Preparation method of catalytic electrode for electrochemical synthesis of borohydride

A borohydride, catalytic electrode technology, applied in electrodes, electrolysis components, electrolysis processes, etc., can solve the problems of difficult separation and purification of products, industrialized production, lack of practical value, etc., to achieve optimized stability and reversible performance, Effects of multiple catalytically active sites, excellent electrical conductivity and corrosion resistance

Inactive Publication Date: 2020-04-28
HENAN UNIV OF SCI & TECH
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Problems solved by technology

Literature search found that the existing conversion schemes mainly use active metals Na, Mg or their hydrides NaH, MgH 2 Direct reduction of NaBO with isostrong reducing agent 2 NaBH 4 , these reactions require high temperature and high pressure conditions, and the products are not easy to separate and purify, so industrial production has not yet been realized
Cooper et al. reported the electrolysis of NaBO 2 Solution preparation NaBH 4 method (US3734842-A), that is, the cathodic reduction reaction is realized by electrolysis: BO 2 - + 6H 2 O + 8e = BH 4 - + 8OH - , but its current efficiency is very low, the electrolysis speed is slow, and noble metals are needed as electrode catalysts, the cost is high, so it still lacks due practical value

Method used

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  • Preparation method of catalytic electrode for electrochemical synthesis of borohydride
  • Preparation method of catalytic electrode for electrochemical synthesis of borohydride
  • Preparation method of catalytic electrode for electrochemical synthesis of borohydride

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preparation example Construction

[0034] A method for preparing a catalytic electrode for electrochemically synthesizing borohydride mainly comprises the following steps:

[0035] (1) Hydrothermal growth of titanium oxide micro-nano wires on the titanium substrate: select a piece of metal titanium sheet with an appropriate area and thickness, immerse it in the degreasing agent, treat it with ultrasonic waves for 20~40min, and then put it into the etching solution for 40~ Ultrasonic treatment at 60°C for 25-35min, take out the titanium sheet, wash it with distilled water, immerse it in the hydrothermal solution in an upright manner, and conduct a hydrothermal treatment at 200-250°C for 8-12h; after the hydrothermal treatment, take out the titanium sheet and wash it with water clean, and then vacuum dry at 40~60℃ for 5~8h to get TiO 2 -NWs / Ti, placed in a vacuum desiccator for standby;

[0036] (2) Ammonia nitrogen reduction of titanium oxide micro-nanowires on titanium sheet: the TiO obtained in step (1) 2 -N...

Embodiment 1

[0045] A method for preparing a catalytic electrode for electrochemically synthesizing borohydride, comprising the following steps:

[0046] Step 1: Take a 1.0 cm×1.5cm×0.3mm metal titanium sheet, immerse it in 20ml of a mixed solvent composed of acetone and absolute ethanol (the volume ratio of the two is 2:1), and ultrasonically treat it for 30 minutes; take it out and put it in In 20ml of etching solution formed by ammonium fluoride, hydrogen peroxide, nitric acid and urea (molar ratio 1:1:1:0.05), ultrasonically treat at 50°C for 30min; take out the titanium sheet, wash it with distilled water, and set it upright immersion in 1.0 mol∙l -1 In the hydrothermal solution of tetramethylammonium hydroxide, hydrothermal treatment was carried out at 200°C for 8h; after hydrothermal treatment, the titanium sheet was taken out, cleaned with water, and then vacuum-dried at 40°C for 5h to obtain TiO 2 -NWs / Ti, placed in a vacuum desiccator for standby;

[0047] Step 2: TiO obtained ...

Embodiment 2

[0051] Step 1: Take a 1.0 cm×2.0cm×0.5mm metal titanium sheet, immerse it in 20ml of a mixed solvent composed of acetone and absolute ethanol (the volume ratio of the two is 2:1), and ultrasonically treat it for 20 minutes; take it out and put it in In 20ml of etching solution formed by ammonium fluoride, hydrogen peroxide, nitric acid and urea (molar ratio 1:1:1:0.05), ultrasonically treat at 60°C for 25min; take out the titanium sheet, wash it with distilled water, and set it upright way to immerse in 2.0 mol∙l -1 In the hydrothermal solution of tetramethylammonium hydroxide, hydrothermal treatment was carried out at 250°C for 12h; after hydrothermal treatment, the titanium sheet was taken out, cleaned with water, and then vacuum-dried at 60°C for 8h to obtain TiO 2 -NWs / Ti, placed in a vacuum desiccator for standby;

[0052] Step 2: TiO obtained in Step 1 2 -NWs / Ti is placed in a tube-type atmosphere furnace at a rate of 150ml∙min -1 Nitrogen gas was fed at the same flow...

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Abstract

The invention provides a preparation method of a catalytic electrode for electrolytic synthesis of hydroboron. The preparation method comprises the following steps of: carrying out titanium oxide micro-nanometer wire hydrothermal growth on a titanium substrate; carrying out ammonia nitrogen reduction of a titanium oxide micro-nanometer wire on the titanium substrate; chemically depositing a composite metal Ni-Pb sub-layer; and chemically replacing and depositing an Au surface layer. The prepared catalytic electrode is high in rigidness, resistant to corrosion, stable in performances, porous insurface and quite high in conductivity; by mutual collaborative action of a plurality of metals, the catalytic electrode has good catalytic activity. According to measurement, after a finished electrode product is used as a cathode catalytic electrode, the average current efficiency is as high as 35%, and a NaBH4 product can be obtained by reduction. The preparation method provided by the invention is simple in steps and convenient to operate, realizes the aim that a byproduct metaborate generated after the hydroboron is hydrolyzed to generate hydrogen is transformed into hydroboron again, thus the production cost and the application cost of the hydroboron are lowered, boron resources are saved, and the environmental pollution is reduced.

Description

technical field [0001] The invention relates to a catalyst for preparing borohydride by electrolytically reducing metaborate based on electrochemical principles and a method for preparing a catalytic electrode, which belong to the field of new energy materials and related fields. Background technique [0002] The increasing energy crisis and environmental pollution are the main challenges facing human society, and actively seeking high-efficiency, high-energy, environment-friendly green alternative energy is the key way to solve these problems. Hydrogen energy has high energy density, fast conversion speed, high conversion efficiency, and can be discharged cleanly (the product is water). It is regarded as an ideal alternative energy source for traditional fossil fuels. Therefore, the development and utilization of hydrogen energy has attracted widespread attention in recent years. . With the improvement of proton exchange membrane fuel cell (PEMFC) technology, the status of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/06C25B1/14
CPCC25B1/14C25B11/091
Inventor 张军王杨董亚娜朱一明段永华杜西刚米刚宋帮才
Owner HENAN UNIV OF SCI & TECH
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