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Method for preparing sodium aluminum hydride

A technology of sodium aluminum hydride and hydrogen, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of cumbersome steps and not suitable for mass production, and achieve the effect of fewer reaction steps

Active Publication Date: 2009-09-16
YINGLI ENERGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The above-mentioned method for preparing sodium aluminum hydride is suitable for synthesizing sodium aluminum hydride in the laboratory, and needs to be carried out step by step, and the steps are loaded down with trivial details, so it is not suitable for mass production in factories

Method used

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  • Method for preparing sodium aluminum hydride
  • Method for preparing sodium aluminum hydride
  • Method for preparing sodium aluminum hydride

Examples

Experimental program
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Effect test

Embodiment 1

[0030] First, purify the reaction system with nitrogen, add 40 kg of toluene, 13 kg of aluminum powder, 1000 ppm (part per million) of titanium in 13 kg of aluminum powder, and 0.5 kg of TEA (triethylaluminum). Stir and heat to 110 degrees (°C), add 10 kg of molten sodium, continue heating to 130 degrees, feed hydrogen to pressurize the reactor to 15168KPa, and continue the reaction for 2.5 hours. During the reaction, control the reaction temperature at 135 degrees and the pressure at 15168KPa. The exhaust was cooled to room temperature. Settling and discharging the upper layer toluene clear liquid, then washing with toluene, settling and discharging the upper layer toluene clear liquid, drying to obtain sodium aluminum hydride solid. The conversion of sodium aluminum hydride on a sodium basis was 98%.

Embodiment 2

[0032] First purify the reaction system with nitrogen, add 40 kg of toluene, 13 kg of aluminum powder, 1000 ppm of titanium and 0.5 kg of TEA in the 60 liter autoclave equipped with agitator and cooling coil. Stir and heat to 110°C, add 10 kg of molten sodium, continue heating to 130°C, feed hydrogen to pressurize the reactor to 15168KPa, and continue the reaction for 2.8 hours. During the reaction, control the reaction temperature at 130°C and the pressure at 15168KPa. The exhaust was cooled to room temperature. Settling and discharging the upper layer toluene clear liquid, then washing with toluene, settling and discharging the upper layer toluene clear liquid, drying to obtain sodium aluminum hydride solid. The conversion of sodium aluminum hydride on a sodium basis was 96%.

Embodiment 3

[0034] First purify the reaction system with nitrogen, add 40 kg of toluene, 13 kg of aluminum powder, 1000 ppm of titanium and 0.5 kg of TEA in the 60 liter autoclave equipped with agitator and cooling coil. Stir and heat to 110°C, add 10 kg of molten sodium, continue heating to 130°C, feed hydrogen to pressurize the reactor to 15168KPa, and continue the reaction for 2.2 hours. During the reaction, control the reaction temperature at 145°C and the pressure at 15168KPa. The exhaust was cooled to room temperature. Settling and discharging the upper layer toluene clear liquid, then washing with toluene, settling and discharging the upper layer toluene clear liquid, drying to obtain sodium aluminum hydride solid. The conversion of sodium aluminum hydride on a sodium basis was 94%.

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Abstract

The invention discloses a method for preparing sodium aluminum hydride, wherein liquid sodium, solid aluminum and hydrogen gas are reacted at heating condition to prepare the sodium aluminum hydride. The invention provides sodium aluminum hydride prepared by the method. The invention belongs to inorganic synthesis field. Compared with prior art, the method for preparing sodium aluminum hydride can finish preparation of the sodium aluminum hydride by one step. The technical scheme provided by the present invention is especially suitable for sodium aluminum hydride industrialization production.

Description

technical field [0001] The invention relates to a preparation method of sodium aluminum hydride, which belongs to the field of inorganic synthetic chemistry. Background technique [0002] The chemical formula of sodium aluminum hydride is NaAlH 4 , is a highly reductive complex hydride, and its reducibility is similar to that of lithium aluminum hydride. Shen Juanwen and Che Yunxia of Nankai University described a synthesis method of sodium aluminum hydride in China ZL89108190. The reaction can be divided into two steps: the first step is the hydrogenation reaction of metal sodium, and the reaction equation is as follows: [0003] [0004] In the reaction formula, s represents a solid, and g represents a gas. The reaction conditions of the first step are normal temperature and pressure, and the catalysts used are naphthalene and titanium tetrachloride, which are reacted in tetrahydrofuran; the second step is sodium hydride and three The reaction of aluminum chloride, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
Inventor 张月和薛明李青娟蔡春立王伟
Owner YINGLI ENERGY CHINA
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