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Catalyst for producing difluoro acetylfluoride and preparation method thereof

A technology of difluoroacetyl fluoride and catalyst, which is applied in the field of catalyst for the production of difluoroacetyl fluoride and its preparation, can solve the problems of easy carbon deposition and deactivation of the catalyst, and achieve increased anti-carbon deposition ability, improved stability, and low The effect of carbon deposition

Inactive Publication Date: 2011-10-19
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a catalyst for the preparation of difluoroacetyl fluoride by catalytic cracking of low-cost 1,1,2,2-tetrafluoroethyl alkyl ether with high catalytic activity, and to solve the problem that the catalyst is prone to carbon deposition and deactivation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 240 g of pseudoboehmite (Al 2 o 3 ·H 2 O) Calcined in air at 500°C for 4h, then passed nitrogen gas at 200°C for 12h, and then activated with difluorodichloromethane for 12h, the gas flow rate was 40mL / min. The sample is designated as Al-1.

Embodiment 2

[0015] Take 143.2 g of ZrOCl 2 ·8H 2 O was dissolved in 600 grams of water, and 240 grams of pseudoboehmite (Al 2 o 3 ·H 2 O) Immerse in the above solution, and gradually add 25% ammonia water during stirring until the pH value reaches 8, and the mixed precipitate obtained at this time continues to stir and age for 2 hours. Then filter, wash with 3 liters of water, dry at 120°C for 12 hours, calcinate at 500°C in air for 4 hours, and finally activate at 200°C for 12 hours with nitrogen and difluorodichloromethane at a gas flow rate of 40mL / min. The molar ratio of metal elements in the sample is Al:Zr=9:1, and the sample is designated as AlZr-2.

Embodiment 3

[0017] Take 170.2 grams of Y (NO 3 ) 3 ·6H 2 O was dissolved in 600 grams of water, and 240 grams of pseudoboehmite (Al 2 o 3 ·H 2 O) Immerse in the above solution, and gradually add 25% ammonia water during stirring until the pH value reaches 8, and the mixed precipitate obtained at this time continues to stir and age for 2 hours. Then filter, wash with 3 liters of water, dry at 120°C for 12 hours, calcinate at 500°C in air for 4 hours, and finally activate at 200°C for 12 hours with nitrogen and difluorodichloromethane at a gas flow rate of 40mL / min. The sample metal element molar ratio Al:Y=9:1 sample is recorded as AlY-3.

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Abstract

The invention discloses a catalyst for producing difluoro acetylfluoride by catalyzing and cracking 1, 1, 2, 2-tetrafluoethyl alkyl ether and a preparation method thereof. The preparation method comprises the following steps of taking pseudo-boehmite powder (specific surface area of 400m2 / g) and at least one type of water-soluble salt of other elements such as zirconium, yttrium, lanthanum cerium and praseodymium as an original raw material; mixing the original raw material with water; gradually adding ammonia in the solution during the mixing process till the pH value of colloidal substance achieves 7 to 9; subsequently carrying out ageing, filtering, water washing, drying, roasting in air, pressing and forming; and then pumping HF / N2 mixed gas or fluorochloromethane, thus obtaining the catalyst by activation. The catalyst has the advantages such as a high specific surface area, a plurality of uniformly distributed active acid centers and excellent mechanical strength, thereby having high activity and high stable performance.

Description

technical field [0001] The invention relates to a catalyst for producing difluoroacetyl fluoride by catalytically cracking 1,1,2,2-tetrafluoroethyl alkyl ether and a preparation method thereof. Background technique [0002] Difluoroacetic acid is a class of important drug intermediates, such as can be used to prepare drugs such as imidazoles, the drug has anti-cancer, anti-fungal, treatment of hypoglycemia and physiological disorders and other effects (CN1760185). Difluoroacetic acid can also be used in rapamycin and its derivatives for the treatment and prevention of cardiovascular disorders, tumors, anti-rejection of organ transplantation and the treatment of autoimmune diseases such as rheumatoid arthritis, lupus erythematosus, and psoriasis. In addition, using difluoroacetic acid as a raw material, many fine chemical intermediates can be prepared (US6946025). Difluoroacetic acid and its anhydride can also be used as catalysts for reactions such as esterification and acy...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J23/10C07C53/48C07C51/58
Inventor 李宏峰周强王树华叶立峰
Owner JUHUA GRP
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