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A kind of preparation method of ditetraethylammonium decahydrodecaborate

A technology of bistetraethylammonium and decahydrodecaboric acid is applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc., and can solve the problems of low product yield and long reaction time, etc. problems, to achieve the effect of simplifying the reaction steps, improving the catalytic activity, and facilitating the operation

Active Publication Date: 2016-08-24
ZHENGZHOU SIGMA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wherein the ditetraethylammonium decahydrodecaborate is a higher ionic borohydride salt of application value, "Journal of Chemistry" No. 4 in 1978 reported "Research on boron compounds I. Synthesis of decaboron decahydrogen (B 10 h 10 2- ) new method, which adopts oil bath pyrolysis method to synthesize ditetraethylammonium decahydrodecaborate, the reaction time is long, and the product yield is low (less than 40%). Therefore, it is urgent to improve its preparation method at present

Method used

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  • A kind of preparation method of ditetraethylammonium decahydrodecaborate
  • A kind of preparation method of ditetraethylammonium decahydrodecaborate

Examples

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Embodiment 1

[0015] Add 34g of sodium borohydride, 166g of tetraethylammonium chloride, 0.2g of Ni and alumina composite catalyst, 50g of deionized water, and 332g of paraffin oil in sequence in the microwave reactor with exhaust gas absorption. 300W microwave irradiation for 50s, then 800W microwave irradiation at 175~180°C for 1 hour, then take out the reaction mixture, disperse with 664g petroleum ether, filter, add 500g of acetonitrile to the filter cake, heat and reflux at 80~85°C for 1 hour and then cool Filtrate, evaporate the filtrate to dryness, then add 100g of methanol with a volume percentage of 85%, heat and reflux at 65~70°C for half an hour, then heat filter, cool the filtrate, and filter at room temperature to obtain a white crystalline ditetraethylammonium decahydrodecaborate product 34.6 g (91.5% yield). (For NMR boron spectrum, see figure 1 ). The mass ratio of Ni and alumina is 1:1.

Embodiment 2

[0017] Add 24g of sodium borohydride, 83g of tetraethylammonium chloride, 0.2g of Cu and magnesium oxide composite catalyst, 33g of deionized water, and 240g of paraffin oil in sequence in the microwave reactor with tail gas absorption. 300W microwave irradiation for 60s, then 800W microwave irradiation at 175~180°C for 50min, then take out the reaction mixture, filter it with 480g petroleum ether, add 400g acetonitrile to the filter cake, heat and reflux at 80~85°C for 1 hour, then cool and filter. After the filtrate was evaporated to dryness, 100 g of 85% methanol was added, heated and refluxed at 65 to 70° C. for half an hour, then heated and filtered, the filtrate was cooled, and filtered at room temperature to obtain 17.1 g of a white crystalline ditetraethylammonium decahydrodecaborate product (yield 90.5%). The mass ratio of Cu and magnesium oxide is 1:2. (For NMR boron spectrum, see figure 1 ).

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Abstract

The invention discloses a method preparing de-hydrogen de-boric acid bi-tetraethyl ammonium. The method comprises the following steps: sequentially adding tetraethyl ammonium chloride, sodium boro-hydride, a composite catalyst, deionized water and paraffin oil in a microwave reaction device provided with a tail gas absorption device; conducting 300 W microwave irradiation on the materials for 50-80 s at 25-30 DEG C after stirring the materials uniformly; conducting 800 W microwave irradiation for 40 min to 1 hour at 175-180 DEG C; taking out the mixture obtained from the reaction; filtering the mixture by petroleum ether; adding acetonitrile in a filter cake; conducting heating reflux, cooling and filtering; evaporating the filter liquor to dryness; adding methanol of which the volume fraction is 85%; conducting heating reflux, hot filtering, filter liquor cooling and filtering to obtain white crystalloid de-hydrogen de-boric acid bi-tetraethyl ammonium product. The method has the advantages that the method is simple and convenient to operate, short in reaction time, and high in product yield.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of ditetraethylammonium decahydrodecaborate. Background technique [0002] Ionic borohydride-based ultra-high burning rate modifiers have the advantages of high combustion value, low toxicity, and good stability. Compared with carboranes, they are more convenient to synthesize and lower in cost. The United States has started the preparation and research of this type of compound in the 1970s. Among them, U.S. Patent No. 4,138,282 discloses that this type of compound can significantly increase the burning rate of the propellant when used in composite propellants and double-base propellants. Wherein the ditetraethylammonium decahydrodecaborate is a higher ionic borohydride salt of application value, "Journal of Chemistry" No. 4 in 1978 reported "Research on boron compounds I. Synthesis of decaboron decahydrogen (B 10 h 10 2- ) new method, which a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 胡孝伦李义波王建莉杨勇王娅娟
Owner ZHENGZHOU SIGMA CHEM
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