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Preparation method of caesium decahydrodecaborate

A technology of decahydrodecaboric acid and ditetraethylammonium decahydrodecaborate, which is applied in the field of cesium decahydrodecaborate, can solve the problems of long route and many reaction steps, and achieve high yield

Active Publication Date: 2013-09-11
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Therefore, this method reaction step is more, and route is longer

Method used

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  • Preparation method of caesium decahydrodecaborate
  • Preparation method of caesium decahydrodecaborate
  • Preparation method of caesium decahydrodecaborate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Step 1: Add 7.6g (20mmol) ditetraethylammonium decahydrodecaborate and 180mL methanol into a reaction flask with a reflux and stirring device, stir, and heat to 60°C to dissolve ditetraethylammonium decahydrodecaborate ;

[0032] Step 2, add 8.0g (48mmol) cesium chloride and 200mL methanol into the reaction flask with condenser tube, stirrer thermometer and feeding valve, heat up to 60°C under stirring to dissolve cesium chloride, keep the temperature, and Add the ditetraethylammonium decahydrodecaborate methanol solution prepared in Step 1 into the reaction flask under strong stirring. After adding the materials, continue to stir and react at 60°C for 2 hours, cool to room temperature, and filter the reaction mixture , washed the filter cake with methanol, and dried the obtained solid to obtain 7.5 g of cesium decahydrodecaborate, with a yield of 98.7%.

[0033] Structure Identification:

[0034] Elemental analysis (B 10 h 10 Cs 2 ):

[0035] Calculated value (%)...

Embodiment 2

[0041] Step 1: Add 7.6g (20mmol) ditetraethylammonium decahydrodecaborate and 150mL methanol into a reaction flask with a reflux and stirring device, stir, and heat to 65°C to dissolve the material;

[0042] Step 2: Add 6.7g (40.2mmol) cesium chloride and 180mL methanol into a reaction flask with a condenser tube, a stirrer thermometer and a feed valve, heat up to 65°C under stirring to dissolve the material, maintain this temperature, and Add the methanol solution of ditetraethylammonium decahydrodecaborate prepared in Step 1 into the reaction flask under stirring. After the addition, continue stirring and reacting for 1 h at 65°C, cool to room temperature, and filter the reaction mixture. The filter cake was washed with methanol, and the obtained solid was dried to obtain 7.3 g of cesium decahydrodecaborate with a yield of 96.1%.

[0043] The structure identification result of the product obtained in this example is the same as that in Example 1.

Embodiment 3

[0045] Step 1: Add 7.6g (20mmol) bistetraethylammonium decahydrodecaborate and 250mL methanol into a reaction flask with a reflux and stirring device, stir, and heat to 40°C to dissolve the material;

[0046] Step 2: Add 16.6g (99.6mmol) of cesium chloride and 976mL of methanol into the reaction flask, heat to 40°C with stirring to dissolve; maintain the temperature, and under strong stirring, decahydrodeca prepared in step 1 Add the methanol solution of ditetraethylammonium borate into the reaction flask, continue to stir and react for 6 hours at a temperature of 40°C, filter, wash the filter cake with methanol, and dry to obtain 7.4 g of cesium decahydrodecaborate, with a yield of 97.4%.

[0047] The structure identification result of the product obtained in this example is the same as that in Example 1.

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Abstract

The invention relates to caesium decahydrodecaborate and provides a preparation method of the caesium decahydrodecaborate. The preparation method comprises the following steps of: with ditetraethylammonium decahydrodecaborate as a raw material and methanol as a solvent, enabling the tetraethylammonium decahydrodecaborate and caesium chloride to react in mole ratio of 1: 2-1: 5 for 1-6 hours at 40-65 DEG C while stirring, and preparing the caesium decahydrodecaborate adopting a one-step method. The preparation method of the caesium decahydrodecaborate comprises only one reaction step, and a preparation line in the prior art adopts a two-step reaction step; and according to the preparation method disclosed by the invention, the yield is higher, and the highest yield in terms of tetraethylammonium decahydrodecaborate can be 98.7%.

Description

technical field [0001] The invention relates to cesium decahydrodecaborate, in particular to a preparation method of cesium decahydrodecaborate. Background technique [0002] The ionic borohydride type ultra-high burning rate regulator has the advantages of high combustion calorific value, low toxicity, good stability, etc. Compared with carborane, it has the characteristics of convenient synthesis and low cost. Therefore, the United States and other developed countries have started the preparation and application research of this type of compound in the 1970s. The U.S. patent [US4138282] discloses this type of compound Both composite propellants and double-base propellants can significantly increase the burning rate of propellants. Among them, cesium decahydrodecaborate is an ionic borohydride salt with high application value, and the research on its synthesis method is as follows. [0003] [Chemistry of boranes.Ⅷ.Salts and acids of B 10 h 10 and B 12 h 12 , E.L.Muett...

Claims

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Application Information

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IPC IPC(8): C01B35/18
Inventor 薛云娜吕剑李亚妮王为强李娇毅万洪李凤仙杨建明李春迎
Owner XIAN MODERN CHEM RES INST
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