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Method for preparing chromium-based fluorination catalyst by utilizing waste chromic acid washing liquid

A technology of base fluorination catalyst and chromic acid lotion is applied in the field of preparing chromium based fluorination catalyst by using waste chromic acid lotion, which can solve the problems of long drying time, catalyst impregnation, etc. The effect of good sex and high activity

Pending Publication Date: 2018-09-28
HUBEI HONGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the hazards of waste chromic acid lotion in existing laboratories and the long time required for catalyst impregnation and drying in existing experimental methods, the present invention provides a method for preparing a chromium-based fluorination catalyst suitable for gas-phase fluorination reactions

Method used

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  • Method for preparing chromium-based fluorination catalyst by utilizing waste chromic acid washing liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Measure 500ml of waste chromic acid lotion, add 500ml of absolute ethanol, stir for 2 hours, add 30.35g of Al(NO3)3 9H2O, 5.45g of glucose and 6.50g of zinc chloride, stir and mix evenly, add 10% ammonia water to adjust the pH value Adjust to 8, age at 65oC for 4h, filter and wash, dry at 105oC for 4h, and then roast at 450oC for 6h.

Embodiment 2

[0026] Measure 500ml of waste chromic acid lotion, add 500ml of absolute ethanol, stir for 2 hours, add 30.35g of Al(NO3)3 9H2O, 5.45g of glucose, 6.50g of zinc chloride and 3.18g of magnesium chloride, stir and mix evenly, then add 10% The pH value was adjusted to 8 with ammonia water, aged at 65oC for 4h, filtered and washed, dried at 105oC for 4h, and then calcined at 450oC for 6h.

Embodiment 3

[0028] Measure 500ml of waste chromic acid lotion, add 500ml of absolute ethanol, stir for 2 hours, add 30.35g of Al(NO3)3 9H2O, 5.45g of glucose, 6.50g of zinc chloride and 3.16g of CoCl2 6H2O, stir and mix evenly, then add 10 % ammonia water to adjust the pH value to 8, age at 65oC for 4h, filter and wash, dry at 105oC for 4h, and then roast at 450oC for 6h. After roasting, the material is pulverized and pressed into tablets to obtain a catalyst precursor;

[0029] The above-mentioned catalyst precursor is loaded into a reactor, and a mixed gas of nitrogen and anhydrous hydrogen fluoride is introduced to carry out fluorination at 350°C to obtain a fluorination catalyst.

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Abstract

The invention discloses a method for preparing a chromium-based fluorination catalyst by utilizing a waste chromic acid washing liquid. The method comprises the following steps: preparing a chromium-based salt solution by using the waste chromic acid washing liquid, preparing a catalyst precursor, and performing fluorination. The method disclosed by the invention adopts the waste chromic acid washing liquid obtained after residual organic matter is cleaned as a raw material and solves the problems that the waste chromic acid washing liquid is difficult to handle and has damage to the environment; a carrier active metal of a prepared catalyst has a large effective loading capacity and high activity; and active components of the catalyst are not easy to loss, and the catalyst has good repeatability and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to the preparation and application of a fluorination catalyst, in particular to a chromium-based fluorination catalyst for the nucleophilic substitution reaction of straight-chain chlorinated hydrocarbons and derivatives thereof, especially chromium for the catalytic preparation of R134a Based fluorination catalyst and its preparation method. Background technique [0002] At present, the industry mainly adopts gas-phase fluorination reaction to synthesize chlorofluorocarbons (CFCs), and produces fluorocarbons through fluorine-chlorine exchange reaction. The method is easy to control, has a long service life of the catalyst and low pollutant emission, and is widely applicable to large-scale industrial production. The core technology of preparing fluorocarbons is the catalyst used in the gas-phase fluorination process. Chromium-based catalysts are widely used due to their higher catalytic activity and stability in the gas-p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/26B01J23/86B01J37/03B01J37/08C07C17/20C07C19/08
CPCC07C17/206B01J23/26B01J23/864B01J37/03B01J37/082C07C19/08
Inventor 舒伟锋贾雪枫尹国平邓支华张响飞肖鹏
Owner HUBEI HONGYUAN PHARMA