activated carbon, thereby deactivating the catalyst quickly
Therefore, the fluorination catalysts reported in the above literature have the defects of low service temperature, low catalytic activity and short service life.

Method used

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  • Fluorination catalyst, and preparation method and use thereof
  • Fluorination catalyst, and preparation method and use thereof
  • Fluorination catalyst, and preparation method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Dissolve chromium nitrate in water, add precipitant ammonia water at 60°C, control the pH range of the solution to 7.5-8.5, make it fully precipitate under stirring conditions, filter the formed slurry, wash with deionized water until neutral , and then dried at 150°C for 12 hours to obtain chromium hydroxide.

[0030] The obtained chromium hydroxide and zinc tungstate were divided into 60% and 40% by mass percentage, uniformly mixed, and pressed into tablets to obtain a catalyst precursor, and 60 mL of the catalyst precursor was loaded into a SUS316 glass with an inner diameter of 1 inch and a length of 23.6 inches. Tubular reactor, fed with nitrogen and roasted at 450°C for 8 hours, nitrogen space velocity is 200h -1 , and then lower the temperature to 300°C, and at the same time pass a mixed gas composed of hydrogen fluoride and hydrogen with a mass ratio of 10:1, and the total space velocity of the gas is 220h -1 , activate for 12 hours, stop the above mixed gas, a...

Embodiment 2

[0033] The preparation process of the catalyst is basically the same as in Example 1, except that the mass percentages of chromium hydroxide and zinc tungstate are 95% and 5%.

[0034] The specific surface area of ​​the catalyst was determined by BET low temperature nitrogen adsorption method = 174.4m 2 / g, pore volume=0.46cc / g, average pore diameter 52.8

Embodiment 3

[0036] The catalyst preparation process is basically the same as in Example 1, except that the mass percentages of chromium hydroxide and zinc tungstate are 40% and 60%.

[0037] The specific surface area of ​​the catalyst was determined by BET low temperature nitrogen adsorption method = 184.8m 2 / g, pore volume=0.58mL / g, average pore diameter 62.8

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Abstract

The invention discloses a fluorination catalyst, and a preparation method and a use thereof, and belongs to the field of chemical synthesis. The precursor of the catalyst is formed by blending 40-95mass% of a trivalent chromium compound with 5-60mass% of tungstate, wherein the trivalent chromium compound can be chromic oxide or chromium hydroxide, and the tungstate can be zinc tungstate, nickel tungstate, magnesium tungstate, aluminum tungstate, silicotungstic acid, ammonium tungstate, ammonium paratungstate or ammonium metatungstate. The fluorination catalyst has the advantages of high use temperature, high catalysis activity and long service life, and can be mainly used in reactions for preparing fluorinated alkenes through gas phase catalysis of fluorination of alkenyl halides at a high temperature.

Description

technical field [0001] The invention relates to a fluorination catalyst, in particular to gas-phase catalytic fluorination of halogenated olefins at high temperature to prepare fluorine-containing olefins. Background technique [0002] Generally, the industrial production of fluorine-containing olefins mostly adopts the method of gas-phase fluorination of halogenated olefins. This method has the advantages of simple process, easy continuous large-scale production, and safe operation. Fluorination catalysts play a central role in gas-phase catalytic fluorination of haloalkenes. [0003] Chinese patent CN1192995C has reported a kind of fluorination catalyst, adopts impregnation method to Cr(NO 3 ) 3 Loaded on activated carbon, obtained by drying, roasting, and hydrogen fluoride activation, at 330 ° C, it is used to catalyze the fluorine-chlorine exchange reaction between 1,2-dichlorohexafluorocyclopentene and hydrogen fluoride to prepare 1-chloroheptafluorocyclopentene. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/30B01J23/888B01J27/24C07C17/20C07C23/08C07C21/18
Inventor 张呈平周晓猛陈朝晖权恒道
Owner 泉州宇极新材料科技有限公司
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