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Preparation process of monochlorodifluoromethane

A technology for difluoromonochloromethane and a preparation process is applied in the field of preparation of difluoromonochloromethane, and can solve the problems of poor product selectivity of difluoromonochloromethane, complicated separation and purification process of trifluoromethane, low conversion rate and the like, Achieve the effect of improving selectivity, improving catalyst performance, and reducing side reactions

Active Publication Date: 2020-09-08
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The above method has the problems of complex separation and purification process of trifluoromethane or low purity, poor product selectivity and low conversion rate in the production of difluorochloromethane

Method used

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  • Preparation process of monochlorodifluoromethane
  • Preparation process of monochlorodifluoromethane
  • Preparation process of monochlorodifluoromethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The main catalyst is prepared by impregnation method: the nitrate of the active component Al is stirred and dissolved with deionized water to obtain a metal salt solution, that is, the impregnation solution; the dried multi-level micro / mesoporous Cr 2 o 3 The carrier was impregnated in the impregnating solution for 4 hours at room temperature, then filtered, and dried in a drying oven at 114°C for 8 hours to obtain a precursor. Finally, the obtained precursor was calcined under inert gas argon, and calcined at 500°C for 4 hours to obtain the main catalyst. Among them, the multi-level micro / mesoporous Cr 2 o 3 The specific surface area is 86.5m 2 / g, the average pore diameter is 9.5nm, 55.2% of the pore diameter is 0.2-2nm, and 14.5% of the pore diameter is 15-50nm.

[0056] By physically grinding and mixing with the host catalyst, adding metal doping components 2wt% Ru and rare earth additives 5wt% Sm 2 o 3 , 1wt% SmCl 3 , the added amount is based on the mass of ...

Embodiment 2

[0059] The main catalyst is prepared by impregnation method: the sulfate salt of the active component Mg is stirred and dissolved in deionized water to obtain a metal salt solution, that is, the impregnation solution; the dried multi-level micro / mesoporous Cr 2 o 3Immerse in the impregnating solution for 4 hours at room temperature, then filter, put in a drying oven and dry at 114°C for 8 hours to obtain a precursor. Finally, the obtained precursor is calcined under inert gas argon, and calcined at 500°C for 4 hours to obtain the main catalyst. Among them, the multi-level micro / mesoporous Cr 2 o 3 The specific surface area of ​​the carrier is 85.8m 2 / g, the average pore diameter is 9.5nm, 55.2% of the pore diameter is 0.2-2nm, and 14.5% of the pore diameter is 15-50nm.

[0060] By physically grinding and mixing with the main catalyst, adding the metal doping component 2wt% Pd and the rare earth additive 3wt% La 2 o 3 , 2wt% LaCl 3 , the added amount is based on the mass...

Embodiment 3

[0079] Trifluoromethane, chloroform and chlorine are raw materials to produce difluorochloromethane product, comprising the following steps:

[0080] In step 1), the mixed gas (1) containing trifluoromethane by-products is sent into an extraction separation tower, and high-purity trifluoromethane gas (2) is obtained after purification, and the extract in the extraction separation tower is pyridine tetrafluoroboron acid salt; step 2), the high-purity trifluoromethane gas (2) is sent into a microchannel reactor as a reaction raw material, and chloroform and chlorine are added, and the reaction is carried out in the presence of the catalytic system of Example 1 to obtain a microchannel reactor containing The reaction product flow (3) of difluorochloromethane, the reactor heating temperature is 230 ℃, and the mol ratio of trifluoromethane, trichloromethane and chlorine is 3:0.6:1; step 3), will contain difluorochloromethane The reaction product stream (3) of methane is sent into t...

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Abstract

The invention discloses a preparation process for producing a monochlorodifluoromethane product with high additional value by taking trifluoromethane, trichloromethane and chlorine as raw materials. According to the preparation process, a micro-channel reactor is used; an active component, a carrier, a metal doping component and a rare earth auxiliary agent with specific types and proportions arearranged; the reaction of trifluoromethane and chlorine and the reaction of trifluoromethane and trichloromethane are effectively promoted; multistage micro / mesoporous Cr2O3 is used as a carrier to promote fluorine-chlorine exchange reactions, and the catalyst performance is further enhanced. In the reaction process, excessive trifluoromethane is selected, full conversion of trichloromethane and chlorine is promoted, meanwhile, in a subsequent separation system, proper extraction liquid tetrafluoroborate or tetrafluorethionate is selected, trifluoromethane is fully extracted and recycled and serves as a reaction raw material, the reaction raw material enters an initial reactor in a circulating mode, and full utilization of the raw material is promoted.

Description

technical field [0001] The present invention relates to a preparation process of difluorochloromethane, in particular to a method of reacting trifluoromethane, chloroform and chlorine as raw materials in the presence of a catalyst to produce a high value-added difluorochloromethane product preparation process. Background technique [0002] Chlorodifluoromethane, also known as Freon-22 (HCFC-22), has an ozone depletion potential (ODP) of 0.05 and a GWP of 1780. It is the most widely used HCFCs substance, mainly used in blowing agents, aerosols, and refrigeration As raw materials for chemicals and other chemical products, the production and consumption of difluorochloromethane are developing rapidly in my country. [0003] Trifluoromethane (CHF 3 ) also known as fluoroform, as a by-product of industrial preparation of chlorodifluoromethane (HCFC-22), its content in the generated HCFC-22 is about 1.5-3 wt%, and its annual output in my country is as high as about 13,000-15,000 ...

Claims

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Application Information

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IPC IPC(8): C07C19/10C07C17/20B01J23/652B01J35/10
CPCC07C17/202B01J23/6522B01J35/613B01J35/647C07C19/10Y02P20/40
Inventor 张建君刘武灿王术成周飞翔韩文锋
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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