A kind of preparation method of high specific surface area fluorine-chlorine exchange catalyst

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 uneven distribution of active components, low specific surface area, low service life, etc. The effect of abundant inner pores, high specific surface area and uniform distribution of additives

Active Publication Date: 2020-12-01
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 in this embodiment includes the following steps in sequence:

[0022](1) Add 1.0g of metal organic framework material MIL-101(Cr) to 200mL of anhydrous cyclohexane, ultrasonically disperse for 15min, add 2mL Zn(NO3)2The aqueous solution was stirred for 2 hours, and then filtered to prepare a catalyst. The catalyst was dried at room temperature for 24 hours and then at 200°C for 10 hours;

[0023](2) Add 1.0g of the above-mentioned dried catalyst to 12mL 5-hydroxymethylfurfural, stir for 12 hours, filter, wash with absolute ethanol, dry for 12 hours at room temperature, and then place the catalyst in a tube furnace. Keep at 150°C for 24 hours in an inert gas atmosphere, raise the temperature to 800°C for 6 hours, and then lower to room temperature, thereby obtaining a fluorine-chlorine exchange catalyst precursor. The specific surface area measured by the BET method is 653m2 / g.

[0024]...

Embodiment 2

[0026]The preparation method of the high specific surface area fluorine-chlorine exchange catalyst provided in this embodiment includes the following steps in sequence:

[0027](1) Add 1.0g of metal organic framework material MIL-101(Cr) to 200mL of anhydrous cyclohexane, ultrasonically disperse for 15min, add 2mL of Co(NO3)2The aqueous solution was stirred for 2 hours, and then filtered to prepare a catalyst. The catalyst was dried at room temperature for 24 hours and then at 180°C for 12 hours;

[0028](2) Add 1.0g of the above-mentioned dried catalyst to 11mL furfural, stir for 12 hours, filter, wash with absolute ethanol, and dry for 12 hours at room temperature, then place the catalyst in a tube furnace and place it in an inert gas atmosphere. Keep it at 160°C for 20 hours, increase the temperature to 890°C for 7 hours, and then lower to room temperature to obtain a fluorine-chlorine exchange catalyst precursor. The specific surface area measured by the BET method is 573m.2 / g.

[0029](...

Embodiment 3

[0031]The preparation method of the high specific surface area fluorine-chlorine exchange catalyst provided in this embodiment includes the following steps in sequence:

[0032](1) Add 1.0g of metal organic framework material MIL-101(Cr) to 200mL of anhydrous n-hexane, ultrasonically disperse for 15min, add 2mL of Ni(NO3)3The aqueous solution was stirred for 2 hours, and then filtered to prepare a catalyst. The catalyst was dried at room temperature for 24 hours and then at 180°C for 12 hours;

[0033](2) Add 1.0 g of the above-mentioned dried catalyst to 11 mL of ethylene glycol, stir for 12 hours, filter, 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 The medium was kept at 230°C for 20 hours, heated to 890°C for 8 hours, and then lowered to room temperature to obtain a fluorine-chlorine exchange catalyst precursor. The specific surface area measured by the BET method was 631m2 / g.

[0034](3) Load t...

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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, and particularly relates to a preparation method of a fluorine-chlorine exchange catalyst with a high specific surface area.Background technique[0002]At present, most of the industrial production of hydrofluorocarbons (HFCs) or hydrofluoroolefins (HFOs) adopts the gas phase catalytic fluorine-chlorine exchange reaction method of halogenated organics, which has the advantages of simple process, easy continuous large-scale production, and safe operation. The fluorine-chlorine exchange catalyst plays a central role in the gas-phase catalytic fluorine / chlorine exchange reaction of halogenated organics. The common fluorine-chlorine exchange catalyst is a chromium-based catalyst, the main component of which is chromium. At present, the preparation methods of chromium-based catalysts mainly include co-precipitation method and impregnation method, but these preparation methods have defects such as low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/132B01J35/10B01J37/08B01J37/26
CPCB01J27/132B01J35/0093B01J35/10B01J35/1019B01J37/084B01J37/086B01J37/26
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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