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Preparation method of nanometer aluminum fluoride-based catalyst

A technology of aluminum fluoride and catalyst, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of complex process, amorphous structure of aluminum fluoride, high energy consumption, etc., and meet the preparation conditions Mild, catalytic reaction, simple operation

Active Publication Date: 2016-05-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The aluminum fluoride preparation method of above-mentioned report still has following problem at least: (1) anhydrous sol-gel fluorination method is that the organic solvent of metal source and anhydrous HF is fluorine source with expensive organic metal, and This method must be operated under anhydrous conditions, the process is complicated, and it is difficult to apply to industrial production. At the same time, the aluminum fluoride obtained has an amorphous structure, is unstable at high temperatures, and is easy to crystallize into fluorides with low specific surface area; (2) carbon fluoride method Although the raw materials are easy to obtain, the process is complicated, and high-temperature carbonization and carbon removal processes need to be repeated, and the energy consumption is high. When the temperature is higher than 350°C, the specific surface area of ​​aluminum fluoride drops rapidly to 30m 2 / g or so; (3) Although the silicon dioxide fluorination method is easy to get raw materials and easy to operate, the silicon tetrafluoride gas generated is easy to cool and condense and block the pipeline, so it is not suitable for industrial production

Method used

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  • Preparation method of nanometer aluminum fluoride-based catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Embodiment 1: Preparation of large specific surface area, nano aluminum fluoride

[0049] Dissolve 0.5M aluminum source in 50mL organic solvent, reflux at 20-80°C for 6 hours, then slowly add the fluorinated reagent aqueous solution to the above solution with stirring, and the dropping time is 1 hour. Stir for another 6 hours to obtain a liquid sol; then statically age at 60-90°C for more than 24 hours to obtain a solid gel; then dry at 100-160°C for more than 24 hours, and finally roast at 350-450°C for more than 4 hours to obtain a high-temperature High specific surface area, nanocrystalline aluminum fluoride. The texture properties of aluminum fluoride prepared under different aluminum sources, organic solvents, fluorinating reagents, and calcination temperatures are shown in Table 1.

[0050] The physical and chemical property results of aluminum fluoride in Example 1 of table 1

[0051]

[0052]

Embodiment 2

[0053] Embodiment 2: Preparation of large specific surface area, nano aluminum fluoride

[0054] Dissolve 0.5M aluminum nitrate in 50mL of ethylene glycol, reflux at 60°C for 6 hours, then slowly add HF aqueous solution to the above solution dropwise with stirring, the dropping time is 1 hour, and then stir for 6 hours after the dropping is completed , to obtain a liquid sol; then aged at 90°C for more than 24 hours to obtain a solid gel; then dried at 150°C for more than 24 hours, and finally roasted at 400°C for more than 4 hours to obtain a nanocrystalline fluoride with a large specific surface area at high temperature Aluminum based catalysts. The textures of aluminum fluoride-based catalysts prepared with different amounts of fluorinating reagents are shown in Table 2.

[0055] The physical and chemical property results of aluminum fluoride in embodiment 2 of table 2

[0056]

Embodiment 3

[0057] Example 3: Preparation of large specific surface area, nano-aluminum fluoride-based catalyst

[0058] Dissolve 0.5M aluminum nitrate and doping components in 50mL of ethylene glycol, and reflux at 60°C for 6h with stirring, then slowly add HF aqueous solution into the above solution dropwise with stirring for 1h, dropwise Stir for 6 hours after completion to obtain a liquid sol; then statically age at 90°C for more than 24 hours to obtain a solid gel; then dry at 150°C for more than 24 hours, and finally roast at 400°C for more than 4 hours to obtain a large specific surface area at high temperature , Nanocrystalline aluminum fluoride-based catalyst. The specific surface areas of aluminum fluoride-based catalysts prepared with different doping components are shown in Table 3.

[0059] The physicochemical property result of the aluminum fluoride-based catalyst of table 3 embodiment 3

[0060]

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Abstract

The invention discloses a nanometer aluminum fluoride-based catalyst with large specific surface area, and a preparation method and applications thereof. The preparation method is used for solving problems in conventional preparation methods of aluminum fluoride-based catalysts that high temperature specific area is small, thermal stability is poor, and the conventional preparation method is complex, and is high in cost. The preparation method comprises following steps: (1) a solution containing an aluminium source precursor, an organic solvent, and a doping ingredient is prepared, and is subjected to refluxing at 20 to 80 DEG C; (2 ) an aqueous solution of a fluorinating reagent is added into the solution obtained in (1) dropwise for fluorination, and a liquid sol is obtained via aging at 60 to 90 DEG C; and (3) the liquid sol is dried at 100 to 160 DEG C so as to obtain a solid gel, and roasting is carried out at 350 to 450 DEG C so as to obtain the nanometer aluminum fluoride-based catalyst.

Description

technical field [0001] The invention relates to a nano-aluminum fluoride catalyst, in particular to a mild and simple preparation method of a nano-crystal aluminum fluoride catalyst with a large specific surface area at high temperature. Background technique [0002] In the gas-phase catalytic synthesis of fluorine-containing halogenated hydrocarbons, such as the preparation of the third-generation refrigerant hydrofluorocarbons (HFCs) and the fourth-generation refrigerant hydrofluoroolefins (HFOs), strong corrosive HF or one of the reactants 1. It may be generated during the reaction, so the catalyst used must be a material that can exist stably in a high-temperature HF atmosphere. So far, aluminum fluoride has been proved to be stable for a long time in the above-mentioned strong corrosive atmosphere, and it is an important catalytic active component or carrier for the preparation of fluorine-containing halogenated hydrocarbons. However, if aluminum fluoride is to be used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/125
Inventor 毛伟吕剑白彦波王博徐强王伟杜咏梅石磊秦越杨志强
Owner XIAN MODERN CHEM RES INST
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