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Method for synthesizing M(BH4)n and/or M2/nB12H12

A technology of nb12h12 and B10H14, which is applied in the field of inorganic material synthesis process, can solve the problems of increased risk and complexity, and achieve the effects of high safety, environmental protection and simple reaction conditions

Active Publication Date: 2017-11-14
SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this reaction, stringent conditions such as highly reactive metallic sodium, liquid ammonia, 0.3 MPa H 2 Pressure and temperatures above 400°C exacerbate risks and complexity in actual operation

Method used

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  • Method for synthesizing M(BH4)n and/or M2/nB12H12
  • Method for synthesizing M(BH4)n and/or M2/nB12H12
  • Method for synthesizing M(BH4)n and/or M2/nB12H12

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a pure Ar protected glove box, use commercial NaNH 2 and B 10 h 14 As the initial reactant, NaNH 2 and B 10 h 14 Grind in a mortar and mortar for 30 minutes at a molar ratio of 5:1 until well mixed.

[0034] Take about 0.15g of a well-mixed sample and place it in a volume of 0.7cm 3 Inside the stainless steel reaction crucible, sealed. The stainless steel reaction crucible after sealing the sample was heated in a muffle furnace under the following conditions: 300°C for 1 hour; 300°C for 5 hours; 300°C for 10 hours; 400°C for 10 hours. After the temperature dropped to room temperature, the reaction crucible was taken out, opened in an Ar protection glove box, and the sample was recovered.

[0035] figure 1 It is the XRD and Raman diagram of the reaction product, and a single NaBH is obtained 4 .

[0036] XRD and Raman two detection methods for NaBH 4 and Na 2 B 12 h 12 Sensitivity is different, XRD is easier to detect NaBH 4 , Raman is easier to detect ...

Embodiment 2

[0039] In a pure Ar protected glove box, use commercial NaNH 2 and B 10 h 14 As the initial reactant, NaNH 2 and B 10 h 14 Grind in a mortar and mortar for 30 minutes at a molar ratio of 3.5:1 until well mixed.

[0040] Take about 0.15g of a well-mixed sample and place it in a volume of 0.7cm 3 Inside the stainless steel reaction crucible, sealed. The stainless steel reaction crucible after sealing the sample was heated in a muffle furnace under the following conditions: 100°C for 10 hours; 200°C for 10 hours; 300°C for 10 hours; 400°C for 10 hours. After the temperature dropped to room temperature, the reaction crucible was taken out, opened in an Ar protection glove box, and the sample was recovered.

[0041] figure 2 is the XRD and Raman diagram of the reaction product, NaBH 4 more than Na 2 B 12 h 12 , a weaker Na can be seen in the Raman spectrum 2 B 12 h 12 peak. In addition to the ratio of raw materials, the reaction conditions can also significantly af...

Embodiment 3

[0043] In a pure Ar protected glove box, use commercial NaNH 2 and B 10 h 14 As the initial reactant, NaNH 2 and B 10 h 14 Grind in a mortar and mortar for 30 minutes at a molar ratio of 2:1 until well mixed.

[0044] Take about 0.15g of a well-mixed sample and place it in a volume of 0.7cm 3 Inside the stainless steel reaction crucible, sealed. The stainless steel reaction crucible after sealing the sample was heated in a muffle furnace under the following conditions: 100°C for 10 hours; 200°C for 10 hours; 300°C for 10 hours; 400°C for 10 hours. After the temperature dropped to room temperature, the reaction crucible was taken out, opened in an Ar protection glove box, and the sample was recovered.

[0045] image 3 is the XRD and Raman diagram of the reaction product, Na 2 B 12 h 12 more than NaBH 4 . In addition to the ratio of raw materials, the reaction conditions can also significantly affect the product. The reaction did not occur at 100 °C, but partially ...

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Abstract

The invention belongs to the field of inorganic material synthesis processes, and discloses a method for synthesizing M(BH4)n and / or M2 / nB12H12. Specifically, M(BH4)n and the M2 / nB12H12 are obtained through reaction of M(NH2)n and B10H14, M is selected from Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba and Al and n is 1, 2 or 3. A precedent of preparing borohydride is initiated through reaction of metal amide and B10H14; a new way is provided for synthesis of a metal borohydride material; and the condition that a plasma strategy is effective means of synthesis of a metal dodecane compound is provided. The reaction conditions are simple, the security is high, a product can be obtained without dewatering treatment, a solvent does not need to be used and the environment is protected.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis technology, in particular to a synthetic M(BH 4 ) n and / or M 2 / n B 12 h 12 Methods. Background technique [0002] Metal borohydride M(BH 4 ) n As an important inorganic compound, it has been widely used in chemical reactions, hydrogen storage materials, and solid-state ion batteries, thus attracting great research interest. In numerous M(BH 4 ) n Compound, sodium borohydride NaBH 4 , is the most widely used and most important, and thousands of tons of sodium borohydride are produced and consumed every year, far exceeding the levels of any other borohydride. Because of its high hydrogen storage density (10.7wt%, 114.5kg / m 3 ), sodium borohydride is also considered as a promising hydrogen storage material. In the hydrogen absorption and desorption cycle of sodium borohydride, the formation of stable B 12 Skeleton Na 2 B 12 h 12 Reaction intermediates affect its hydrogen ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/19C01B6/21C01B35/18
CPCC01B6/19C01B6/21C01P2002/72C01P2002/82C01P2002/86
Inventor 卢周广何礼青
Owner SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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