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Lithium borohydride tetrahydrofuran solution preparation method

A technology of tetrahydrofuran and lithium borohydride, applied in the directions of borane/diborane hydride, instruments, analytical materials, etc., to achieve the effects of mild reaction conditions, good safety, and easy storage

Inactive Publication Date: 2017-12-29
庄英俊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a lithium borohydride tetrahydrofuran solution, which solves the safety problem in actual production, has a mild reaction process, safe and stable transportation and storage, and lithium borohydride has a relatively high active hydrogen content

Method used

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  • Lithium borohydride tetrahydrofuran solution preparation method
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  • Lithium borohydride tetrahydrofuran solution preparation method

Examples

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Embodiment 1

[0037] A preparation method of lithium borohydride tetrahydrofuran solution, comprising the following steps:

[0038] (1) Add 55g of potassium borohydride to 650mL of tetrahydrofuran and stir evenly;

[0039] (2) Add 47g of lithium chloride to step (1), raise the temperature to 24°C, and react for 8 hours;

[0040] (3) Filter the product obtained in step (2), and further distill the filtrate to obtain a lithium borohydride tetrahydrofuran solution with the required concentration.

Embodiment 2-8

[0042] The steps are the same as in Example 1, and the amounts of reactants and the reaction conditions are shown in Table 1.

Embodiment 9

[0044] The assay method of the active hydrogen content of lithium borohydride in the lithium borohydride tetrahydrofuran that embodiment 1-8 makes:

[0045] (1) Distill the lithium borohydride tetrahydrofuran solution prepared in Examples 1-8 to remove tetrahydrofuran to obtain a lithium borohydride solid;

[0046] (2) Take a dry and clean Erlenmeyer flask and weigh it accurately, take the sample and put it in the Erlenmeyer flask, seal it tightly, and record it as W;

[0047] (3) The mixed solution of water and dioxane (the volume ratio of water: dioxane is 5:5) is added in the constant pressure funnel;

[0048] (4) The constant pressure funnel is connected with the Erlenmeyer flask with the sample and the gas constant pressure capacity measuring instrument to form a closed system, write down the volume number of the scale tube in the gas constant pressure capacity measuring instrument, and record it as V 1 ;

[0049] (5) Place the Erlenmeyer flask containing the sample in ...

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Abstract

The invention discloses a lithium borohydride tetrahydrofuran solution preparation method. The method includes steps: (1) adding potassium borohydride into tetrahydrofuran, and well stirring; (2) adding lithium chloride into a material obtained at the step (1), heating to 20-26 DEG C, and allowing reaction for 18-30h; (3) filtering a product obtained at the step (2), and further distilling filtrate to obtain lithium borohydride tetrahydrofuran solution in required concentration. Lithium borohydride prepared according to the method is high in content of activated hydrogen, and mild reaction conditions, high safety and convenience in utilization, transport and storage are realized.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry, in particular to a preparation method of lithium borohydride tetrahydrofuran solution. Background technique [0002] Lithium borohydride (LiBH 4 ) is one of the most important reducing agents in organic chemistry and belongs to the borohydride family. It is used as a hydrogen source and a reducing agent for organic groups (such as aldehydes, ketones, esters), and is mainly used in the pharmaceutical, spice and pesticide industries. With the rapid development of my country's economy, the demand for this product is increasing day by day. However, solid lithium borohydride powder is easy to absorb moisture and decompose in the air, and it is flammable and extremely unsafe, and it is inconvenient to store. It needs to be stored under the protection of nitrogen and isolated from water vapor, and it should be operated and used in a fume hood. Therefore, there is an urgent need in the art f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/21G01N7/18
CPCC01B6/21G01N7/18
Inventor 庄英俊王天野史建忠
Owner 庄英俊
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