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Preparation method of high purity borane gas and application of borane gas

A borane gas and borane technology, applied in the field of new energy, can solve the problems of danger, inability to guarantee safety, unfavorable social resource protection and effective utilization, etc., and achieve the effect of safety guarantee and effective utilization improvement.

Inactive Publication Date: 2014-10-08
SHANGHAI SCIENTIA PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also, when people prepare borane, the safety of post-processing and the practicability of processing products have always been a difficult problem
At present, the reprocessing of most laboratories or manufacturers is dangerous, and their processed products are treated as waste, which not only cannot guarantee safety, but also causes great pollution to the environment, which is not conducive to the protection of social resources and use efficiently

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0033] Preparation of main raw material borane gas;

[0034] Raw material A: Lewis acid, such as BF3 gas and its complexes, such as boron trifluoride ether, boron trifluoride tetrahydrofuran, boron trifluoride acetonitrile, boron trifluoride acetic acid, etc. HCl, concentrated sulfuric acid, Lewis acid, etc. are also applicable. The raw material A is one or more of the above reagents, but not limited to the above reagents.

[0035] Raw material B: Lewis base, such as potassium borohydride, sodium borohydride, lithium borohydride, sodium hydride and the like. The raw material B is one or more of the above reagents, but is not limited to the above reagents.

[0036] Solvent C: neutral solvent, such as ethylene glycol diethyl ether, ethylene glycol dimethyl ether, ethylene glycol dibutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl ethyl ether, Triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, ethylene glycol ...

Embodiment 1

[0039] Put 100kg of sodium borohydride into a 2000L reactor replaced with argon, add 280L of ethylene glycol diethyl ether under stirring conditions; then use a precise flow pump to pour 500L of boron trifluoride ether solution into it to react The temperature is controlled at minus 30 to 50°C (-30°C to 50°C). In the reaction process, the prepared borane gas is introduced into the buffer tank, and then passed through the low-temperature cooling tower, acid gas absorption tower, and drying tower in sequence; the organic solvent and acid gas boron trifluoride brought in by borane are effectively absorbed; In this way, a high-purity borane gas of more than 99% will be obtained. At present, the purity of borane gas generally prepared in the world is 90%-95%.

Embodiment 2

[0041] Put 145 kg of potassium borohydride into a 2000L reactor replaced with argon, add 350L of ethylene glycol diethyl ether under stirring conditions; then use a precise flow pump to pour 510L of boron trifluoride ether solution into it to react The temperature is controlled at minus 30 to 50°C (-30°C to 50°C). In the reaction process, the prepared borane gas is introduced into the buffer tank, and then passed through the low-temperature cooling tower, acid gas absorption tower, and drying tower in sequence; the organic solvent and acid gas boron trifluoride brought in by borane are effectively absorbed; In this way, high purity borane gas will be obtained.

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Abstract

The invention relates to a preparation method of a high purity borane gas. The preparation method comprises the following steps: putting Lewis base in a reaction kettle and adding a neutral solvent to obtain a solution; adding the solution into Lewis acid to react to obtain a low purity borane gas and a reaction residue liquid; introducing the low purity borane gas into a buffer kettle, and then sequentially passing through a low temperature cooling tower, an acid gas absorption tower and a drying tower to obtain the high purity borane gas; and filter-pressing the quenched reaction residue liquid to obtain a filter solution and a solid, rectifying the filter solution to obtain a rectified product and recrystallizing the solid to obtain a recrystallized product. The invention further provides an application of the borane gas. By adopting the preparation of the borane gas and the application of the borane gas provided by the invention, the borane gas with the purity being over 99% can be obtained, and great improvement is made to effective utilization of post-treatment and treatment products for preparing the borane gas, so that the post-treatment is safer, the treatment products can turn waste into wealth, and the high purity product can be prepared.

Description

Technical field [0001] The present invention relates to the field of new energy and medicine, in particular to a preparation method of borane compounds, and specifically refers to a preparation method of high-purity borane gas and the application of the borane gas. Background technique [0002] Diborane (B2H6) is a flammable gas and a Lewis acid. Diborane and Lewis base form a variety of complexes, these complexes are summarized as borane products and their derivatives. These compounds are widely used in the fields of biomedical synthesis, chiral synthesis, fine chemical synthesis, and new energy. Many possible methods for the synthesis of diborane have been published. The most typical and commercially available synthesis method is to use boron trifluoride and sodium borohydride in an ether solvent such as diglyme. But most manufacturers have not solved the problem of solvent and acid gas entrained in borane gas. In this way, it will have a significant impact on the purity of...

Claims

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Application Information

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IPC IPC(8): C07F5/02C07F5/04C01B35/06
CPCC01B35/06C07F5/02C07F5/04
Inventor 冯虎姚俊娜
Owner SHANGHAI SCIENTIA PHARMA TECH
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