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New process for producing potassium borohydride

A technology of potassium borohydride and sodium hydride, which is applied in the field of preparing potassium borohydride, and can solve the problems of low yield and the like

Inactive Publication Date: 2020-03-06
NINGXIA BEST PHARMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention patent with the publication number CN 107601432 A discloses a method for preparing potassium borohydride by using potassium metaborate, but the yield of this method is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 41g of waste potassium metaborate and add it to 123g of methanol, heat and reflux for 100min, then evaporate to dryness to obtain 84g potassium tetramethoxy borate, add potassium tetramethoxy borate to 154g of 30% sodium hydride / white oil system, and hydrogenate In the sodium / white oil dispersion system, the sodium hydride is 60%, and the white oil is 40%, wherein the molar ratio of tetramethoxy boropotassium to sodium hydride is 1.08, and the heating rate of the reaction is 8°C / min, heated to 220°C, The stirring speed was 150r / min, and the reaction was 300min; after the reaction, the temperature was lowered to 0°C at 10°C / min; the temperature was kept for 1h; then extracted with isopropylamine, and the upper layer was evaporated to dryness to obtain 33g of potassium borohydride.

Embodiment 2

[0022] Take 41g of waste potassium metaborate and add it to 123g of methanol, heat and reflux for 100min, then evaporate to dryness to obtain 84g potassium tetramethoxy borate, add potassium tetramethoxy borate to 154g of 30% sodium hydride / white oil system, and hydrogenate In the sodium / white oil dispersion system, the sodium hydride is 60%, and the white oil is 40%, wherein the molar ratio of potassium tetramethoxyborate to sodium hydride is 1.10, and the heating rate of the reaction is 12°C / min, heated to 300°C, The stirring speed is 200r / min, and the reaction is 60min; after the reaction, the temperature is lowered to 0°C at 10°C / min; the temperature is kept for 1-2h; then extracted with isopropylamine, and the upper layer is evaporated to dryness to obtain 34g of potassium borohydride.

Embodiment 3

[0024] Take 41g of waste potassium metaborate and add it to 123g of methanol, heat and reflux for 100min, then evaporate to dryness to obtain 84g potassium tetramethoxyborate, add potassium tetramethoxyborate to 154g of 30% sodium hydride / white oil system, and hydrogenate In the sodium / white oil dispersion system, sodium hydride is 60%, white oil is 40%, heated to 270°C for 120 minutes, wherein the molar ratio of potassium tetramethoxyborate to sodium hydride is 1.09, and the heating rate of the reaction is 10°C / min, heated to 270°C, the stirring speed was 180r / min, and reacted for 120min; after the reaction was completed, the temperature was lowered to 0°C at 10°C / min; kept for 1-2h; potassium.

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PUM

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Abstract

The invention discloses a method for preparing potassium borohydride by using potassium metaborate. The method comprise the following steps: first adding potassium metaborate into excess methanol, andcarrying out a reaction to obtain a solution of potassium tetramethanolatoborate; performing distillation to obtain a potassium tetramethanolatoborate solid; then adding the potassium tetramethanolatoborate solid into a sodium hydride / white oil dispersion system, performing stirring, raising the temperature to 220 DEG C-300 DEG C for carrying out a reaction to obtain a potassium borohydride, sodium methoxide / white oil dispersion system, wherein a molar ratio of potassium tetramethanolatoborate to sodium hydride is 1.08-1.10, the temperature raising rate of the reaction is 8-12 DEG C / min, andthe reaction time is 60 min-300 min; performing cooling at a rate of 10 DEG C / min to 0 DEG C after the reaction is completed; keeping the temperature for 1-2 h; and performing extraction to obtain potassium borohydride. According to the method, the waste potassium metaborate is converted to potassium tetramethanolatoborate, and then a high-temperature condensation reaction with sodium hydride is carried out to obtain potassium borohydride. The recycling of potassium metaborate can be realized, and the yield is stably improved to 80% or more.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing potassium borohydride by using potassium metaborate. Background technique [0002] Potassium borohydride is an excellent reducing agent for the reduction reaction of organic selective groups, and can reduce organic functional groups RCHO, RCOR, RCOCl to RCH2, CHR2, HOHR, RCH2OH, etc.; it can also be used to produce hydrogen and other boron Hydrides are widely used in analytical chemistry, paper industry, treatment of mercury-containing wastewater, and synthesis of cellulose potassium. [0003] The preparation of potassium borohydride is mainly obtained by double decomposition method, and the reaction equation is as follows: [0004] NaBH4+KOH=KBH4+NaOH [0005] Potassium borohydride is used to reduce aldehydes, ketones, and acid chlorides and is oxidized to produce a large amount of waste. Its main component is potassium metaborate. Waste is m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/21
CPCC01B6/21
Inventor 郑志浩杨彬张顺利
Owner NINGXIA BEST PHARMA CHEM CO LTD
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