Preparation process of lithium aluminium hydride reduction

A technology of lithium aluminum hydride and aluminum salt, which is applied to various metal hydrides and other directions, can solve the problems of unsafety, many by-products, etc., and achieve the effects of simple production method, complete utilization, and reduced production cost.

Inactive Publication Date: 2005-12-28
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are still many by-products and potential unsafe problems in this step reaction.

Method used

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  • Preparation process of lithium aluminium hydride reduction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 241.43g of aluminum chloride hexahydrate and 42.41g of lithium chloride, add water to dissolve, add a certain amount of sodium carbonate solution, wait until the precipitation is complete, put it aside for suction filtration, dry the solid and then calcinate at a high temperature of 500-600°C After decomposing for 4 hours, the oxide was obtained, the oxide was in the autoclave, and CaH was added 2 As a catalyst, at 180°C and 20kg / cm 2 After hydrogenation of the solid under hydrogen pressure for 4-5 hours, a mixed element of aluminum and lithium is obtained. Adding catalyst naphthalene and TiCl in the organic solvent tetrahydrofuran 4 , hydrogenation at normal temperature and pressure by introducing hydrogen gas for 4-5 hours, and the lithium aluminum hydride product can be obtained.

[0018] Product analysis: The content analysis of Li, Al and H was carried out on this product. The analysis of Li was carried out by atomic absorption method; the analysis of Al wa...

Embodiment 2

[0021] Weigh 241.43g of aluminum chloride hexahydrate and 42.41g of lithium chloride, add water to dissolve, add a certain amount of sodium oxalate solution, wait until the precipitation is complete, put it aside for suction filtration, dry the solid and then calcinate at a high temperature of 500-600°C After decomposing for 4 hours, the oxide was obtained, the oxide was in the autoclave, and CaH was added 2 As a catalyst, at 180°C and 20kg / cm 2 After hydrogenation of the solid under hydrogen pressure for 4-5 hours, a mixed element of aluminum and lithium is obtained. Adding catalyst naphthalene and TiCl in the organic solvent tetrahydrofuran 4 , hydrogenation at normal temperature and pressure by introducing hydrogen gas for 4-5 hours, and the lithium aluminum hydride product can be obtained.

Embodiment 3

[0023] Weigh 375g of aluminum nitrate and 69g of lithium nitrate, add water to dissolve, add a certain amount of sodium oxalate solution, wait until the precipitation is complete, put it aside for suction filtration, and after the solid is dried, it is calcined at 500-600°C for 4 hours and then oxidized. material, the oxide in an autoclave, and adding CaH 2 As a catalyst, at 180°C and 20kg / cm 2 After hydrogenation of the solid under hydrogen pressure for 4-5 hours, a mixed element of aluminum and lithium is obtained. Adding catalyst naphthalene and TiCl in the organic solvent tetrahydrofuran 4 , hydrogenation at normal temperature and pressure by introducing hydrogen gas for 4-5 hours to obtain the lithium aluminum hydride product.

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Abstract

The invention relates to a metal hydride, in particular to a preparation method of lithium aluminum hydride. It is characterized in that soluble aluminum salt and lithium salt are used as raw materials, and a precipitant is added to the aqueous solution to make Al 3+ , Li + Ion co-precipitation; the precipitate is dried and pyrolyzed to obtain its oxide; the oxide is hydrogenated and reduced to obtain a mixed element of aluminum and lithium, and the mixed element is hydrogenated at normal temperature and pressure to obtain lithium aluminum hydride. The preparation process of the present invention has low temperature and normal pressure operation, which not only reduces energy consumption and eliminates potential dangers, but also has easy-to-obtain raw materials and simple process, and provides a new environmentally friendly clean production process for preparing lithium aluminum hydride.

Description

1. Technical field [0001] The invention relates to a metal hydride, in particular to a preparation method of lithium aluminum hydride. 2. Background technology [0002] Lithium aluminum hydride (LiAlH 4 ) was first synthesized in 1947. It is a strong reducing agent capable of reducing organic functional groups. The most typical method of synthesizing lithium aluminum hydride is to react lithium metal with hydrogen at high temperature to generate lithium hydride (LiH), then finely grind lithium hydride and react with aluminum trichloride in the presence of an initiator in anhydrous ether to form lithium aluminum hydride. Large-scale production is hindered due to the addition of initiators and the very fine particle size and flammability of lithium hydride. Later, it was proposed that under the condition of high-pressure hydrogen, metal and hydrogen react to produce metal complex hydrides, but this method has certain limitations due to a series of problems such as the reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B6/24
Inventor 张智敏王自为任建国马琦刘爱坤
Owner SHANXI UNIV
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