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Mesoporous chromium-based fluorination catalyst and preparation method of same

A base fluorination catalyst and a fluorination catalyst technology are applied in the field of catalyzing the preparation of a chromium base fluorination catalyst for R134a and the field of preparation thereof, which can solve the problem of uneven distribution of catalyst active metals, high selectivity of by-product R134, and uneven distribution of catalyst pore structure. Equalization problem, to achieve the effect of increasing specific surface area, reducing selectivity, and good pore structure

Active Publication Date: 2017-12-22
RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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 excessively high selectivity of by-product R134 in the existing experimental methods, the present invention will The mesoporous structure is introduced into the traditional chromium-based fluorination catalyst, and a chromium-based fluorination catalyst with a mesoporous structure and its preparation method are provided

Method used

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  • Mesoporous chromium-based fluorination catalyst and preparation method of same
  • Mesoporous chromium-based fluorination catalyst and preparation method of same
  • Mesoporous chromium-based fluorination catalyst and preparation method of same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Weigh 21.78g CrCl respectively 3 ·6H 2 O, 12.84g AlCl 3 , 3.86g InCl 3 1. Dissolve 0.626g OBS in 100mL deionized water, and adjust the pH value to 9 by adding ammonia water. The generated slurry material was transferred to a 200mL stainless steel synthesis kettle and heated to 120°C to continue the reaction for 72h. After the reaction was completed, it was cooled to room temperature. The material was unloaded and washed several times with a centrifuge, and the filter cake was dried at room temperature. Then, it was calcined in a tube furnace at 400°C for 3 hours in a nitrogen atmosphere. The calcined samples were pulverized and sieved, mixed with graphite, and pressed into tablets to obtain a catalytic precursor.

[0049] Then, the catalyst precursor was loaded into a reactor, and a mixed gas of nitrogen and HF was introduced to fluorinate at 340° C. to prepare a chromium-based fluorination catalyst.

[0050] Using the specific surface area and pore structure tester...

Embodiment 2

[0052] Weigh 34.84g CrCl respectively 3 ·6H 2 O, 10.86g AlCl 3 , 3.86g InCl 3 1. Dissolve 0.364g of trimethylhexadecylammonium bromide (CTAB) in 90mL of deionized water, and adjust the pH value to 8 by adding ammonia water. The generated slurry material was transferred to a 200mL stainless steel synthesis kettle and heated to 110°C to continue the reaction for 80h. After the reaction was completed, it was cooled to room temperature. The material was unloaded and washed several times with a centrifuge, and the filter cake was dried at room temperature. Then, it was calcined at 350° C. for 4 h in a tube furnace under a nitrogen atmosphere. The calcined samples were pulverized and sieved, mixed with graphite, and pressed into tablets to obtain a catalytic precursor.

[0053] Then, the catalyst precursor was loaded into a reactor, and a mixed gas of nitrogen and HF was introduced to fluorinate at 330° C. to prepare a chromium-based fluorination catalyst.

[0054] Using the spe...

Embodiment 3

[0056] Weigh 17.42g CrCl respectively 3 ·6H 2 O, 14.82g AlCl 3 , 3.86g InCl 3 1. Dissolve 0.948g of ammonium oxide in 80mL of deionized water, and adjust the pH value to 10 by adding ammonia water. The generated slurry material was transferred to a 200mL stainless steel synthesis kettle and heated to 130°C to continue the reaction for 80h. After the reaction was completed, it was cooled to room temperature, and the material was unloaded and washed several times with a centrifuge, and the filter cake was dried at room temperature. Then, it was calcined in a tube furnace at 400°C for 3 hours in a nitrogen atmosphere. The calcined samples were pulverized and sieved, mixed with graphite, and pressed into tablets to obtain a catalytic precursor.

[0057] Then, the catalyst precursor was loaded into a reactor, and a mixed gas of nitrogen and HF was introduced to fluorinate at 320° C. to prepare a chromium-based fluorination catalyst.

[0058] Using the specific surface area and ...

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Abstract

The invention relates to a mesoporous chromium-based fluorination catalyst and a preparation method of same. The fluorination catalyst includes chromium, aluminum and other metals according to the mass ratio of 40-80:20-30:0-20. A precursor of the fluorination catalyst is 6.0-8.0 nm in pore diameter and is 400-500 m<2> / g in specific surface area. The preparation method includes the steps of: dissolving chromium salt, aluminum salt, salts of other metals, and a surfactant in water; performing precipitation with ammonia water; moving the liquid to a crystallization tank, and performing crystallization to obtain a turbid liquid; filtering the turbid liquid, water-washing a solid, drying and roasting the solid, crushing and mixing the solid, and tabletting the solid to form a catalyst precursor; and fluorinating the precursor to obtain the fluorination catalyst. The mesoporous chromium-based fluorination catalyst has large specific surface area, excellent pore structure and high catalytic activity, and is suitable for application of gas-phase fluorination reaction; especially, the catalyst, when being applied to preparation of R134a, is good in control effect on byproducts.

Description

technical field [0001] The present invention relates to a fluorination catalyst, its preparation and application, in particular to a chromium-based fluorination catalyst with a mesoporous structure used for gas-phase fluorination of halogenated hydrocarbons and hydrogen fluoride, especially for the catalytic preparation of R134a Chromium-based fluorination catalyst and its preparation method. 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. The gas-phase fluorination catalyst is the core of the process route for the production of fluorinated hydrocarbons ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J35/10C07C17/20C07C19/08
CPCC07C17/206B01J27/132B01J35/615B01J35/647C07C19/08
Inventor 李义涛张宏清唐火强邓龙辉胡为晴孙明刚黄永锋胡聿明马鹏程
Owner RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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