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Preparation method of bis tetraethylammonium dodecahydrododecaborate

A technology of bistetraethylammonium borate and tetraethylammonium chloride, which is applied to the preparation of amino compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of long reaction time, low product yield, separation and purification steps To simplify the reaction steps, enhance the interaction and improve the catalytic activity

Active Publication Date: 2015-04-29
ZHENGZHOU SIGMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current method for synthesizing dodecahydrododecaborate has a long reaction time, cumbersome separation and purification steps, and low product yield, so it is urgently needed to improve its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] This preparation method comprises the steps:

[0013] Add sodium borohydride 40g, tetraethylammonium chloride 199.2g, zinc and manganese dioxide composite catalyst 0.3g, deionized water 56g, paraffin oil 558g successively in the microwave reactor with tail gas absorption, after stirring evenly, in 25 300W microwave irradiation at ℃ for 70s, then 800W microwave irradiation at 200℃ for 70min, then take out the reaction mixture, disperse with 1116g of petroleum ether, filter, add 500g of water to the filter cake, heat and reflux at 80~85℃ for 1 hour, then cool and filter After evaporating the filtrate to dryness, add 120g of 80% isopropanol by volume, heat and reflux at 65~70°C for half an hour, heat filter, cool the filtrate, and filter at room temperature to obtain off-white crystalline dodecahydrododecaborate Ethylammonium product 25.5g (yield 72%). Zn and MnO 2 The mass ratio is 1:2.5.

Embodiment 2

[0015] This preparation method comprises the steps:

[0016] Add sodium borohydride 21g, tetraethylammonium chloride 124.5g, zinc and manganese dioxide composite catalyst 0.2g, deionized water 37.6g, paraffin oil 376g successively in the microwave reactor with tail gas absorption, after stirring evenly, in 300W microwave irradiation at 25°C for 60s, then 800W microwave irradiation at 205°C for 70min, then take out the reaction mixture, filter with 752g of petroleum ether, add 350g of water to the filter cake, heat and reflux at 80~85°C for 1 hour, then cool and filter. Evaporate the filtrate to dryness, then add 75g of 80% isopropanol, heat and reflux at 65~70°C for half an hour, then heat filter, cool the filtrate, and filter at room temperature to obtain off-white crystalline ditetraethylammonium dodecahydrododecaborate Product 113.21g (yield 71%). Zn and MnO 2 The mass ratio is 1:2.

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Abstract

The invention discloses a method for preparing bis tetraethylammonium dodecahydrododecaborate, belonging to the field of inorganic chemical synthesis. The method comprises the following steps: sequentially adding tetraethylammonium chloride, sodium borohydride, a composite catalyst, deionized water and paraffin oil into a microwave reactor provided with a tail gas absorption unit, stirring uniformly, carrying out 300W microwave irradiation at 25-30 DEG C for 60-80 seconds, carrying out 800W microwave irradiation at 200-205 DEG C for 60-80 minutes, taking out the reaction mixture, filtering with petroleum ether, adding water into the filter cake, heating under reflux, cooling, filtering, drying the filtrate by distillation, adding 80 vol% isopropanol, heating under reflux, carrying out hot filtration, cooling the filtrate, and filtering to obtain the bis tetraethylammonium dodecahydrododecaborate. The method is simple to operate, and has the advantages of short reaction time, high product yield and the like.

Description

technical field [0001] The invention belongs to the field of inorganic chemical synthesis, and in particular relates to a preparation method of ditetraethylammonium dodecahydrododecaborate. technical background [0002] Ionic borohydride-based ultra-high burning rate modifiers have the advantages of good stability, low toxicity, high combustion value, convenient synthesis, and low cost. Therefore, in recent years, the preparation and research of this type of compound have received more and more attention wider attention. Among them, dodecahydrododecaborate has an icosahedral configuration and has high stability, so it has broad application prospects in high-energy rocket fuel additives, new materials, and chemical hydrogen storage. However, the current method for synthesizing dodecahydrododecaborate has long reaction time, tedious separation and purification steps, and low product yield. Therefore, it is urgent to improve its preparation method. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/00
Inventor 杨勇胡孝伦王建莉郝家金李义波赵萍萍王娅娟
Owner ZHENGZHOU SIGMA CHEM
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