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Process method for preparing ammonia borane from boroxol acid ammonium through electrochemical reduction in recycling manner

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 that ammonia borane has not been found, and achieve mild preparation conditions, low energy consumption, and cheap and easy-to-obtain raw materials Effect

Inactive Publication Date: 2015-05-20
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

The invention discloses a process method for preparing ammonia borane from boroxol acid ammonium through electrochemical reduction in a recycling manner. According to the process method, electrochemical reduction is carried out by virtue of a three-dimensional negative electrode with relatively high hydrogen overpotential under an electrochemical reduction principle based on ammonia borane hydrolysate ammonia metaborate as a raw material, so that conversion of boroxol acid radical ions into borone hydrogen acid radical ions is promoted. White floppy ammonia borane solid can be prepared through operation steps such as boroxol acid ammonium electroreduction, freeze-drying dehydration, dissolution backflowing, centrifugal treatment, rotation evaporation, crystallization and the like. The process method is gentle in preparation condition, short in process, low in energy consumption, simple and convenient to operate, free of waste discharge and free of environment pollution, and the raw materials which are byproducts generated from hydrolysis hydrogen release of ammonia borane are low in price and easily available. In addition, due to adoption of an appropriate electrode material, the current efficiency of electroreduction of a negative electrode chamber to generate hydroboron 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 Applications(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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