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A kind of method utilizing Grignard reagent method to synthesize sodium aluminum hydride

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 high energy consumption, high equipment requirements and slow reaction rate.

Inactive Publication Date: 2016-08-17
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid phase method mainly uses aluminum trichloride and aluminum halides to synthesize NaAlH in tetrahydrofuran or ether solvents. 4 On the one hand, this method requires the purity of the raw materials to be quite high, on the other hand, the reaction rate of sodium hydride and aluminum trichloride is relatively slow during the reaction process, and the NaCl generated by the reaction is easy to deposit on the surface of sodium hydride, preventing sodium hydride and trichloride The further reaction of aluminum chloride, so the conversion rate of raw materials is low; the requirements of solid phase reaction conditions are relatively harsh, often carried out under high pressure, energy consumption is large, and the requirements for equipment are high

Method used

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  • A kind of method utilizing Grignard reagent method to synthesize sodium aluminum hydride
  • A kind of method utilizing Grignard reagent method to synthesize sodium aluminum hydride
  • A kind of method utilizing Grignard reagent method to synthesize sodium aluminum hydride

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 using a Grignard reagent method, and relates to a preparation method of sodium aluminum hydride. A method for synthesizing sodium aluminum hydride using the Grignard reagent method, using ethyl bromide and activated aluminum powder to prepare the Grignard reagent for aluminum, and further dehalogenating it to generate alkyl aluminum hydride. The present invention uses the reaction of activated aluminum and ethyl bromide to prepare organoaluminum compounds, and on the basis of preparing the mixture of alkylaluminum bromide and alkylaluminum hydride, uses a highly active organoaluminum reagent to directly react with sodium hydride to form Sodium aluminum hydride with high purity was obtained.

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 Patents(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