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A kind of preparation method of nitrogen-boron doped carbon-based catalyst

A carbon-based catalyst, nitrogen-boron technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., to achieve good industrial application prospects, aerobic reduction activity and stability, and simple process effects

Active Publication Date: 2018-05-11
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the preparation of nitrogen-boron-doped carbon-based catalysts using nitrogen-boron co-carburized materials as oxygen reduction catalysts for fuel cells.

Method used

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  • A kind of preparation method of nitrogen-boron doped carbon-based catalyst
  • A kind of preparation method of nitrogen-boron doped carbon-based catalyst
  • A kind of preparation method of nitrogen-boron doped carbon-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Weigh 20g of conductive carbon black (EC300J) and soak it in dilute sulfuric acid with a concentration of 0.5 mol / L for 24 hours, then filter it with suction, wash it with distilled water for 3 times, and dry it in vacuum at 60°C for 1 hour to obtain the pretreatment carbon materials;

[0033] (2) Weigh 10g of conductive carbon black (EC300J) pretreated in step (1), and polyaniline (nitrogen donor), sodium fluoroborate and fluoboric acid (boron donor) and thiourea (activator) by mass The percentages are 60%, 18%, 10%, and 12%, respectively, mixed in a mortar and mechanically ball-milled for 60 minutes, wherein the mass ratio of the boron-donating agent sodium fluoroborate and fluoroboric acid is 1:1;

[0034] (3) Move the mixture of mechanical ball milling in step (2) into a ceramic boat, and then put it into a quartz tube resistance furnace. Under the protection of an inert gas (nitrogen), first raise the temperature to 300°C at a rate of 15°C / min. Keep it for 10 mi...

Embodiment 2

[0039] (1) Weigh 20g of conductive carbon black (Vulcan XC-7) and soak it in dilute sulfuric acid with a concentration of 0.25 mol / L for 6 hours, then filter it with suction, wash it with twice distilled water 4 times, and dry it in vacuum at 40°C for 2 hour, obtain the pretreated carbon material;

[0040] (2) Weigh 10g of conductive carbon black (Vulcan XC-7) pretreated in step (1), mix with o-phenanthrene (nitrogen donor), sodium fluoroborate and fluoroboric acid (boron donor) and hydrogen fluoride Sodium bicarbonate (activator) was 50%, 30%, 6%, and 14% by mass percentage, mixed in a mortar and mechanically ball-milled for 30 minutes, and the mass ratio of boron-donating agent sodium fluoroborate to fluoroboric acid was 1:1 ;

[0041] (3) Move the mixture of mechanical ball milling in step (2) into a ceramic boat, and then put it into a quartz tube resistance furnace. Under the protection of an inert gas (nitrogen), first raise the temperature to 300°C at a rate of 10°C / mi...

Embodiment 3

[0045] (1) Weigh 20g of conductive carbon black (BP2000) and soak it in dilute sulfuric acid with a concentration of 1.5 mol / L for 48 hours, then filter it with suction, wash it with twice distilled water for 5 times, and dry it in vacuum at 100°C for 4 hours to obtain Pretreated carbon materials;

[0046] (2) Weigh 10g of conductive carbon black (BP2000) pretreated in step (1), and melamine (nitrogen donor), sodium fluoroborate and fluoroboric acid (boron donor) and urea (activator) respectively by mass percentage 74%, 10%, 6%, 10%, mixed in a mortar and mechanically milled for 120 minutes, wherein the mass ratio of boron-donating agent sodium fluoroborate to fluoroboric acid is 1:1;

[0047] (3) Move the mixture of mechanical ball milling in step (2) into a ceramic boat, and then put it into a quartz tube resistance furnace. Under the protection of an inert gas (argon), first raise the temperature to 300°C at a rate of 20°C / min. , kept for 60 minutes, and then raised to 110...

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Abstract

The invention discloses a preparation method for a nitrogen-boron-doped carbon-based catalyst, which belongs to the technical field of catalytic materials. The method comprises the following steps: pretreating a carbon material; then mixing the pretreated carbon material with a nitrogen supplying agent, a boron supplying agent and an activator and carrying out mechanical ball milling; then subjecting a mixture obtained after ball milling to nitrogen-boron co-penetration heat treatment of the carbon material at a temperature of 500 to 1100 DEG C under the protection of inert gas for 1 to 3 h; and finally carrying out pickling so as to prepare the nitrogen-boron-doped carbon-based catalyst. The nitrogen-boron-doped carbon-based catalyst prepared by using the method can be used as a negative electrode oxygen reducing catalyst for a fuel cell; the preparation method has the advantages of low prices of raw materials, simple process, low requirements on equipment and applicability to large-scale production of the catalyst; and the catalyst shows good oxygen reduction activity and stability under both acidic and alkaline conditions.

Description

technical field [0001] The invention relates to a preparation method of a nitrogen-boron-doped carbon-based catalyst, which belongs to the technical field of electrocatalysts. Background technique [0002] As a new type of clean energy device, fuel cells have the advantages of high efficiency, easy start-up, zero pollution, and high capacity. major. However, the cathode and anode of proton exchange membrane fuel cells mainly use platinum (Pt)-based catalysts. Due to the slow oxygen reduction kinetic activity of the cathode, the cathode needs more platinum to promote the oxygen reduction reaction, and the cathode occupies 90% of the platinum catalyst in the fuel cell. % platinum catalyst. Because platinum catalysts account for a large proportion of fuel cell costs, platinum resources are scarce and expensive, resulting in high fuel cell prices. So far, the high cost of fuel cell platinum catalysts is still one of the main bottlenecks restricting its large-scale commerciali...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 杨喜昆余江英王光华江克柱陈琳燕
Owner KUNMING UNIV OF SCI & TECH
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