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Bis(tetrazolyl) boric acid ionic liquid and preparation method thereof

A technology of ionic liquid and imidazolium cation, which is applied in the field of bis-boric acid ionic liquid and its preparation, can solve the problems of explosion hazard and achieve the effects of reducing risk, wide liquid range, and good thermal stability

Active Publication Date: 2017-09-12
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually by powdery 1H-tetrazole and sodium borohydride or potassium borohydride, high yield bis(tetrazole) borate sodium salt or potassium salt can be obtained under stirring (Lu D.et al.Complexes of the [K(18 -Crown-6)] + Fragment with bis(tetrazolyl)borate ligands:unexpected boron-nitrogen bond isomerism and associated enforcement ofκ 3 -N,N',H-LigandChelation.Inorg.Chem.2010,49,5795-5797), but there is a certain risk in the preparation of tetrazole powder, and there is a potential explosion hazard when the powder is stirred

Method used

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  • Bis(tetrazolyl) boric acid ionic liquid and preparation method thereof
  • Bis(tetrazolyl) boric acid ionic liquid and preparation method thereof
  • Bis(tetrazolyl) boric acid ionic liquid and preparation method thereof

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Embodiment 1

[0048] The preparation steps of 1-allyl-3-methyl-1H-imidazole bis(tetrazole) borate are as follows:

[0049] (1) Under the protection of argon, first add 106mmol of sodium borohydride to 70mL of anhydrous acetonitrile, and then add 212mmol of 1H-tetrazole in batches to obtain the reaction solution I; the reaction solution I is refluxed and stirred at 85°C for 72h , cooled to room temperature, filtered and collected solid matter, vacuum-dried to obtain bis(tetrazole) borate sodium salt;

[0050] (2) Add 40mmol 1-allyl-3-methyl-1H-imidazolium chloride salt and 44mmol bis(tetrazole) borate sodium salt to 100mL acetonitrile to obtain reaction solution II; reaction solution II was stirred at 25°C After reacting for 7 days, filter and collect the filtrate; after removing the acetonitrile solvent in the filtrate by rotary evaporation, first dissolve it with 50mL of dichloromethane, then wash it with water three times, then dry it with anhydrous sodium sulfate, then carry out vacuum d...

Embodiment 2

[0060] Synthesis of 1-ethyl-3-methyl-1H-imidazolium bis(tetrazole)borate

[0061] (1) Under the protection of argon, first add 106mmol of sodium borohydride into 70mL of anhydrous acetonitrile, and then add 212mmol of 1H-tetrazole in batches to obtain the reaction solution I; the reaction solution I was refluxed and stirred for 72 hours at 85°C, then cooled to room temperature, filtered and collected solid matter, and dried in vacuo to obtain bis(tetrazole) borate sodium salt;

[0062] (2) Add 40mmol 1-ethyl-3-methyl-1H-imidazolium chloride salt and 44mmol bis(tetrazole) borate sodium salt to 100mL acetonitrile to obtain reaction solution II; reaction solution II was stirred at 25°C for 7 Days later, filter and collect the filtrate; after the acetonitrile solvent in the filtrate was removed by rotary evaporation, dissolve it with 50mL of dichloromethane, wash with water three times, then dry with anhydrous sodium sulfate, then carry out vacuum distillation, and finally vacuum ...

Embodiment 3

[0072] Synthesis of 1-ethylpyridine bis(tetrazole) borate

[0073] (1) Under the protection of argon, first add 106mmol of sodium borohydride to 70mL of anhydrous acetonitrile, and then add 212mmol of 1H-tetrazole in batches to obtain the reaction solution I; after the reaction solution I was refluxed and stirred at 85°C for 72h, Cool to room temperature, filter and collect solid matter, vacuum dry to obtain bis(tetrazole) borate sodium salt;

[0074] (2) Add 40mmol 1-ethylpyridinium bromide and 44mmol bis(tetrazole)borate sodium salt into 100mL of acetonitrile to obtain reaction solution II; reaction solution II was stirred and reacted at 25°C for 7 days, filtered and the filtrate was collected; After evaporating the acetonitrile solvent in the filtrate, first dissolve it with 50mL of dichloromethane, then wash it with water three times, then dry it with anhydrous sodium sulfate, then carry out vacuum distillation, and finally dry it in vacuum to obtain 8.809g 1-ethylpyridine b...

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Abstract

The invention relates to bis(tetrazolyl) boric acid ionic liquid and a preparation method thereof and belongs to the field of organic synthesis and spontaneous combustion liquid propellants. The bis(tetrazolyl) boric acid ionic liquid is prepared through replacement reaction between bis(tetrazolyl) sodium borate and corresponding imidazole, pyrrolidine or pyridine halogeno salt in an organic solvent; furthermore, the bis(tetrazolyl) boric acid ionic liquid has very high nitrogen content, positive enthalpy formation, high density, wide liquid range, lower viscosity, good thermal stability, acceptable ignition delay time and potential application value in the field of spontaneous combustion liquid propellants. The invention further provides a preparation method of safe bis(tetrazolyl) sodium borate. The method can stably control system temperature and meanwhile reduces danger in a stirring process by adding an organic solvent.

Description

technical field [0001] The invention relates to a bis(tetrazole) borate ionic liquid and a preparation method thereof, belonging to the field of organic synthesis and spontaneous combustion liquid propellant. Background technique [0002] Propellants are gunpowder that burn regularly to release energy and gases to propel rockets and missiles. Liquid propellants are divided into unit propellants and binary propellants. A unit propellant is a substance that releases thermochemical energy without the addition of additional components. Binary propellant fuel and oxidizer are stored separately and mixed only in the combustion chamber. Binary propellants can be classified into non-pyrophoric and pyrophoric types. The self-igniting binary propellant fuel and oxidant can undergo spontaneous combustion reaction, eliminating the need for an ignition device, and can control the start and end of combustion at any time according to needs. Traditional self-igniting binary propellant f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 陈甫雪李兴业
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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