Production method of amine borane complex

A production method and complex technology, applied in the field of amine borane complex production, can solve the problems of high production process cost, harsh experimental conditions, slow reaction, etc., and achieve moderate cost, equipment compatibility, and high product purity Effect

Inactive Publication Date: 2015-05-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] In general, the above methods are relatively complicated to operate, some experimental c

Method used

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  • Production method of amine borane complex
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  • Production method of amine borane complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1, preparation of ethylenediamine borane complex

[0034] use figure 1 The reaction device, wherein the reaction chamber is a 1000mL glass three-necked bottle, operates at room temperature. 6.5g NaBH 4 Put it into the borane generator after grinding, put 5ml H2 SO 4 The solution was added to a constant pressure funnel, and the air in the reaction chamber was replaced with nitrogen, and 3 ml of anhydrous ethylenediamine was added to a flask placed in a hot water bath. During the reaction, the inert gas flow of ethylenediamine and the carrier gas of borane were connected, and the concentrated H 2 SO 4 Put the solution into the borane generator, react for 2 hours, close the settling tube and the ethylenediamine inert gas flow inlet valve after the white mist in the reaction chamber settles, and continue to add concentrated H 2 SO 4 After 0.5 hours of solution, the white pure EDAB product was collected. Product XRD results see figure 2 (a). This substan...

Embodiment 2

[0035] Embodiment 2, preparation of dimethylamine borane complex

[0036] use figure 1 A similar reaction device, wherein the reaction chamber is a 1000mL glass three-necked bottle, the three-necked bottle is placed in an ice-salt bath, and the borane uses industrial borane gas diluted with argon. The reaction chamber was first replaced with argon for air. During the reaction, the borane diluted with argon was first passed into the inert gas flow of dimethylamine, and after 1 hour of reaction, the borane gas was turned off, and the dimethylamine inert gas flow was continued to be passed into for 1 hour. After the ice-salt bath was removed, the reaction The chamber performs vacuum operation. The white dimethylamine borane complex product was collected after 3 hours in vacuo. Product XRD such as figure 2 (b) shown.

Embodiment 3

[0037] Embodiment 3, preparation of tert-butylamine borane complex

[0038] use figure 1 Reaction device, wherein the reaction chamber is a 1000mL glass three-necked bottle, and the borane generator is a 150mL glass three-necked bottle. 5 g LiBH 4 Put into the borane generator after grinding, put 4ml BCl 3 The solution was added to the constant pressure funnel. The reaction chamber was replaced with nitrogen for air. During the reaction, the inert gas flow of tert-butylamine and borane carrier gas were connected, and BCl was slowly added dropwise. 3 Put the solution into the borane generator, react for 2 hours, close the settling tube and the outlet valve of the borane generator after the white smoke in the reaction chamber settles, and collect the white pure tert-butylamine borane complex. Product XRD such as figure 2 (c).

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PUM

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Abstract

The invention belongs to the technical field of material preparation, and particularly relates to a production method of an amine borane complex. The production method provided by the invention comprises the following steps: directly reacting borane with inert gas flow of amine, regulating and controlling the proportion of the two components, and carrying out further aftertreatment if necessary to prepare the final product, namely the amine borane complex. No salt impurities are introduced in the reaction process, and no organic solvent is used; such safe reagents as hydroboron are used for producing the borane, and the borane is used once being prepared to avoid the direct operation of the toxic gas borane. The method provided by the invention is simple to operate, high in product purity, low in cost and capable of achieving continuous scale production. Meanwhile, the method is compatible with equipment for producing the amine borane complex in other manners, and the production equipment can be used for producing via the method after simple adjustment.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a series of production methods of amine borane complexes. Background technique [0002] The chemical formula of the amine borane complex is , is a series of white, non-volatile, salt-like crystals with excellent selective reduction properties, and is an alkylation reduction agent for proteins. Compared with sodium borohydride, it has the following advantages: mild reduction, can be used in a wide range of pH Wide range of applications, and can be better soluble in water and organic solvents. It can also be used for electroplating nickel to obtain high-purity nickel film. The nickel film has high melting point, good heat resistance, high hardness, low resistance and good welding performance. It is also used in the production process of printed circuit boards. At the same time, some materials have hydrogen storage capacity and high energy density charac...

Claims

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Application Information

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IPC IPC(8): C07F5/02C07F5/00
CPCC07F5/027
Inventor 郭艳辉郑雄飞宋袁周
Owner FUDAN UNIV
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