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Method for preparing fluoro-chlorine exchange catalyst with high specific surface area

A high specific surface area, catalyst technology, used in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low service life, uneven distribution of active components, low specific surface area, etc. The effect of uniform distribution of additives, abundant inner pores and high specific surface area

Active Publication Date: 2018-11-27
天津航大翼安科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation methods of chromium-based catalysts mainly include coprecipitation method and impregnation method, but these preparation methods have defects such as low specific surface area, uneven distribution of active components, and low service life.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation method of the high specific surface area fluorine-chlorine exchange catalyst provided by this embodiment comprises the following steps carried out in order:

[0022] (1) Add 1.0g metal-organic framework material MIL-101(Cr) to 200mL anhydrous cyclohexane, ultrasonically disperse for 15min, add 2mL Zn(NO 3 ) 2 Aqueous solution, continue to stir for 2 hours, then filter to make a catalyst, dry the catalyst at room temperature for 24 hours, and then dry at 200°C for 10 hours;

[0023] (2) Get 1.0g of the above-mentioned dried catalyst and join in 12mL 5-hydroxymethylfurfural, filter after stirring for 12 hours, wash with dehydrated alcohol, dry at room temperature for 12 hours, then place the catalyst in a tube furnace, In an inert gas atmosphere, it was kept at 150°C for 24 hours, raised to 800°C for 6 hours, and then lowered to room temperature to obtain a fluorine-chlorine exchange catalyst precursor. The specific surface area measured by the BET method...

Embodiment 2

[0026] The preparation method of the high specific surface area fluorine-chlorine exchange catalyst provided by this embodiment comprises the following steps carried out in order:

[0027] (1) Add 1.0g metal-organic framework material MIL-101(Cr) to 200mL anhydrous cyclohexane, ultrasonically disperse for 15min, add 2mL Co(NO 3 ) 2 Aqueous solution, continue to stir for 2 hours, then filter to make a catalyst, dry the catalyst at room temperature for 24 hours, and then dry at 180°C for 12 hours;

[0028] (2) Get 1.0g of the above-mentioned dried catalyst and add it to 11mL of furfural, filter after stirring for 12 hours, wash with absolute ethanol, dry at room temperature for 12 hours, then place the catalyst in a tube furnace, and place it in an inert gas atmosphere Keep it at 160°C for 20 hours, raise the temperature to 890°C and keep it for 7 hours, and then lower it to room temperature to obtain a fluorine-chlorine exchange catalyst precursor. The specific surface area me...

Embodiment 3

[0031] The preparation method of the high specific surface area fluorine-chlorine exchange catalyst provided by this embodiment comprises the following steps carried out in order:

[0032] (1) Add 1.0 g metal-organic framework material MIL-101 (Cr) to 200 mL of anhydrous n-hexane, ultrasonically disperse for 15 min, add 2 mL of Ni(NO 3 ) 3 Aqueous solution, continue to stir for 2 hours, then filter to make a catalyst, dry the catalyst at room temperature for 24 hours, and then dry at 180°C for 12 hours;

[0033] (2) Take 1.0 g of the above-mentioned dried catalyst and add it to 11 mL of ethylene glycol, filter after stirring for 12 hours, wash with absolute ethanol, and dry at room temperature for 12 hours, then place the catalyst in a tube furnace, in an inert gas atmosphere Keep it at 230°C for 20 hours, raise the temperature to 890°C and keep it for 8 hours, and then lower it to room temperature, thus obtaining the fluorine-chlorine exchange catalyst precursor, the specifi...

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Abstract

The invention discloses a method for preparing a fluoro-chlorine exchange catalyst with high specific surface area. The method comprises the following steps: carbonizing a metal-organic framework material MIL-101 (Cr) serving as a raw material and metal brine serving as an assistant, and performing fluoridation treatment, thereby obtaining the fluoro-chlorine exchange catalyst with high specific surface area. The method disclosed by the invention has the advantages that the metal-organic framework material MIL-101 (Cr) with high specific surface area, high internal pore volume and uniform andordered Cr element distribution serves as the raw material of the fluoro-chlorine exchange catalyst, so that the prepared fluoro-chlorine exchange catalyst also has the characteristics of high specific surface area, high internal pore volume and uniform and ordered Cr element distribution; the assistants are added by an adsorption method, so that the distribution of the assistants is uniform, andthe effective utilization rate of the assistants is improved; and the product has the characteristics of high specific surface area, rich internal pores, high catalytic activity, uniform assistant distribution and the like, and is applicable to the fluoro-chlorine exchange reaction.

Description

technical field [0001] The invention belongs to the technical field of catalytic synthesis, in particular to a preparation method of a high specific surface area fluorine-chlorine exchange catalyst. Background technique [0002] At present, the industrial production of hydrofluorocarbons (HFCs) or hydrofluoroolefins (HFOs) mostly adopts the gas-phase catalytic fluorine-chlorine exchange reaction method of halogenated organic compounds, which has the advantages of simple process, easy continuous large-scale production, and safe operation. Fluorine-chlorine exchange catalysts play a central role in gas-phase catalyzed fluorine / chlorine exchange reactions of halogenated organic compounds. Common fluorine-chlorine exchange catalysts are chromium-based catalysts, the main component of which is chromium. At present, the preparation methods of chromium-based catalysts mainly include coprecipitation method and impregnation method, but these preparation methods have defects such as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J35/10B01J37/08B01J37/26
CPCB01J27/132B01J37/084B01J37/086B01J37/26B01J35/399B01J35/60B01J35/615
Inventor 李秀涛罗星娜王明超周晓猛
Owner 天津航大翼安科技发展有限公司
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