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Preparation method and application of theta-AlF3 micro-nano-spherical catalyst

A technology of micro-nanospheres and catalysts, which is applied in the direction of physical/chemical process catalysts, dehydrohalogenation preparation, chemical instruments and methods, etc., which can solve the limitations of catalytic performance improvement, complex preparation methods, and difficulty in obtaining high-quality trifluoroethylene products, etc. problems, achieve the effects of shortening the fluorination time, high production efficiency, and short production cycle

Active Publication Date: 2018-01-09
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production methods of trifluoroethylene mainly include (1) gas-phase catalytic hydrodechlorination, such as using 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113) as raw material, and using group VIII Metals, transition metals, etc. are catalytically active components, and the porous material Al 2 o 3 、TiO 2 etc. are carriers for catalytic hydrodechlorination [CN01133432]; but this process is mainly based on the production of chlorotrifluoroethylene, and it is difficult to obtain high-quality trifluoroethylene products
All these methods are complicated to prepare and produce dense α-AlF 3 or amorphous AlF 3 , thus limiting the catalytic performance improvement
[0005] The present invention is prepared based on the dissolution-roasting method θ Phase aluminum fluoride micro-nanospheres, no report

Method used

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  • Preparation method and application of theta-AlF3 micro-nano-spherical catalyst
  • Preparation method and application of theta-AlF3 micro-nano-spherical catalyst
  • Preparation method and application of theta-AlF3 micro-nano-spherical catalyst

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Experimental program
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Effect test

Embodiment 1

[0024] Take 6g of aluminum nitrate and 6g of PVDF, and dissolve them in 40mL of DMF under the condition of heating and stirring in a water bath at 70°C. After the dissolution is complete, a colorless and transparent gel-like precursor solution is formed, and the above-mentioned gel-like precursor solution is placed in a blast drying oven for 100 Dry at ℃ for 24 hours, remove the organic solvent, then calcinate the completely dried solid in a muffle furnace, the calcination temperature is 300 ℃, the heating rate is 5 ℃ / min, and keep at the calcination temperature for 12 hours, and finally cool naturally in the air atmosphere , that is, 1.9 g of aluminum fluoride was obtained, and then it was crushed to 20-40 mesh (0.45-0.9mm) after being pressed into a tablet at 15MPa to obtain a catalyst precursor.

Embodiment 2

[0026]Take 4g of aluminum nitrate and 6g of PVDF, and dissolve them in 40mL of DMF under the condition of heating and stirring in a water bath at 70°C. After the dissolution is complete, a colorless and transparent gel-like precursor solution is formed, and the above-mentioned gel-like precursor solution is placed in a blast drying oven for 120 Dry at ℃ for 36 hours, remove the organic solvent, then calcinate the completely dried solid in a muffle furnace, the calcination temperature is 390 ℃, the heating rate is 5 ℃ / min, and keep at the calcination temperature for 10 hours, and finally cool naturally in the air atmosphere , that is, 1.2g of aluminum fluoride is obtained, and then it is crushed to 20-40 mesh (0.45-0.9mm) after being pressed into a tablet at 15MPa to obtain a catalyst precursor.

Embodiment 3

[0028] Take 3g of aluminum nitrate and 6g of PVDF, and dissolve them in 40mL of DMF under the condition of heating and stirring in a water bath at 70°C. After the dissolution is complete, a colorless and transparent gel-like precursor solution is formed, and the above-mentioned gel-like precursor solution is placed in a blast drying oven for 120 Dry at ℃ for 24 hours, remove the organic solvent, then calcinate the completely dried solid in a muffle furnace, the calcination temperature is 450 ℃, the heating rate is 10 ℃ / min, and keep at the calcination temperature for 5 hours, and finally cool naturally in the air atmosphere , that is, 0.8g of aluminum fluoride, 15MPa tablet molding and then crushing it to 20-40 mesh (0.45-0.9mm) to get the catalyst precursor, the scanning electron microscope (SEM) picture of the prepared aluminum fluoride is as follows Figure 2 shows. It can be seen from Fig. 2 that the morphology of the product is a uniform micro-nanosphere with a size of abo...

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Abstract

The invention relates to a preparation method of a theta-AlF3 micro-nano-spherical catalyst and an application of the theta-AlF3 micro-nano-spherical catalyst to catalytic cracking of 1,1,1,2-tetrafluoroethane for preparation of trifluoroethylene. The preparation method of the theta-AlF3 micro-nano-spherical catalyst comprises the following steps: a fluorine-containing polymer is dissolved in an organic solvent under heating and stirring conditions, then aluminium salt is added to the polymer solution and stirred to be dissolved completely, and a colorless transparent gel-like precursor solution is formed; drying is performed to remove the organic solvent, calcining treatment is performed, and the AlF3 catalyst is obtained. The AlF3 catalyst synthesized with the method has higher catalyticactivity and good stability in a cracking reaction for preparing trifluoroethylene from 1,1,1,2-tetrafluoroethane, the process is simple, a few operation steps are required, the efficiency is high, equipment requirements are low, and repeatability is good.

Description

technical field [0001] The invention belongs to the technical field of preparation of metal fluoride micro-nano catalysts, and specifically relates to a θ -AlF 3 Preparation method and application of micro-nanosphere catalyst. Background technique [0002] As a second-generation refrigerant, 1,1,1,2-tetrafluoroethane (HFC-134a) is widely used in automobile air conditioners, home appliances and industrial and commercial refrigeration equipment. HFC-134a is the most important refrigerant at present. Although it will not destroy the ozone layer, its GWP value is as high as 1300, and its global warming potential value is very high. Extensive use will cause global warming. At present, its use has also entered the Countdown phase. [0003] Trifluoroethylene (TrFE) is an important polymer basic structure unit, which can be used to synthesize fluorine-containing resins, fine chemicals and functional high-molecular fluoropolymers with excellent performance. The production methods...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/12B01J35/08C07C17/25C07C21/18C01F7/50
Inventor 韩文锋习苗王海丽周胜兰唐浩东王志昆
Owner 浙江诺亚氟化工有限公司
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