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Preparation method of fluorination catalyst

A fluorination catalyst and catalyst technology, which can be used in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., and can solve problems such as unseen pore structures.

Inactive Publication Date: 2015-09-09
JIANGSU SANMEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Many patent documents have mentioned that higher specific surface area is beneficial to improve the activity of catalyst, but there is no research on the pore structure related to specific surface area

Method used

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  • Preparation method of fluorination catalyst
  • Preparation method of fluorination catalyst

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Experimental program
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Embodiment 1

[0021] Mix cobalt and chromium metal salts according to the atomic ratio of 0.05:1 to prepare a solution, use ammonia water as a precipitant for precipitation reaction, pH is 7, and continue to stir and age for 9 minutes, then filter, wash with deionized water until neutral, filter The cake was dried at a temperature of 110°C, and finally roasted at a temperature of 350°C in an inert gas environment to prepare a catalyst precursor. The catalyst precursor was crushed and mixed with 2% graphite, and the uniformly mixed powder was pressed The tablet is not broken by hand, and at a temperature of 200°C, the mixed gas of inert gas and hydrogen fluoride is passed through for fluorination to prepare the required catalyst. The pore structure of the catalyst precursor is as figure 1 shown.

Embodiment 2

[0023] Mix cobalt and chromium metal salts according to the atomic ratio of 0.15:1 to prepare a solution, use ammonia water as a precipitant for precipitation reaction, pH is 8, and continue to stir and age for 10 minutes, then filter, wash with deionized water until neutral, filter The cake was dried at a temperature of 110°C, and finally roasted at a temperature of 350°C in an inert gas environment to prepare a catalyst precursor. The catalyst precursor was crushed and mixed with 3% graphite, and the uniformly mixed powder was pressed The tablet is not broken by hand, and at a temperature of 300°C, the mixed gas of inert gas and hydrogen fluoride is passed through for fluorination to prepare the required catalyst. The pore structure of the catalyst precursor is as figure 1 shown.

Embodiment 3

[0025] Mix cobalt and chromium metal salts according to the atomic ratio of 0.25:1 to prepare a solution, use ammonia water as a precipitant for precipitation reaction, pH is 9, and continue to stir and age for 11 minutes, then filter, wash with deionized water until neutral, filter The cake is dried at a temperature of 110°C, and finally roasted at a temperature of 350°C in an inert gas environment to prepare a catalyst precursor. The catalyst precursor is crushed and mixed with 4% graphite, and the uniformly mixed powder is pressed The tablet is not broken by hand, and at a temperature of 400°C, the mixed gas of inert gas and hydrogen fluoride is passed through for fluorination to prepare the required catalyst. The pore structure of the catalyst precursor is as figure 1 shown.

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Abstract

The invention discloses a preparation method of a fluorination catalyst. The preparation method is as follows: preparing a solution of active component metal salts, wherein preferably the atomic ratio of Co / Cr is 0.05-0.25 and the atomic ratio of Y / Cr is preferably 0.01-0.15; reacting with ammonia water as a precipitant at a PH value between 7 and 9; further stirring and aging for 9-11 minutes; filtering, and washing with deionized water till the solution is neutral; drying a filter cake at a temperature of 100-150 DEG C; carrying out calcination in an inertial gas environment to obtain a catalyst precursor; crushing the catalyst precursor and mixing the catalyst with graphite; laminating the uniformly mixed powder till the lamina cannot be crushed with hands; at the temperature of 200-400 DEG C, introducing inertial gas and hydrogen fluoride mixed gas, and carrying out fluorination to obtain the catalyst, wherein metal cobalt and yttrium form corresponding metal oxide during calcination stage; small metal oxide particles move in the catalyst precursor and the catalyst precursor is etched by the particles, the etching of the residual moisture in the catalyst precursor to the catalyst precursor can also be catalyzed, so as to form a series of porous structures in which medium pores take a great proportion.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a catalyst for preparing 1,1,1,2-tetrafluoroethane by gas-phase fluorination. Background technique [0002] In recent years, the destruction of the ozone layer by CFCs has become increasingly serious, and 1,1,1,2-tetrafluoroethane (HFC-134a) is a colorless, non-toxic, non-combustible chemical substance, and is a HFC-type refrigeration agent, the Ozone Depletion Potential (ODP) value is zero. The thermodynamic performance of HFC-134a is very similar to that of CFC-12, and its safety is comparable to that of CFC-12. It has been recognized as the best substitute of CFC-12. [0003] HFC-134a is generally prepared from trichlorethylene and anhydrous hydrogen fluoride. Currently, there are two preparation methods: liquid phase method and gas phase method. The liquid-phase method generally uses antimony halides as catalysts, but this method has disadvantages such as low conversion...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J23/26B01J35/10B01J37/08B01J37/26C07C17/20C07C19/08
Inventor 王洪祥林寿洪徐志雄
Owner JIANGSU SANMEI CHEM