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Magnesium fluoride-based catalyst and application of magnesium fluoride-based catalyst

A magnesium fluoride-based catalyst and catalyst technology, applied in the direction of physical/chemical process catalysts, dehydrohalogenation preparation, chemical instruments and methods, etc., can solve the problems of thermal stability deterioration, poor thermal stability, small specific surface area, etc., to achieve Rich pore structure, high thermal stability, and large specific surface area

Inactive Publication Date: 2015-03-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned magnesium fluoride-based catalysts for dehydrohalogenation have the problems of small specific surface area and poor thermal stability.
More importantly, the thermal stability of magnesium fluoride catalysts deteriorates sharply above 400 °C, the grains grow rapidly, and the specific surface area decreases sharply, resulting in a decrease in dehydrohalogenation reaction activity, which is difficult to apply to continuous high-temperature gas-phase preparation of fluorine-containing olefins

Method used

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  • Magnesium fluoride-based catalyst and application of magnesium fluoride-based catalyst
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  • Magnesium fluoride-based catalyst and application of magnesium fluoride-based catalyst

Examples

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Embodiment 1

[0060] Example 1: Preparation of magnesium fluoride with high thermal stability and large specific surface area by liquid phase fluorination

[0061] Dissolve the mixture of 30.0g metallic magnesium insoluble salt and 15.0g surfactant in 200mL of water, and reflux the suspension at 100°C for 6h while stirring, then suction filter to obtain a solid, wash it with deionized water until neutral, Then it was dried at 100°C overnight to obtain a magnesium oxide precursor. Then the former body was roasted in a muffle furnace for 6 hours to obtain magnesium oxide with a large specific surface area. Slowly add the aqueous solution of fluorinating reagent dropwise to the aqueous solution containing the above-mentioned magnesia, then suction filter to obtain a solid, wash it with deionized water until it is neutral, then dry it at 100°C overnight, and put the former body in a muffle furnace Calcined for 4h to obtain magnesium fluoride.

[0062] Catalyst N 2 Adsorption and desorption p...

Embodiment 2

[0066] Dissolve 8.0g of alkali metal chlorides of Li, Na, K, Rb, and Cs in 100ml of distilled water to make a solution, and then add 2 / g of magnesium fluoride with large specific surface area, impregnated for 4 hours, dried at 80°C for more than 12 hours, and then roasted the precursor in a muffle furnace at 400°C for 6 hours to obtain a magnesium fluoride-based dehydrohalogenation catalyst.

[0067] A series of alkali metal-doped magnesium fluoride catalysts prepared were used as dehydrochlorination catalysts, and 60ml of catalysts were loaded into a fixed-bed tubular reactor with a diameter of Φ38mm. At a reaction temperature of 400°C, 2-chloro -1,1,1,2-Tetrafluoropropane passes through the catalyst bed with a residence time of 30s. The product is washed with water and alkali to remove HCl and HF, and then analyzed by gas chromatography. The analysis method is the area normalization method. After 24 hours of reaction, the results of dehydrochlorination are shown in Table 2...

Embodiment 3

[0071] Dissolve 12.0g of sulfates of transition metals Cr, Al, Fe, Zr in 100ml of distilled water to make a solution, and then add 2 / g of magnesium fluoride with large specific surface area, impregnated for 6 hours, dried at 100°C for more than 12 hours, and then roasted the precursor in a muffle furnace at 500°C for 6 hours to obtain a magnesium fluoride-based dehydrohalogenation catalyst.

[0072] The prepared series of transition metal-doped magnesium fluoride-based catalysts were used as dehydrofluorination catalysts, and 60ml of catalysts were loaded into a fixed-bed tubular reactor with a diameter of Φ38mm. At a reaction temperature of 350°C, 1, 1,1,3,3-Pentafluoropropane passes through the catalyst bed with a residence time of 30s. The product is washed with water and alkali to remove HCl and HF, and then analyzed by gas chromatography. The analysis method is the area normalization method. After reacting for 24 hours, the results of dehydrofluorination are shown in Ta...

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Abstract

The invention discloses a magnesium fluoride-based catalyst which is stable at the temperature of over 400 DEG C and large in specific surface area and application of the magnesium fluoride-based catalyst. The invention aims at solving the problems such as low thermal stability and small specific surface area existing in the preparation of the magnesium fluoride-based catalyst in the prior art. The method for preparing the magnesium fluoride-based catalyst disclosed by the invention comprises the following steps: (1) preparing a turbid liquid solution containing a magnesium metal insoluble salt and a surfactant, refluxing at the temperature of 100 DEG C, roasting under the condition of 400-550 DEG C for 4 hours, thereby obtaining magnesium oxide with the large specific surface area; (2) dropwise adding an aqueous solution of hydrofluoric acid or ammonium fluoride into the magnesium oxide base body obtained in the step (1) for fluorinating, roasting at the temperature of 400-500 DEG C for 4 hours, thereby preparing magnesium fluoride; and (3) dropwise adding the aqueous solution doped with components into the magnesium oxide base body obtained in the step (2), and finally roasting at the temperature of 400-500 DEG C so as to prepare the catalyst. According to the catalyst disclosed by the invention, high-efficiency dehydrohalogenation reaction can be realized by virtue of halofluoroalkane.

Description

technical field [0001] The invention relates to a magnesium fluoride-based catalyst and a preparation method thereof, in particular to a magnesium fluoride-based catalyst for preparing fluorine-containing olefins from halofluoroalkanes under gas phase conditions and a preparation method thereof. Background technique [0002] Fluorinated olefins, especially hydrofluoroolefins, such as 2,3,3,3-tetrafluoropropene (HFO-1234yf), 1,3,3,3-tetrafluoropropene (HFO-1234ze) are a class of zero ozone depleting Novel organic fluorine compounds with low potential value (ODP) and low GWP value have been considered as the best substitutes for the widely used HFCs at present, as refrigerants and other applications. [0003] Vapor-phase dehydrohalogenation of halofluoroalkanes is an important method for the laboratory and industrial preparation of fluorinated alkenes. The method has the advantages of simple equipment, easy continuous mass production, and safety. The dehydrohalogenation cata...

Claims

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Application Information

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IPC IPC(8): B01J27/138C07C17/25C07C21/18
CPCB01J21/10B01J23/78B01J23/80B01J27/12C07C17/25C07C21/18
Inventor 吕剑毛伟白彦波秦越王博万洪王志轩杜咏梅李春迎李凤仙
Owner XIAN MODERN CHEM RES INST
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