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A kind of spherical preparation method of cuprous tetraethylammonium decahydrodecaborate

The technology of tetraethylammonium decahydrodecaborate and decahydrodecaboric acid is applied in the field of spheroidization preparation of tetraethylammonium decahydrodecaborate cuprous acid, which can solve the problems of low degree of spheroidization and high particle aspect ratio, Achieve the effect of high degree of spheroidization, good process performance and easy leveling

Active Publication Date: 2017-03-08
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a kind of tetraethyl decahydrodecaborate with an aspect ratio close to 1 and a high degree of spheroidization aiming at the high aspect ratio and low spheroidization degree of product particles in the above-mentioned prior art. Method for preparing spheroidized particles of cuprous ammonium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Spherical crystallization of tetraethylammonium cuprous decahydrodecaborate

[0016] (1) Dissolve cuprous tetraethylammonium decahydrodecaborate in acetonitrile at a temperature of 90°C, wherein the mass ratio of cuprous tetraethylammonium decahydrodecaborate to acetonitrile is 1:2.

[0017] (2) Add methanol to the solution obtained in step (1) under stirring at a temperature of 90°C, wherein the mass ratio of tetraethylammonium decahydrodecaborate cuprous to methanol is 1:30.

[0018] (3) Under the condition of stirring, the mixed system obtained in step (2) is cooled to -10°C, and then filtered, washed, and dried to obtain spherical cuprous tetraethylammonium decahydrodecaborate, with an average particle size of 100 microns with an aspect ratio of 1.1.

Embodiment 2

[0019] Example 2 Spherical crystallization of tetraethylammonium cuprous decahydrodecaborate

[0020] (1) Dissolve cuprous tetraethylammonium decahydrodecaborate in N,N-dimethylformamide at 0°C, wherein cuprous tetraethylammonium decahydrodecaborate and N,N-di The mass ratio of methylformamide is 1:50.

[0021] (2) Add ethanol to the solution obtained in step (1) under stirring at a temperature of 0°C, wherein the mass ratio of cuprous tetraethylammonium decahydrodecaborate to ethanol is 1:200.

[0022] (3) Cool the mixed system obtained in step (2) to -15°C while stirring, then filter, wash, and dry to obtain spherical cuprous tetraethylammonium decahydrodecaborate, with an average particle size of 200 microns with an aspect ratio of 1.2.

Embodiment 3

[0023] Example 3 Spherical crystallization of tetraethylammonium cuprous decahydrodecaborate

[0024] (1) Dissolve cuprous tetraethylammonium decahydrodecaborate in dimethyl sulfoxide at a temperature of 200° C., wherein the mass ratio of cuprous tetraethylammonium decahydrodecaborate to dimethyl sulfoxide is 1: 0.5.

[0025] (2) Add water to the solution obtained in step (1) under stirring at a temperature of 150° C., wherein the mass ratio of tetraethylammonium decahydrodecaborate cuprous to water is 1:0.5.

[0026] (3) Cool the mixed system obtained in step (2) to 50°C while stirring, then filter, wash, and dry to obtain spheroidized cuprous tetraethylammonium decahydrodecaborate with an average particle size of 50 Micron, aspect ratio is 1.2.

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PUM

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Abstract

The invention discloses a spheroidized preparation method of cuprous decahydrodecaborate tetraethylammonium. The method comprises the following steps: (1) dissolving cuprous decahydrodecaborate tetraethylammonium in 0.5-50 times of a solvent A by mass at 0-200 DEG C, wherein the solvent A is dimethylsulfoxide, N, N-dimethylformamide, acetonitrile or N-methyl-2-pyrrolidinone; (2) adding 0.5-200 times of a solvent B in mass into the solution obtained in the step (1) at 0-150 DEG C while stirring and stirring and uniformly and fully mixing, wherein the solvent B is ethanol, methanol, isopropanol, normal butanol, water and acetone; and (3) cooling the mixed system obtained in the step (2) under stirring to (-15)-50 DEG C and filtering, washing and drying to obtain the spheroidized cuprous decahydrodecaborate tetraethylammonium, wherein the length-diameter ratio reaches 1.1 and the yield reaches 95%. The method disclosed by the invention is used for spheroidized granule preparation process of cuprous decahydrodecaborate tetraethylammonium. The product as a functional fuel with a high heat value and a high burning rate is used in a solid propellant or a fuel-enriched explosive.

Description

technical field [0001] The invention relates to a method for preparing tetraethylammonium cuprous decahydrodecaborate into a spheroid, belonging to the field of energetic materials. Background technique [0002] Polyhedral borohydride compounds have aromaticity, heat resistance and excellent chemical stability due to the delocalization of boron cage electrons, and are used in many fields such as high-energy fuels, functional materials, biomedicine and catalysts. Cuprous tetraethylammonium decahydrodecaborate contains cuprous ions and cage-shaped decahydrodecaborate ions in the molecule, so it has both the combustion and catalytic function of aluminum powder in solid propellants or fuel air explosives, and because of its high heat It has the function of increasing the calorific value, so it is a polyhedral borohydride compound with high application value. However, in the prior art, tetraethylammonium decahydrodecaborate obtained through chemical reaction synthesis has a smal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 薛云娜吕剑李娇毅万洪郝志军杜咏梅李春迎陆居有孙道安王志轩张建伟
Owner XIAN MODERN CHEM RES INST
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