Sub-nano AlF3 catalyst as well as preparation method and application thereof

A catalyst and sub-nanometer technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, dehydrohalogenation preparation, etc., can solve the problems of catalyst deactivation, etc., so as to achieve less carbon deposition and deactivation, short preparation cycle, high The effect of catalytic activity and stability

Active Publication Date: 2021-04-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned carbon deposition and sintering phenomena existing in existing catalysts, which lead to the problem of catalyst deactivation, the purpose of the present invention is to provide a kind of MIL-53-Al as the precursor to prepare sub-nanometer AlF 3 Methods and Applications of Catalysts

Method used

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  • Sub-nano AlF3 catalyst as well as preparation method and application thereof
  • Sub-nano AlF3 catalyst as well as preparation method and application thereof
  • Sub-nano AlF3 catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 6.698g of Al(NO 3 ) 3 9H 2 O and 2.586g of organic ligands were placed in a polytetrafluoroethylene liner and stirred for 30min, stirred evenly and then placed in a hydrothermal kettle for 0.5d at 160°C. Then wash with DMF and ethanol in a water bath at 60°C for 2h, and dry at 60°C for 10h to obtain white powder MIL-53-Al. Put MIL-53-Al into the atmosphere tube furnace, and feed the gas phase fluorine source CHClF at 300°C 2 , the gas phase fluorine source flow rate is 20ml / min fluorination for 1h, and then wait until the gas phase fluorination is completed, fluorination for 1h; switch the atmosphere in the tube furnace to N 2 Until the natural cooling to room temperature, the stable sub-nanometer AlF 3 catalyst. The obtained catalyst sample was sieved with a 20-40 mesh sieve.

[0023] The above-prepared subnano-AlF 3 The catalyst is used to catalyze the cracking of 1,1-difluoroethane (HFC-152a) to produce vinyl fluoride. The reaction formula is as follows:

[0...

Embodiment 2

[0027] 6.698g of Al(NO 3 ) 3 9H 2 O and 2.586g of organic ligands were placed in a polytetrafluoroethylene liner and stirred for 30min, stirred evenly and then placed in a hydrothermal kettle for 3d at 220°C. Then wash with DMF and ethanol in a water bath at 80°C for 4.5h, and dry at 120°C for 24h to obtain white powder MIL-53-Al. Put MIL-53-Al into 20ml of 40wt% HF solution, put it in a water bath at 60°C for 8h with stirring, wash it by centrifugation, and dry it at 60°C to prepare the catalyst, 400°C N 2Calcined under the atmosphere for 3h and then cooled down to room temperature naturally to obtain stable sub-nanometer AlF 3 Catalyst, the obtained catalyst sample is sieved with a 20-40 mesh sieve.

[0028] The above-prepared subnano-AlF 3 The catalyst is used to catalyze the cracking of 1,1,1,3,3-pentafluoropropane (HFC-245fa) to produce 1,3,3,3-tetrafluoropropene (HFO-1234ze), the reaction formula is as follows:

[0029]

[0030] The reaction conditions are: the ...

Embodiment 3

[0032] 6.698g of Al(NO 3 ) 3 9H 2 O and 2.586g of organic ligands were placed in a polytetrafluoroethylene liner and stirred for 30min, stirred evenly and then placed in a hydrothermal kettle for 3d at 220°C. Then wash with DMF and ethanol in a water bath at 80°C for 4.5h, and dry at 120°C for 24h to obtain white powder MIL-53-Al. 5.366g of MIL-53-Al and 13.686g of ammonium bifluoride (NH 4 HF 4 ) into the ball mill jar, and put the ball mill jar into the ball mill to fix it. The program of the ball mill is set to 400r / min, and the ball mill is suspended for 30 minutes every hour for 3 hours until the program ends. Put the ball mill jar and its milled samples into an oven for 6 h at 80°C, take out the samples, and put them in a tube furnaceN 2 Calcined at 400°C for 3 h under atmosphere. The catalyst sample was obtained and sieved with a 20-40 mesh sieve.

[0033] The above-prepared subnano-AlF 3 The catalyst is used to catalyze the cracking of 1,1,1,3,3-pentafluoropro...

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Abstract

The invention discloses a sub-nano AlF3 catalyst and a preparation method and application thereof.The preparation method comprises the steps that MIL-53-Al serves as a precursor to prepare the sub-nano AlF3 catalyst, and the specific preparation process comprises the steps that a proper amount of Al (NO3) 3 . 9 H2O and an organic ligand are put into a polytetrafluoroethylene lining to be stirred for 30 min, then put into a hydrothermal kettle and subjected to a hydrothermal reaction at 160-220 DEG C for 0.5-3 d, and naturally cooled to room temperature; and respectively washing with DMF (Dimethyl Formamide) and ethanol in a water bath at 60-80 DEG C for 2-4.5 hours, and drying at 60-120 DEG C for 10-24 hours to obtain white powder MIL-53-Al for later use, and under the action of a fluorine source, fluorinating the white powder (MIL-53-Al) to obtain the sub-nano AlF3 catalyst. The catalyst prepared by the method disclosed by the invention shows extremely high activity and stability in the reaction of preparing fluorine-containing olefin by removing HF from fluorine-containing alkane in a gas phase. The catalyst provided by the invention has the characteristics of simple preparation, high conversion rate, good selectivity, high stability and difficulty in carbon deposition.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, in particular to subnano AlF 3 Catalyst and its preparation method and application. Background technique [0002] Fluorinated alkanes (HFCs) are indispensable functional chemical substances in modern society, and are widely used in refrigerants, foaming agents, mold release agents and cleaning agents. However, fluorine-containing alkanes are greenhouse gases with relatively high greenhouse effect potential (GWP). Extensive use will cause harm to the environment. They are gases that are controlled under the Kyoto Protocol. Therefore, in order to cope with climate change, it is the general trend to convert fluorine-containing alkanes into fluorine-containing olefins. Fluorinated olefins (HFOs) have less impact on the environment and are considered to be the most ideal substitutes for HFCs. Fluorinated alkanes are widely used in fluorine-containing rubber, fluorine-containing resin, fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/125B01J37/10B01J37/08B01J37/26C07C17/25C07C21/18
Inventor 韩文锋贾忠盛吴森王传钊余厚霖刘兵韦小丽唐浩东李瑛
Owner ZHEJIANG UNIV OF TECH
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