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Catalyst used in preparation of fluorine-containing olefin through dehydrohalogenation of halohydrofluoroalkane and preparation method of catalyst

A technology for dehydrohalogenation and halofluoroalkanes, which is applied in the field of highly active catalysts and their preparation, can solve the problems of difficult large-scale preparation of fluorine-containing olefins, poor selectivity of target fluoroolefins, easy carbon deposition and deactivation, etc., and achieve the target product High yield, good resistance to carbon deposition, and high dehydrohalogenation selectivity

Active Publication Date: 2012-12-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The gas-phase dehydrohalogenation catalysts reported above have poor selectivity of target fluoroolefins, low conversion rate and easy carbon deposition and deactivation during their use, making them difficult to apply in the process of large-scale preparation of fluorinated olefins

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve the mixture of magnesium nitrate and calcium chloride in water, add the precipitant NH at 80°C 3 ·H 2 O, control the pH of the solution within 8.5 to 9.5, make it fully precipitate under stirring, filter the precipitated solid with suction, wash it to neutral with deionized water, and then dry it overnight at 110°C to obtain the complex Mg(OH ) 2 -Ca(OH) 2 matrix;

[0020] Dissolve the mixture of ferric chloride and lanthanum chloride in water to make impregnating solution, add complex Mg(OH) 2 -Ca(OH) 2 The substrate was immersed at 50°C for 6h, the solution was filtered off, the catalyst precursor was dried at 120°C for 12h, and calcined in a muffle furnace at 400°C for 6h. The mass percentage of the prepared catalyst was: 2wt.%Fe-1wt. %La / 60wt.%MgO-CaO.

[0021] 60mL of the above catalyst (2wt.%Fe-1wt.%La / 60wt.%MgO-CaO) was loaded into a nickel tube fixed-bed tubular reactor with an inner diameter of 38mm, the reaction temperature was 350°C, and the sp...

Embodiment 2

[0023] The preparation process of the catalyst is basically the same as in Example 1, except that calcium chloride is changed into barium chloride, ferric chloride is changed into aluminum chloride, lanthanum chloride is changed into cerium nitrate, and the mass percentage of the prepared catalyst is composed of : 3wt.%Al-2wt.%Ce / 80wt.%MgO-BaO.

[0024] In a nickel-tube fixed-bed tubular reactor with an inner diameter of 38 mm, 60 mL of the catalyst prepared above (3wt.%Al-2wt.%Ce / 80wt.%MgO-BaO) was loaded, the reaction temperature was 350°C, HFC-245fa Airspeed 50min -1 , The reaction continued to run for 100h, and the gas product was washed with water, washed with alkali and dried, and analyzed by gas chromatography. The average conversion rate of HFC-245fa was 85%, and the selectivity of HFO-1234ze was 95%.

Embodiment 3

[0026] The preparation process of the catalyst is basically the same as in Example 1, except that the ferric chloride is changed into zirconium chloride, and the lanthanum chloride is changed into iridium nitrate, and the mass percentage of the prepared catalyst is composed of: 5wt.%Zr-1wt.% Ce / 50wt.%MgO-CaO.

[0027] In a nickel-tube fixed-bed tubular reactor with an inner diameter of 38 mm, 60 mL of the prepared catalyst (5wt.%Zr-1wt.%Ce / 50wt.%MgO-CaO) was loaded, and the reaction temperature was 350°C, 2,3 -Space velocity of dichloro-1,1,1-trifluoropropane 50min -1 , the reaction was run continuously for 100h, and the gas product was analyzed by gas chromatography after being washed with water, alkali washed and dried. The average conversion rate of 2,3-dichloro-1,1,1-trifluoropropane was 97%, 1-chloro-3, The selectivity of 3,3-trifluoropropene is 99%.

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Abstract

The invention discloses a catalyst used in preparation of fluorine-containing olefin through dehydrohalogenation of halohydrofluoroalkane. The catalyst is represented as nwt. %Y / X, wherein Y represents a catalyst promoter and is one or more selected from alkali metal ions Na<+>, K<+> and Cs<+>, rare earth metal ions La<3+>, Ce<4+>, Y<3+> or high-valence metal ions Al<3+>, Fe<3+>, Ti<4+> and Zr<4+>; X represents a main active ingredient and is one or a mixture of more of alkali metal magnesium, calcium and / or barium oxide; n is the using amount of the catalyst promoter and accounts for 30 percent of the main active ingredient at most; and the catalyst is mainly used for preparation of the fluorine-containing olefin through gas-phase dehydrohalogenation of the halohydrofluoroalkane.

Description

technical field [0001] The invention relates to a catalyst, in particular to a highly active catalyst for preparing fluorine-containing olefins by gas-phase catalytic dehydrohalogenation of halofluoroalkanes and a preparation method thereof. Background technique [0002] Fluoroolefins, 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 New organic fluorides with potential value (ODP) and low GWP value have been considered as the best substitutes for the widely used HFCs at present, as blowing agents, refrigerants, aerosol propellants, solvents, etc. [0003] Fluorinated olefins can be prepared by gas-phase catalytic dehydrohalogenation of halofluoroalkanes, such as dehydrochlorination of 1,1,1,2-tetrafluoro-2-chloropropane (HCFC-244bb) to obtain HFO-1234yf, 1,1,1,3 , 3-pentafluoropropane (HFC-245fa) dehydrofluorination to obtain HFO-1234ze. The method has the advantages...

Claims

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Application Information

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IPC IPC(8): B01J23/83B01J23/10C07C17/25C07C21/18
Inventor 毛伟王博
Owner XIAN MODERN CHEM RES INST
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