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Method for preparing sodium borohydride

A technology of sodium borohydride and hydride, applied in the field of compound preparation, can solve the problems of high equipment requirements, increase production costs and the like, and achieve the effects of simple process, avoiding strict requirements and high yield

Inactive Publication Date: 2008-09-24
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the research papers published at home and abroad, metal hydride and sodium metaborate are used as raw materials, and the reaction needs to be carried out under high-pressure hydrogen above 2MPa. The reaction is based on the principle of gas-solid heterogeneous reaction, so the reaction process requires more equipment. high, increasing production costs

Method used

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  • Method for preparing sodium borohydride
  • Method for preparing sodium borohydride
  • Method for preparing sodium borohydride

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Remove mineral oil from industrial-grade sodium hydride (Shanghai Senhao Fine Chemical Co., Ltd.), weigh 9.6 g under nitrogen protection for use; remove water from sodium metaborate (Sinopharm Group), crush it to 100-200 mesh, and weigh 6.58 g g for use; crush silicon dioxide (Sinopharm Group) to 100-200 mesh, and weigh 12g. The reactants weighed above were then mechanically mixed for 2 hours under nitrogen protection. Under the protection of nitrogen, the above mixture was rolled into a block with a pressure of 20 MPa. Then, under the protection of 0.1atm hydrogen, the temperature was raised to 510°C at a rate of 10°C / min, calcined for 8 hours, and cooled to room temperature with the furnace. The reaction product was pulverized, and 150 ml of isopropylamine was added as an extractant, extracted with a Soxhlet extractor for 2 h, and then the isopropylamine was recovered by distillation to obtain 2.97 g of sodium borohydride, and the yield was 78.6% of the theoretical v...

Embodiment 2

[0026] Remove mineral oil from industrial-grade sodium hydride (Shanghai Senhao Fine Chemical Co., Ltd.), weigh 12g under nitrogen protection for use; remove water from sodium metaborate (Sinopharm Group), crush it to 100-200 mesh, and weigh 6.58g Stand-by; crush silicon dioxide (Sinopharm Group) to 100-200 mesh, and weigh 12g. The reactants weighed above were then mechanically mixed for 2 hours under nitrogen protection. Under the protection of nitrogen, the above mixture was rolled into a block with a pressure of 20 MPa. Then, under the protection of high-purity nitrogen at normal pressure, the temperature was raised to 500°C at a rate of 5°C / min, calcined for 8 hours, and cooled to room temperature with the furnace. The reaction product was pulverized, and 150 ml of isopropylamine was added as an extractant, extracted with a Soxhlet extractor for 2 h, and then the isopropylamine was recovered by distillation to obtain 2.876 g of sodium borohydride, and the yield was 76.1% ...

Embodiment 3

[0028] Remove mineral oil from industrial-grade sodium hydride (Shanghai Senhao Fine Chemical Co., Ltd.), weigh 9.6 g under nitrogen protection for use; remove water from sodium metaborate (Sinopharm Group), crush it to 100-200 mesh, and weigh 6.58 g g for use; crush silicon dioxide (Sinopharm Group) to 100-200 mesh, and weigh 12g. The reactants weighed above were then mechanically mixed for 2 hours under nitrogen protection. Under the protection of nitrogen, the above mixture was rolled into a block with a pressure of 20 MPa, and the block was crushed to 50-100 mesh again. Then, under the protection of 2atm hydrogen, the temperature was raised to 480°C at a rate of 10°C / min, calcined for 6 hours, and cooled to room temperature with the furnace. The reaction product was pulverized, and 150 ml of isopropylamine was added as an extractant, extracted with a Soxhlet extractor for 2 h, and then the isopropylamine was recovered by distillation to obtain 3.13 g of sodium borohydride...

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Abstract

The invention belongs to the technical field of compound preparation, in particular relates to a preparation method of sodium borohydride. The invention is different from the traditional gas-solid heterogeneous reaction, and carries out solid-state reaction by a metal hydride and a boron-containing compound, and then the sodium borohydride is prepared. The reaction in the invention is carried out completely at the inner part of solid-state materials, so the sodium borohydride can be obtained under lower hydrogen pressure even in an atmosphere of inert gases, thus, high-pressure hydrogen avoids to be used and the requirement to equipment is reduced. The preparation method has the advantages of simple technical process and easy realization of scale production.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a method for preparing sodium borohydride, more specifically, the invention relates to a method for preparing sodium borohydride by solid-phase reaction of a metal hydride and a boron-containing compound. Background technique [0002] Sodium borohydride has strong reducing properties and has a wide range of applications in organic and inorganic chemistry. It can selectively reduce specific functional groups on aldehydes, ketones, and acid chlorides. In aqueous solution, sodium borohydride can reduce Fe 3+ 、Co 2+ 、Ni 2+ 、HSO -3 , IO -3 Plasma. In industrial production, sodium borohydride is widely used in pharmaceuticals, fine organic synthesis, wood pulp bleaching, industrial wastewater treatment, and can also be used as a raw material for the preparation of boron-containing compounds. Due to its high hydrogen content, the research on sodium borohyd...

Claims

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Application Information

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IPC IPC(8): C01B6/21
Inventor 孙大林张汉平吴宇平
Owner FUDAN UNIV
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