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Method for preparing magnesium-based catalyst for 1,3,3,3-tetrafluoropropylene through dehydrofluorination of 1,1,1,3,3-perfluoropropane

A technology for dehydrofluorination and tetrafluoropropene, which is applied in the direction of dehydrohalogenation preparation, physical/chemical process catalyst, catalyst activation/preparation, etc., can solve the problems of catalyst deactivation and increased separation cost, and achieve high catalytic activity and good life , highly selective effect

Inactive Publication Date: 2019-03-22
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, precious metal compounds are used in the catalyst preparation process, and diluent gases such as nitrogen gas need to be introduced during the reaction process, which increases the subsequent separation cost, and the catalyst is obviously deactivated during the reaction process.

Method used

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  • Method for preparing magnesium-based catalyst for 1,3,3,3-tetrafluoropropylene through dehydrofluorination of 1,1,1,3,3-perfluoropropane
  • Method for preparing magnesium-based catalyst for 1,3,3,3-tetrafluoropropylene through dehydrofluorination of 1,1,1,3,3-perfluoropropane
  • Method for preparing magnesium-based catalyst for 1,3,3,3-tetrafluoropropylene through dehydrofluorination of 1,1,1,3,3-perfluoropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 1 mol of magnesium source, a certain amount of active components and the same mass of complexing agent in 50 mL of polyol, and form a colorless and clear solution after a water bath temperature of 60°C and magnetic stirring; add a metered ratio of 40wt.% hydrofluoric acid, Continue the reaction for 6h; after aging at 80℃~100℃ for 24h, a solid gel is obtained; continue to dry at 110~150℃ to obtain magnesium fluoride xerogel, which is ground into powder, and finally calcined at 400℃ for 5h to obtain catalyst powder. Re-granulation, that is, the magnesium-based catalyst is prepared by the bulk doping method. The catalyst was applied to the HFC-245fa gas-phase dehydrofluorination synthesis reaction of HFO-1234ze. After running for 24 hours, the reaction results are shown in Table 1.

[0026] The active components introduced in Example 1 were Al(NO 3 ) 3 ·9H 2 O, Cr(NO 3 ) 3 ·9H 2 O, Zn(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O,...

Embodiment 2

[0031] The active component introduced in this example is Al(NO 3 ) 3 ·9H 2 O, the molar ratio of active component to carrier ranges from 0.05 to 0.3.

[0032] The catalyst performance evaluation conditions are the same as in Example 1, and the catalyst evaluation results are shown in Table 2.

[0033] Table 2

[0034] Numbering

Embodiment 3

[0036] Take 20% Al / MgF numbered 4 in Example 2 2 The catalyst was subjected to a life test. The catalyst performance evaluation conditions were the same as in Example 1. The reaction was continuously run for 1000 hours. The evaluation results are shown in Table 3.

[0037] table 3

[0038]

[0039]

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Abstract

The invention discloses a method for preparing a magnesium-based catalyst for 1,3,3,3-tetrafluoropropylene through dehydrofluorination of 1,1,1,3,3-perfluoropropane. The composition of the catalyst is: n%X / MgF2, wherein X represents an active component and is selected from soluble salt of Al, Cr, Zn, Fe, Ni or Co; n represents the use amount of the active component; a magnesium fluoride carrier isprepared by a polyalcohol fluorination method; the active component is introduced into the catalyst by a bulk phase doping method; and the catalyst is mainly applied to, but not limited to, preparation of fluorine-containing olefin.

Description

Technical field [0001] The invention relates to a series of dehydrofluorination catalysts, in particular to a magnesium-based catalyst used for the dehydrofluorination of 1,1,1,3,3-pentafluoropropane to prepare 1,3,3,3-tetrafluoropropene. Background technique [0002] HFO-1234ze (1,3,3,3-tetrafluoropropene) is non-flammable, with an ODP value of 0 and a GWP value of 6. Studies have found that HFO-1234ze can directly replace HFC-134a in single-component foams and aerosols, so it has a very large application prospect. At present, the synthesis of HFO-1234ze is mainly divided into 1,1,1,3,3-pentafluoropropane (HFC-245fa) as the raw material dehydrofluorination method, trifluoropropyne direct addition method, and trifluorochloropropene direct substitution method And thermal cracking method, among which HFC-245fa gas phase dehydrofluorination to prepare HFO-1234ze has a simple synthesis route and high target product yield, which is the most promising synthesis route. [0003] Luo Meng...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/138B01J35/10B01J37/26B01J37/08C07C17/25C07C21/18
CPCC07C17/25B01J27/138B01J37/082B01J37/26B01J35/615C07C21/18
Inventor 贾兆华吕剑毛伟王博白彦波李晨田松杨志强郝志军
Owner XIAN MODERN CHEM RES INST
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