Method for synthesizing sodium aluminum hydride by utilizing Grignard reagent method

A technology of Grignard reagent and sodium aluminum hydride, which can be applied to various metal hydrides and other directions, and can solve the problems of slow reaction rate, harsh reaction conditions of solid-phase method, and large energy consumption.

Inactive Publication Date: 2014-11-05
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The liquid phase method mainly uses the principle of synthesizing NaAlH4 by using aluminum trichloride and aluminum halide in tetrahydrofuran or ether solvent. In the process, the reaction rate of sodium hydride and aluminum trichloride is slow, and the NaCl generated by the reaction is easy to deposit on the surface of sodium hydride, preventing the further reaction of sodium hydride and aluminum trichloride, so the conversion rate of raw materials is low; solid phase method reaction conditions The requirements are relatively strict, and it is often carried out under high pressure, which consumes a lot of energy and has high requirements for equipment.

Method used

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  • Method for synthesizing sodium aluminum hydride by utilizing Grignard reagent method
  • Method for synthesizing sodium aluminum hydride by utilizing Grignard reagent method
  • Method for synthesizing sodium aluminum hydride by utilizing Grignard reagent method

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Grignard reagent preparation method, the steps are:

[0038] (1) Weigh 1.00g of aluminum powder into the three-necked bottle, and protect it with hydrogen;

[0039] (2) Add 10ml of ethyl bromide to the bottle, set the temperature at 39°C, and react for 15 minutes;

[0040] (3) Observe the experimental phenomenon, if the reaction is slow or almost no reaction, add a small amount of iodine and anhydrous aluminum chloride to initiate the reaction;

[0041] (4) After the reaction occurs, condense the ethyl bromide to reflux, and set the temperature of the cooling circulating fluid below 0°C. At this time, white smoke in the system escapes through the exhaust device, and it is acidic when tested with pH test paper;

[0042] (5) After continuing to react for 1 hour, add a little sodium slice just cut into it, keep reflux, and react for another 6 hours;

[0043] (6) At this time, the system is a pasty black liquid, take out a little, smoke in the air, and react violently wit...

Embodiment 2

[0046] Utilize Grignard reagent to prepare sodium aluminum hydride, the steps are:

[0047] (1) Weigh 1.00g of aluminum powder into a three-necked bottle, and after protecting it with hydrogen, add iodine and anhydrous aluminum chloride;

[0048] (2) Then add 5ml bromoethane, set the temperature to 39°C for reaction;

[0049](3) After the reaction occurs, the ethyl bromide is condensed and refluxed, and the temperature of the cooling circulating fluid is set below 0°C, at this time, white smoke in the system escapes through the tail gas device;

[0050] (4) After continuing to react for 1 hour, add 3g of sodium hydride, keep reflux, and raise the temperature to 80°C;

[0051] (5) After continuing the reaction for 1 hour, add 10ml of toluene as a dispersant, and raise the temperature to 110°C, and continue the reaction for 5 hours;

[0052] (6) Adjust the temperature to 65°C, add 40ml tetrahydrofuran, and stir for 1 hour;

[0053] (7) After standing and stratifying, take the...

Embodiment 3

[0058] Utilize Grignard reagent to prepare sodium aluminum hydride, the steps are:

[0059] (1) Weigh 0.85g of aluminum powder into a three-necked bottle, and then add iodine and anhydrous aluminum chloride after hydrogen protection;

[0060] (2) Then add 5ml bromoethane, set the temperature to 39°C for reaction;

[0061] (3) After the reaction occurs, the ethyl bromide is condensed and refluxed, and the temperature of the cooling circulating fluid is set below 0°C, at this time, white smoke in the system escapes through the tail gas device;

[0062] (4) After continuing to react for 1 hour, add 3.5g of sodium hydride, maintain reflux, and raise the temperature to 80°C;

[0063] (5) After continuing the reaction for 1 hour, add 10ml of toluene as a dispersant, and raise the temperature to 110°C, and continue the reaction for 5 hours;

[0064] (6) Adjust the temperature to 65°C, add 40ml tetrahydrofuran, and stir for 1 hour;

[0065] (7) After standing and stratifying, take ...

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Abstract

The invention discloses a method for synthesizing sodium aluminum hydride by utilizing a Grignard reagent method and relates to a method for preparing sodium aluminum hydride. The method for synthesizing sodium aluminum hydride by utilizing the Grignard reagent method comprises the following steps: preparing an aluminum Grignard reagent by utilizing bromoethane and activated aluminum powder, further removing halogen atoms, and generating aluminum alkyl hydride. An organic aluminum compound is prepared by reacting activated aluminum and bromoethane, and on the basis that a mixture of aluminum alkyl bromide and aluminum alkyl hydride is prepared, high-purity sodium aluminum hydride is prepared by directly reacting a high-activity organic aluminum reagent and sodium hydride.

Description

technical field [0001] The invention relates to a preparation method of sodium aluminum hydride, in particular to a method for synthesizing sodium aluminum hydride by using the Grignard reagent method. Background technique [0002] As a general reducing agent, sodium aluminum hydride is a complex metal hydride with research and application prospects, and has excellent hydrogen storage performance. where NaAlH 4 The theoretical hydrogen storage capacity is 7.4 wt.%, and the actual hydrogen storage capacity is 5.5 wt.%; Na 3 H 6 The theoretical hydrogen storage capacity is 5.9 wt.%. [0003] The preparation of sodium aluminum hydride mainly includes direct and indirect synthesis. The direct use of sodium, aluminum and hydrogen to prepare sodium aluminum hydride requires expensive triethylaluminum as a catalyst and reacts under high pressure. Under high pressure, sodium and hydrogen react to form sodium hydride, and sodium hydride and aluminum are catalyzed by triethylalumi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/24
Inventor 高建峰汪伟曹端林张彦李永祥邱少君王建龙唐望
Owner ZHONGBEI UNIV
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