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Method for preparing catalyst through solid-state electroreduction

A catalyst and solid-state technology, which is applied in the field of solid-state electroreduction to prepare catalysts, can solve the problem of not being able to solve the problem of one-time large-scale preparation of homogeneous catalysts

Active Publication Date: 2020-07-28
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It does not solve the need for one-time large-scale preparation of homogeneous catalysts

Method used

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  • Method for preparing catalyst through solid-state electroreduction
  • Method for preparing catalyst through solid-state electroreduction
  • Method for preparing catalyst through solid-state electroreduction

Examples

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preparation example Construction

[0025] The reaction device for preparing catalyst of the present invention is as figure 1 As shown, the device includes an insulating tube 13, the two ends of the insulating tube 13 shown are respectively connected to the air inlet port 9 and the gas outlet port 11, and one side of the air inlet port 9 is provided with an air inlet and a positive lead wire inlet, and the air inlet and The positive lead wire inlet is respectively connected to the air intake pipe 10 and the positive lead wire tube 4, and the air outlet port 11 side is provided with an air outlet and a negative electrode lead wire inlet, and the gas outlet and the negative electrode lead wire inlet are respectively connected to the air outlet pipe 12 and the negative electrode lead wire tube 7;

[0026] The insulating tube 13 is provided with a sample tank 2 for placing the sample 1. The two ends of the sample 1 are respectively connected to the positive electrode 3 and the negative electrode 6. The positive elect...

Embodiment 1

[0037] Take 100mg carbon black material (BP), add 30ml 6M HNO 3 , ultrasonic dispersion for 1h, adding 20mg of Pt ions (H 2 Cl 6 Pt solution is the Pt source), stirred in an oil bath at 80°C for 6h. Excess solvent was rotovapped to give a solid powder.

[0038] Take 50mg of solid powder and put it in the sample tank, put the sample tank into the insulating tube, vacuumize the device, remove the air in the reaction system, and then pass the N 2 , and keep N 2 Environment, the two ends of the sample are respectively connected to the positive and negative poles of the constant current and constant voltage power supply, the sample is subjected to 1.5A constant current treatment for 5 hours, and then the sample is washed with deionized water and ethanol several times, and dried in a vacuum oven at 60°C for 24 hours .

[0039] Carry out oxygen reduction test to the sample that embodiment 1 obtains, simultaneously to blank sample, comprise pure BP, BP / HNO 3 Sample after 1.5A 5h...

Embodiment 2

[0044] Take 100mgBP, add 30ml 6M HNO 3 , ultrasonically dispersed for 1 h, then refluxed at 80°C for 6 h, rotary evaporated, and vacuum-dried to obtain BPox treated with nitric acid. Then mix 100mg BPox with 300ml 5wt.% FeCl 3 Aqueous solution (containing FeCl 3 15.26mg) were ultrasonically mixed and dried to obtain BPox-Fe.

[0045] BPox-Fe-Urea was obtained by grinding 100 mg BPox-Fe with 500 mg urea. Put the BPox-Fe-Urea powder compact into the sample tank, put the sample tank into the insulating tube, and pass through the N 2, the two ends of the sample are respectively connected to the positive and negative poles, and a voltage pulse (+10V 10s, -10V 10s, 20V 10s, -20V 10s) is applied to it. Then the samples were washed and dried to obtain BP-NFe.

[0046] By characterizing the chemical valence state of the catalyst of Example 2, it forms a Fe-N-C structure, such as figure 2 The XPS results are shown. By measuring the oxygen reduction performance of the catalyst u...

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Abstract

The invention provides a method for preparing a catalyst through solid-state electroreduction, and belongs to the field of catalyst synthesis. The method comprises the following steps: placing a sample in a sample tank, placing the sample tank in an insulating tube, respectively connecting positive and negative electrodes at two ends of the sample, contacting a thermocouple with one end of the sample, wherein the sample is an oxidation state metal or non-metal solid loaded on a conductive carrier, introducing a gas atmosphere into the insulating tube, starting a power supply device, electrifying the sample, and removing impurities from the electrified sample to obtain the catalyst. The method is simple and efficient, and the catalyst has catalytic activity.

Description

technical field [0001] The invention belongs to the field of catalyst synthesis, and in particular relates to a method for preparing a catalyst by solid-state electroreduction. Background technique [0002] Catalysts play a vital role in the field of energy catalysts, and different energy processes require different catalysts. For example, the fuel cell system that is expected to replace fossil energy currently requires the participation of platinum-based catalysts for the oxygen reduction reaction and the oxidation reaction of fuel (such as hydrogen). The core of the carbon dioxide electroreduction process, which is expected to solve carbon dioxide pollution and reuse, is also a catalyst. There are also important chemical processes such as nitrogen reduction, methanol oxidation, and petroleum cracking processes that require catalysts. Therefore, it is a problem that must be solved in the industry to be able to prepare uniform catalysts cheaply and in large quantities. At...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C25B1/00B01J35/02B01J35/00
CPCB01J27/24C25B1/00B01J35/00B01J35/30Y02E60/50
Inventor 徐维林宫雪阮明波宋平杨吉
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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