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Method for preparing K2B12H12

A kind of K2B12H12, aprotic technology, applied in the field of preparation chemistry of ionic polyboron hydrides, can solve the problems of complex process procedure, rising preparation cost, increasing reaction species, etc.

Inactive Publication Date: 2017-06-13
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Like this, not only increased reaction species, made process procedure complicated, and must cause the preparation cost to rise

Method used

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  • Method for preparing K2B12H12

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Embodiment 1

[0035] In an inert atmosphere, the KBH 4 49.5g and about 500mL Et 3 N·BH 3 After mixing in a two-liter three-neck reaction flask, add about 440mL Et to the constant pressure dropping funnel installed on the reaction flask 3 N·BH 3 . Heating under stirring, the temperature was raised to 200°C by itself, maintained for one hour, and then raised to 215°C. After 1.5 h, about 60 mL of triethylamine was received. Add triethylamine borane dropwise to keep the liquid level in the bottle as high as possible. After 18 hours of reaction, 515 mL of distillate (60-90° C.) was received. Then the reaction intensified, and the distillation temperature increased. After 4 hours, another 100mL of liquid was received; the reaction subsided, and the amount of outgassing decreased significantly. Stop stirring, cool to about 130°C, remove the reflux and fractionation device on the three-necked flask; continue with vacuum distillation; raise the temperature to 160-180°C, and distill off the ...

Embodiment 2

[0037] Add 28g KBH in the device similar to embodiment 1 4 (500mmol) and 288g Et 3 N·BH 3 (2500mmol); heated in an Ar atmosphere, the temperature rose to 180°C (about 2 hours) by itself, hydrogen gas was released, and a small amount of liquid distilled out (Et 3 N); then heated at intervals of 5°C to 210-230°C and heated for 3 hours, the hydrogen release rate slowed down significantly, cooled to about 100°C in an Ar atmosphere, installed a decompression device, decompressed to remove volatiles, and left a light yellow The solid was treated with toluene, petroleum ether, diethyl ether and isopropanol to obtain a white powdery solid. Add deionized water to the solid to dissolve, concentrate the aqueous solution, cool, and precipitate colorless and transparent K 2 B 12 h 12 Crystal, the yield is about 50%.

Embodiment 3

[0039] In a device similar to Example 1, 2.8g KBH 4 (50mmol) and 12g Et 3 N·BH 3 (100mmol) in high purity N 2 In the atmosphere, react in diethylene glycol dimethyl ether at 130°C for 10 hours, then raise the temperature to reflux temperature for 16 hours, cool, filter, and treat the solid with dichloromethane, ether, acetonitrile, methanol and water to obtain a colorless and transparent K 2 B 12 h 12 crystals.

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Abstract

The invention provides a KBH 4 with Et 3 N·BH 3 The product after thermal reaction in an aprotic medium can be directly prepared into pure K by solvent treatment without any chemical transformation. 2 B 12 h 12 Methods. This preparation method avoids the use of highly toxic B 2 h 6 , B 5 h 9 or B 10 h 14 or its derivatives, to avoid the separation step of converting the reaction product into insoluble salts such as triethylamine salt, tetraalkylammonium salt or chitin salt or cesium salt, without passing H + Ion-column exchange, eliminating the need for KOH or K 2 CO 3 Neutralization step. The method involves few chemical species, simple procedure, routine operation, and convenient handling, and is the ideal method for preparing K 2 B 12 h 12 A method with a higher degree of greening.

Description

technical field [0001] The present invention relates to icosahedral closed cage type polyhydrogen polyborate K 2 B 12 h 12 The preparation method belongs to the field of preparation chemistry of ionic polyboron hydride compounds. Background technique [0002] Since 1960, when Hawthorne et al. isolated the bis(triethylammonium)dodecahydrododecaborate [bis(triethylammonium)dodecahydrododecaborate] in low yield for the first time in the reaction of 2-iododecaborane and triethylamine, borohydrogen chemists have Dodecahydrododecaborate anion (B 12 h 12 2- ) preparation method has been continuously improved, and a large amount of B 12 h 12 2- Compounds, their chemistry has been studied extensively, and the possibility of application of such compounds in rocket propellants, hydrogen storage materials, liquid crystal materials, optoelectronic materials, flame retardant materials, medical materials and other fields has been explored. It turns out that B 12 h 12 2- Compoun...

Claims

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Application Information

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IPC IPC(8): C01B6/21
CPCC01B6/21C01P2002/86
Inventor 单自兴杨荣杰吴冰斌绳利丽单燚明
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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