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A kind of preparation method of gas phase dehydrofluorination catalyst

A dehydrofluorination and catalyst technology, which is applied in the field of preparation of dehydrofluorination catalysts, can solve the problems of low reaction selectivity and poor stability, and achieve the effects of simple process, low cost and high specific surface area

Active Publication Date: 2019-04-09
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the defects and deficiencies such as low reaction selectivity and poor stability in the prior art, the purpose of the present invention is to provide a preparation method for gas-phase dehydrofluorination catalyst to improve the selectivity and stability of the catalyst, especially to use Preparation method of catalyst for preparing fluorine-containing olefins from fluorine-containing alkanes under gas phase conditions

Method used

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Examples

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preparation example Construction

[0027] A method for preparing a gas-phase dehydrofluorination catalyst, the catalyst prepared by the invention is suitable for preparing fluorine-containing olefins by dehydrofluorination of fluorine-containing alkanes under gas-phase conditions, comprising the following steps:

[0028](1) First, under the protection of nitrogen at room temperature, weigh a certain amount of fresh magnesium bars and add them to absolute ethanol, control the reaction temperature to 80° C., and the reaction time to 1 h to obtain an ethanol suspension of magnesium ethoxide. Then, under the protection of nitrogen, slowly drop the obtained ethanol suspension of magnesium ethoxide into the ethanol solution of hydrogen fluoride. After completion, control the reaction temperature to 80°C and the reaction time to 10-20 hours. Then, after the reaction is finished, the reaction product is obtained through filtering, washing and drying. Finally, the reaction product is roasted under the protection of nit...

Embodiment 1

[0036] Step 1: Under the protection of nitrogen, first weigh 195 grams of fresh magnesium strips and add them to 600ml of absolute ethanol in batches. After adding the magnesium strips, control the temperature at 80°C for 1 hour to obtain the ethanol suspension of magnesium ethylate; Slowly add the prepared ethanol suspension of magnesium ethoxide to 825 grams of 40% hydrogen fluoride ethanol solution under the protection of nitrogen, control the dropping temperature at 60°C, and react at 80°C for 10 hours after the addition; finally filter and wash and drying, and roasting at 300°C under the protection of nitrogen to obtain a magnesium fluoride matrix with a high specific surface area.

[0037] The second step: first dissolve the chlorides containing 15 grams of Fe, Zr and Cr in 200ml distilled water to form a solution; Drying at ℃ for 8h; Finally, calcining at 300℃ for 10h to prepare the supported magnesium fluoride catalyst.

[0038] Step 3: Soak the prepared supported mag...

Embodiment 2

[0041] Step 1: Under the protection of nitrogen, weigh 200 grams of fresh magnesium strips and add them to 800ml of absolute ethanol in batches. After adding the magnesium strips, control the temperature at 70°C and react for 1 hour to obtain an ethanol suspension of magnesium ethylate; Slowly add the prepared ethanol suspension of magnesium ethoxide to 900 grams of 40% hydrogen fluoride ethanol solution under protection, control the dropping temperature at 60°C, and react at 80°C for 12 hours after the addition; finally filter, wash and Drying and calcining at 340° C. under the protection of nitrogen to obtain a magnesium fluoride matrix with a high specific surface area.

[0042] The second step: first dissolve the nitrates containing 45 grams of La, Cu, and Cr in 300ml distilled water to form a solution; Drying at ℃ for 9h; Finally, calcining at 340℃ for 14h to prepare the supported magnesium fluoride catalyst.

[0043] Step 3: Soak the prepared supported magnesium fluorid...

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Abstract

The invention discloses a preparation method for a gaseous-phase dehydrofluorination catalyst. The preparation method comprises the following steps: (1) enabling magnesium ethylate and hydrofluoric acid to react under the protection of nitrogen gas, carrying out refluxing at the temperature of 80 DEG C, and carrying out roasting at the temperature of 300-400 DEG C, so as to obtain a magnesium fluoride matrix with high specific surface area; (2) dipping the magnesium fluoride matrix with an aqueous solution of a supported component, and carrying out roasting at the temperature of 300-400 DEG C under the protection of nitrogen gas, so as to obtain a supported magnesium fluoride catalyst; and (3) treating and activating the catalyst with perfluorooctanoic acid. According to the preparation method, the magnesium fluoride matrix with high specific surface area and rich pore passage structures is prepared by adopting an anhydrous sol-gel fluorination method and then is supported with transition metal by adopting a dipping method so as to prepare the catalyst, and the catalyst is subjected to surface modification by perfluorooctanoic acid, so that the prepared catalyst is good in activity and high in gaseous-phase dehydrofluorination selectivity; and the reaction conditions are mild, so that reaction can be in long-term stable operation.

Description

technical field [0001] The invention relates to a preparation method and application of a gas-phase dehydrofluorination catalyst, in particular to a preparation method of a dehydrofluorination catalyst used for preparing fluorine-containing alkenes from fluorine-containing alkanes under gas-phase conditions. Background technique [0002] Hydrofluorocarbons (HFCs) have excellent physical and chemical properties, and the ozone depletion potential (ODP) is zero. They are widely used in refrigerants, cleaning agents, foaming agents, fire extinguishing agents, medicines and pesticides, and are very important in the national economy. basic chemical products. However, the greenhouse effect potential (GWP) of HFCs is high, and a large amount of use will cause global warming. Hydrofluoroolefins (HFOs), such as 2,3,3,3-tetrafluoropropene (HFO-1234yf), have similar physical and chemical properties to HFCs, have the advantages of zero ODP and low GWP, and are currently used on a large ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/138C07C17/25C07C21/18
Inventor 吴奕杨仲苗黄明星
Owner JUHUA GROUP TECH CENT
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