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Process method for preparing ammonia borane by recycling ammonium booxate electrochemical reduction

A technology of ammonium oxoborate and process method, which is applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems such as ammonia borane that has not been discovered, achieve mild preparation conditions, improve current efficiency, and cheap and easy-to-obtain raw materials Effect

Inactive Publication Date: 2017-04-12
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, so far, do not find the open literature that directly utilizes ammonium metaborate to prepare ammonia borane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) In an electrolytic cell with a cation exchange membrane installed in the middle and a volume of 500mL for both the positive and negative chambers, add 400mL of hydrochloric acid with a concentration of 1.0mol / L into the anode chamber, and insert a titanium electrode. Put an aqueous solution containing 5% ammonium metaborate, 5% ammonia and 1% tetramethylammonium hydroxide into the cathode chamber, and at the same time, pass helium into the closed cathode chamber, choose sponge titanium as the cathode, and heat it at 25°C and The current density is 50mA / cm 2 Under the condition of electrolysis for 2h;

[0031] (2) After the electrolysis, transfer the electrolyte in the cathodic chamber into a freeze dryer, and carry out freeze-drying treatment at -40°C and a vacuum of 20Pa for 10 hours until the moisture content is lower than 1.0%;

[0032] (3) Put the solid material obtained after freeze-drying into the reflux container, add 200mL tetrahydrofuran, stir and dissolve...

Embodiment 2

[0034] (1) In an electrolytic cell with a cation exchange membrane installed in the middle and a volume of 500mL for both the positive and negative chambers, add 400mL of sulfuric acid with a concentration of 5.0mol / L into the anode chamber, and insert a platinum electrode. Put an aqueous solution containing 40% ammonium tetraborate, 20% ammonia and 25% tetramethylammonium hydroxide into the cathode chamber, and at the same time, pass nitrogen into the closed cathode chamber, choose Raney nickel as the cathode, at 80 ℃ and The current density is 200mA / cm 2 Under the condition of electrolysis for 10h;

[0035] (2) After the electrolysis, transfer the electrolyte in the cathodic chamber into a freeze dryer, and freeze-dry it for 15 hours at -50°C and a vacuum of 15Pa until the moisture content is lower than 1.0%;

[0036] (3) Put the freeze-dried solid material into a reflux container, add 200mL of dioxane, stir and dissolve continuously at a temperature of 50°C, and reflux for...

Embodiment 3

[0038] (1) In an electrolytic cell with a cation exchange membrane in the middle and a volume of 500mL in both chambers, add 400mL of sodium hydroxide with a concentration of 2.0mol / L into the anode chamber, and insert a graphite electrode. Fill the cathode chamber with an aqueous solution containing 20% ​​ammonium pentaborate, 10% ammonia and 10% tetramethylammonium hydroxide, and at the same time pass helium into the closed cathode chamber, and select the composite electrode NLM / C as the cathode. 50°C and a current density of 150mA / cm 2 Under the condition of electrolysis for 6h;

[0039] (2) After the electrolysis, transfer the electrolyte in the cathodic chamber into a freeze dryer, and freeze-dry it at -45°C and a vacuum of 18Pa for 12 hours until the moisture content is lower than 1.0%;

[0040] (3) Put the freeze-dried solid into a reflux container, add 200mL of methyl n-butyl ether, stir and dissolve continuously at a temperature of 30°C, and reflux for 4 hours; then,...

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Abstract

A process for preparing ammonia borane by recycling the electrochemical reduction of ammonium borate, using ammonia borane hydrolysis product ammonium metaborate as the raw material, and according to the principle of electrochemical reduction, electrolytic reduction is carried out with the help of a three-dimensional cathode with a high hydrogen overpotential, which can Promote the transformation of boronate ions into borohydride ions. Through electrolytic reduction of ammonium borate, freeze-drying and dehydration, dissolution and reflux, centrifugation, rotary evaporation and crystallization, a white and loose ammonia borane solid was prepared. The method has mild preparation conditions, short process, low energy consumption, simple operation, no waste discharge, and no environmental pollution. The raw material used belongs to the by-product of ammonia borane water decomposing hydrogen, and is cheap and easy to obtain. Moreover, due to the adoption of appropriate electrode materials, the current efficiency of borohydride generated by electrolytic reduction in the cathode chamber can be improved.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of new energy materials, in particular to a process for preparing ammonia borane, a hydrogen storage material, by recycling ammonium booxate electrochemically. Background technique [0002] Ammonia Borane, Ammonia Borane, molecular formula NH 3 BH 3 . The melting point of ammonia borane is 104°C. It exists as a solid at normal temperature and pressure. It is soluble in water or polar solvents. It is relatively stable in the air, non-volatile, non-toxic and odorless. The theoretical hydrogen content of ammonia borane is 19.59 wt%. It is the hydrogen storage compound with the largest unit hydrogen content found so far. It can release hydrogen through pyrolysis or catalytic hydrolysis. The hydrogen release temperature is low, safe, reliable, and environmentally friendly , and thus is regarded as one of the most promising hydrogen storage materials. [0003] However, the synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04C25B3/25
Inventor 张军李华博姚海瑞张豪宋帮才杜西刚米刚
Owner HENAN UNIV OF SCI & TECH
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