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Method for preparing mesoporous chromium-based gaseous fluorinated catalyst

A phase fluorination catalyst and mesoporous technology, applied in the field of preparation of fluorination catalysts, can solve the problems of uneven distribution of catalyst active metals, high selectivity of by-product R115, uneven distribution of catalyst pore structure, etc. The effect of reducing energy consumption and improving mechanical strength

Active Publication Date: 2017-12-12
RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of uneven distribution of catalyst pore structure, low specific surface area, uneven distribution of catalyst active metals, easy loss of active metals during production and operation, low catalyst performance, and high selectivity of by-product R115 during the preparation of R125 in the existing experimental methods , the present invention provides a method for preparing a mesoporous chromium-based fluorination catalyst suitable for gas-phase fluorination reactions, and introduces an ordered mesoporous structure into the fluorination catalyst through a hard template method

Method used

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  • Method for preparing mesoporous chromium-based gaseous fluorinated catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Under stirring at room temperature, 50g CrCl 3 ·6H 2 O, 10.2g AlCl 3 and 15mL of deionized water were dissolved in 95mL of absolute ethanol, and placed in a sealed autoclave for heat pretreatment at 96°C for 4 hours to obtain a highly dispersed salt solution.

[0043] Weigh 52g of SBA-16 white powder and place it in a flask, connect it to a vacuum pump, and keep it at a vacuum of 60kPa for 200min, add the above-mentioned highly dispersed salt solution into the flask dropwise, and keep the vacuum constant until the sample is dry. Take out the sample and put it in the tube furnace N 2 Calcined at 350°C for 3h in the atmosphere, and the precursor was obtained after natural cooling.

[0044] Weigh 4.05g CoCl 2 Dissolve in 120 mL deionized water, add the solution dropwise to the vacuum-treated precursor, then evaporate the liquid in a water bath, then dry it in an oven at 100 °C for 6 h, and finally heat it in a tube furnace at 340 °C under a nitrogen atmosphere. ℃ for ...

Embodiment 2

[0048] Under stirring at room temperature, 50g CrCl 3 ·6H 2 O, 6.8g AlCl 3 and 10 mL of deionized water were dissolved in 90 mL of absolute ethanol, and placed in a sealed autoclave for heat pretreatment at 98°C for 5 hours to obtain a highly dispersed salt solution.

[0049] Weigh 50g of SBA-16 white powder and place it in a flask, connect it to a vacuum pump, and keep it at a vacuum of 60kPa for 200min, add the above-mentioned highly dispersed salt solution into the flask dropwise, and keep the vacuum constant until the sample is dry. Take out the sample and put it in the tube furnace N 2 Calcined at 360°C for 5h in the atmosphere, and the precursor was obtained after natural cooling.

[0050] Weigh 6.38g MgCl 2 Dissolve in 120 mL deionized water, add the solution dropwise to the vacuum-treated precursor, then evaporate the liquid in a water bath, then dry it in an oven at 110 °C for 7 h, and finally heat it in a tube furnace at 330 °C under a nitrogen atmosphere. ℃ for...

Embodiment 3

[0054] Under stirring at room temperature, 50g CrCl 3 ·6H 2 O, 7.94g AlCl 3 and 20mL of deionized water were dissolved in 80mL of absolute ethanol, and placed in a sealed autoclave at 95°C for heat pretreatment for 4 hours to obtain a highly dispersed salt solution.

[0055] Weigh 50g of SBA-16 white powder and place it in a flask, connect it to a vacuum pump, and keep it at a vacuum of 60kPa for 200min, add the above-mentioned highly dispersed salt solution into the flask dropwise, and keep the vacuum constant until the sample is dry. Take out the sample and put it in the tube furnace N 2 Calcined at 350°C for 4h in the atmosphere, and the precursor was obtained after natural cooling.

[0056] Weigh 2.65g InCl 3 Dissolve in 120 mL deionized water, add the solution dropwise to the vacuum-treated precursor, then evaporate the liquid in a water bath, then dry it in an oven at 120 °C for 8 h, and finally heat it in a tube furnace at 350 °C under a nitrogen atmosphere. ℃ for ...

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Abstract

The invention relates to a method for preparing a mesoporous chromium-based gaseous fluorinated catalyst. The method comprises the steps of taking SBA-16 as a hard template, adding chromium-based metal salt solution dropwise, and performing roasting; adding other metal salt solutions dropwise, and performing drying, roasting, smashing and tabletting to obtain a catalyst precursor; fluoridizing the precursor and removing the SBA-16 template, and obtaining the mesoporous chromium-based gaseous fluorinated catalyst. The prepared mesoporous chromium-based gaseous fluorinated catalyst has a specific surface area of 300-350 m<2> / g and an average pore size of 10-13 nm. The mesoporous chromium-based gaseous fluorinated catalyst is high in catalytic activity and suitable for being applied to gaseous fluoridation, and particularly when the mesoporous chromium-based gaseous fluorinated catalyst is applied to R125 preparation, a by-product control effect is very good.

Description

technical field [0001] The present invention relates to the preparation and application of a fluorination catalyst, in particular to a preparation method of a chromium-based fluorination catalyst with a mesoporous structure used for gas-phase fluorination of halogenated hydrocarbons and hydrogen fluoride, and the preparation of the catalyst Application of R125 gas phase fluorination reaction. Background technique [0002] In recent years, studies have found that hydrofluorocarbons ((HFCs) have an ozone depletion potential (ODP) of 0 and a low global warming potential (GWP), and are widely used in large commercial refrigerants, blowing agents, fire extinguishing agents, etc. At present, the key production process of the mainstream environmentally friendly refrigerants (R125, R134a, R1234yf) in the market is the gas-phase fluorination catalytic reaction process. It is found that the catalytic activity of the fluorination catalyst has a great relationship with the pore volume,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J27/138B01J35/10C07C17/093C07C19/08
CPCC07C17/093B01J27/132B01J27/138B01J35/635B01J35/647B01J35/615C07C19/08
Inventor 李义涛唐火强张宏清孙明刚罗玄锋余航黄永锋胡聿明马鹏程
Owner RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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