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Preparation method of nanomaterial for electrocatalytic hydrogen evolution

一种纳米材料、电催化的技术，应用在催化剂活化/制备、化学仪器和方法、物理/化学过程催化剂等方向，能够解决产物反应活性位点少、电催化析氢性能差、制备原材料成本高等问题，达到没有坍塌、良好析氢性能、好催化效果的效果

Active Publication Date: 2021-03-16
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many preparation methods, the cost of raw materials is high, the preparation process is more polluting to the environment, and no product with a through-hole structure is produced. The product has few reactive sites, poor electrocatalytic hydrogen evolution performance, and poor stability. , short service life, poor electrical conductivity, difficult to recycle

Method used

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  • Preparation method of nanomaterial for electrocatalytic hydrogen evolution
  • Preparation method of nanomaterial for electrocatalytic hydrogen evolution
  • Preparation method of nanomaterial for electrocatalytic hydrogen evolution

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A method for preparing an electrocatalytic hydrogen evolution nanomaterial, which is prepared by the following steps in sequence:

[0028] In the Erlenmeyer flask, weigh 2.48g ammonium molybdate tetrahydrate (NH 4 ) 6 Mo 7 o 24 .4H 2 Add 40ml of uniform deionized water containing 3.28ml of aniline solution to dissolve it, pass through 99.99% nitrogen for protection, the gas flow rate is 25ml / min, at the same time, use microwave to heat to 50 ° C, and then slowly add 1mol / L Adjust the pH value to 4.0 with dilute hydrochloric acid solution, keep at 50 degrees Celsius for 4h to obtain the Mo-MOF precursor intermediate, and then wash with distilled water and ethanol solution respectively for 3 times (the mass of the Mo-MOF precursor intermediate, distilled water and ethanol : volume: volume = 1:45:45), and then centrifuged at 2500 rpm for 15 minutes, and then freeze-dried. Mo-MOF precursors. Transfer the Mo-MOF precursor to the alumina ark, and weigh 2g of sodium hypo...

Embodiment 2

[0034] A method for preparing an electrocatalytic hydrogen evolution nanomaterial, which is prepared by the following steps in sequence:

[0035] In the Erlenmeyer flask, weigh 2.48g ammonium molybdate tetrahydrate (NH 4 ) 6 Mo 7 o 24 .4H 2Add 40ml of uniform deionized water containing 3.28ml of aniline solution to dissolve it, pass through 99.99% nitrogen for protection, the gas flow rate is 20ml / min, at the same time, use microwave to heat to 45°C, and then slowly add 0.8mol / L dilute hydrochloric acid solution to adjust the pH value to 4.5, keep at 45°C for 6h to obtain the Mo-MOF precursor intermediate, and then wash with distilled water and ethanol solution for 3 times respectively (the Mo-MOF precursor intermediate, distilled water and ethanol (mass: volume: volume = 1:40:40), and then centrifuged at 1500 rpm for 15 minutes, and then freeze-dried. The freeze-drying temperature is -45°C, the vacuum is 50Pa, and the drying time is 48h. A precursor containing Mo-MOF is...

Embodiment 3

[0038] A method for preparing an electrocatalytic hydrogen evolution nanomaterial, which is prepared by the following steps in sequence:

[0039] In the Erlenmeyer flask, weigh 2.48g ammonium molybdate tetrahydrate (NH 4 ) 6 Mo 7 o 24 .4H 2 Add 40ml of uniform deionized water containing 3.28ml of aniline solution to dissolve it, pass through 99.99% nitrogen for protection, the gas flow rate is 30ml / min, at the same time, use microwave to heat to 55 ° C, and then slowly drop 1.2mol / L dilute hydrochloric acid solution to adjust the pH value to 3.5, keep at 55°C for 3h to obtain the Mo-MOF precursor intermediate, and then wash with distilled water and ethanol solution for 3 times respectively (the Mo-MOF precursor intermediate, distilled water and ethanol (mass: volume: volume = 1:40:40), and then centrifuged at 3000 rpm for 10 minutes, and then freeze-dried. The freeze-drying temperature is -55°C, the vacuum is 10Pa, and the drying time is 48h. A precursor containing Mo-MO...

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Abstract

The invention discloses a preparation method of a nanomaterial for electrocatalytic hydrogen evolution. The nanomaterial is prepared from ammonium molybdate tetrahydrate, an aniline solution and sodium hypophosphite in a mass ratio of 2.48: 40: 2 through the following sequential steps: (1) preparing a Mo-MOF precursor via a solution method, namely dissolving the ammonium molybdate tetrahydrate inthe aniline solution, and introducing nitrogen for protection; and (2) preparing the MoP / carbon composite nanomaterial via a heat treatment method, namely transferring the Mo-MOF precursor into an aluminum oxide ark, adding sodium hypophosphite into another aluminum oxide ark, putting the aluminum oxide ark to the upstream position of a tube furnace, introducing a mixed gas of hydrogen and nitrogen, conducting heating to 750-850 DEG C, and keeping the temperature for 3-6 hours. The preparation method is simple in raw material, simple in whole process and convenient to operate, and the preparedcomposite nanomaterial has a through hole structure.

Description

[0001] This application is for a divisional application with the application number 201810451177.1 and the title of the invention "A Molybdenum Phosphide / Carbon Composite Nanomaterial for Alkaline Electrocatalytic Hydrogen Evolution". technical field [0002] The invention relates to the technical field of preparation of basic non-noble metal catalysts, in particular to a preparation method of electrocatalyzed hydrogen evolution nanomaterials. Background technique [0003] The noble metal platinum and its alloys are currently the most commonly used catalysts for electrocatalytic hydrogen production due to their low potential and high electrochemical stability in acidic solutions. However, its high cost and scarce resources hinder its practical application, especially in an alkaline environment, which consumes more energy, which limits its application in the field of hydrogen batteries. At present, both theoretical and experimental studies have proved that nanostructured tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J35/00B01J35/10B01J37/08B01J37/10B01J37/28C25B1/02C25B11/091
CPCB01J27/19B01J37/086B01J37/10B01J37/28C25B1/02B01J35/33B01J35/643Y02E60/36
Inventor 陈文波刘碧桃姚昱岑彭玲玲韩涛
Owner CHONGQING UNIV OF ARTS & SCI