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Activation method of alpha-AlF3

A technology of anhydrous hydrogen fluoride and carbonate, applied in chemical instruments and methods, physical/chemical process catalysts, aluminum fluoride, etc., can solve the problems of low production efficiency and difficulty in meeting the catalyst dosage, and achieve high production efficiency and good production conditions mild effect

Active Publication Date: 2020-09-01
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method yields nanostructured active AlF 3 , the preparation efficiency is too low, it is difficult to meet the requirements of industrial gas-phase catalytic reaction on the large amount of catalyst

Method used

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  • Activation method of alpha-AlF3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Fill 10 ml of α-AlF in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30 cm 3 (commercially available, the specific surface area is 2.38m 2 / g). The temperature of the reactor was raised to 400°C, and HF and dimethyl ether were introduced to react. The molar ratio of HF and dimethyl ether was controlled to be 1:8, the contact time was 10 seconds, and the reaction pressure was normal pressure. After 40 hours of reaction, the reaction product passed Washed with water, washed with alkali, separated to obtain organic matter, after drying to remove water, the composition of organic matter was analyzed by gas chromatography, the conversion rate of dimethyl ether was 75%, and the selectivity of fluoromethane was 98%; the obtained γ-AlF 3 The catalyst was cooled to room temperature under the protection of nitrogen, and the BET test was performed, and the specific surface area was 17.36m 2 / g, then carry out XRD detection, the test res...

Embodiment 2

[0040] Fill 10 ml of α-AlF in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30 cm 3 (commercially available, the specific surface area is 2.38m 2 / g). The temperature of the reactor was raised to 400°C, and HF and dimethyl carbonate were introduced to react. The molar ratio of HF and dimethyl carbonate was controlled to be 1:8, the contact time was 10 seconds, and the reaction pressure was normal pressure. After 40 hours of reaction, the reaction The product is washed with water and alkali, and the organic matter is separated. After drying and removing water, the composition of the organic matter is analyzed by gas chromatography. The conversion rate of dimethyl carbonate is 80%, and the selectivity of fluoromethane is 97%. γ-AlF 3 The catalyst was cooled to room temperature under the protection of nitrogen, and the BET test was performed, and the specific surface area was 30.95m 2 / g, then carry out XRD detection, the test results...

Embodiment 3

[0042] Fill 10 ml of α-AlF in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30 cm 3 (commercially available, the specific surface area is 2.38m 2 / g). The temperature of the reactor was raised to 400°C, and HF and vinylene carbonate were introduced to react. The molar ratio of HF and vinylene carbonate was controlled to be 1:12, the contact time was 7 seconds, and the reaction pressure was normal pressure. After 40 hours of reaction, the reaction The product was washed with water and alkali, and the organic matter was separated. After drying and removing water, the composition of the organic matter was analyzed by gas chromatography. The conversion rate of vinylene carbonate was 64%, and the selectivity of 1,2-difluoroethylene was 93%; γ-AlF obtained after treatment 3 The catalyst was cooled to room temperature under the protection of nitrogen, and the BET test was performed, and the specific surface area was 16.54m 2 / g.

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Abstract

The invention relates to an activation method of alpha-AlF3 and belongs to the field of chemical engineering. According to the activation method, alpha-AlF3 is treated for a certain time at a certaintemperature in a gas-phase atmosphere of ether and anhydrous hydrogen fluoride or carbonate and anhydrous hydrogen fluoride, so that alpha-AlF3 can be partially or even completely converted into gamma-AlF3. According to the method, the alpha-AlF3 can be activated and converted into the gamma-AlF3 to be reused, emission of solid waste AlF3 is reduced, and fluorine-containing alkane or fluorine-containing olefin with high additional value can be produced at the same time.

Description

technical field [0001] The present invention relates to a kind of ɑ-AlF 3 Converted to γ-AlF by gas phase fluorination 3 method, especially in the presence of either ether or carbonate and HF, for ɑ-AlF 3 Perform regeneration treatment to obtain γ-AlF 3 Methods. Background technique [0002] AlF 3 There are multiple crystal phase structures such as α, β, γ, η, κ and amorphous phase. Among them, β-AlF 3 , γ-AlF 3 and amorphous AlF 3 It has high catalytic activity and belongs to active AlF 3 . Active AlF 3 As a catalyst, it is widely used in fluorine-chlorine exchange reaction, and can also be used as a catalyst carrier in gas-phase hydrogenation, isomerization and other reactions. However, during use, the active AlF 3 inert α-AlF 3 transformation, resulting in active AlF 3 Catalyst deactivation. Therefore, in industrial production, ɑ-AlF is often 3 As solid waste to be treated, environmental protection is under great pressure. [0003] ɑ-AlF 3 The surface fl...

Claims

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Application Information

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IPC IPC(8): C01F7/50B01J27/125C07C17/00C07C19/08C07C21/18
CPCC01F7/50B01J27/125C07C17/00C01P2002/72C01P2006/12C07C19/08C07C21/18Y02P20/584
Inventor 杨刚张呈平贾晓卿权恒道
Owner 泉州宇极新材料科技有限公司
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