CN109088076A - A kind of preparation method of non-precious metal catalyst - Google Patents

A kind of preparation method of non-precious metal catalyst Download PDF

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Publication number
CN109088076A
CN109088076A CN201810769513.7A CN201810769513A CN109088076A CN 109088076 A CN109088076 A CN 109088076A CN 201810769513 A CN201810769513 A CN 201810769513A CN 109088076 A CN109088076 A CN 109088076A
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China
Prior art keywords
precious metal
metal catalyst
preparation
temperature
filter cake
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Pending
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CN201810769513.7A
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Chinese (zh)
Inventor
杨祝红
朱永笑
吴友琴
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NANJING CARBONDE TECH Co Ltd
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NANJING CARBONDE TECH Co Ltd
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Priority to CN201810769513.7A priority Critical patent/CN109088076A/en
Publication of CN109088076A publication Critical patent/CN109088076A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90Selection of catalytic material
    • H01M4/9075Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to a kind of preparation methods of non-precious metal catalyst, by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stir 0.5-1h, precipitating reagent is put into aforesaid reaction vessel, stir 10-20min, mix precipitating reagent sufficiently uniformly with above-mentioned solution, it is quiet to 2-3h under room temperature, upper product is obtained into filter cake by filtering dehydration, through saturated common salt water washing 2-3 times, then filter cake is subjected to high temperature drying 2-3h by the electric heating case that temperature is 100-200 DEG C, a kind of preparation method of non-precious metal catalyst proposed by the present invention, preparation method is simple, with stronger operability, it is suitble to large-scale production, and raw material are commercially produced product, convenient for purchase, it is cheap, to reduce production cost, it is competing to improve market Power is striven, a kind of preparation method of non-precious metal catalyst proposed by the present invention improves the stability of active carbon, and then improve the catalytic effect of catalyst by carrying out the processing of high-temperature hydrogen atmosphere in active carbon.

Description

A kind of preparation method of non-precious metal catalyst
Technical field
The invention belongs to non-precious metal catalyst production technical field more particularly to a kind of preparations of non-precious metal catalyst Method.
Background technique
Proton Exchange Membrane Fuel Cells, methanol fuel cell, electrolytic water device and integral regeneratable fuel cell are not It directly converts the chemical energy in fuel to by electrochemical reaction mode by burning the power generator of electric energy, belongs to green The color energy;Compared with existing battery and rechargeable battery, there is high-energy, high power, pollution-free, high efficiency and miniaturization The characteristics of, following universal and market prospects are by expectation.However, the catalyst of above-mentioned fuel cell electrode, especially cathode Oxygen reduction catalyst, such as platinum based catalyst, because factors the become containment such as its is expensive, catalytic efficiency is low, stability is poor its One of commercialized main bottleneck.Therefore, developing and develop low noble metal catalyst and non-precious metal catalyst becomes the technology The direction of field development, especially non-precious metal catalyst are increasingly becoming hot spot concerned by people, are expected for the technical field The hope of quantum jump.In recent years, the research of carbon-based non-precious metal catalyst gradually obtains greater advance, predominantly N element and Various structure nano carbon (graphene, carbon nanotube, carbon fiber, carbon ball, the mesoporous carbons of M (metallic elements such as Fe, Co)-N doping And its complex carbon material).So far, the preparation of carbon-based non-precious metal catalyst focuses primarily upon template, high-temperature calcination, change Learn the operating process such as vapour deposition process, hydrothermal synthesis method complexity, the method for preparation condition harshness.
Existing non-precious metal catalyst generally uses active carbon as catalyst carrier, improves the stability of active carbon, Catalyst significant effect may make to improve.
Summary of the invention
The present invention is to solve well-known technique and provide a kind of preparation method of non-precious metal catalyst.
The present invention is adopted the technical scheme that solve well-known technique: a kind of Non-precious Metal Catalysts The preparation method of agent, comprising the following steps:
Step a: it by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stirs Mix 0.5-1h;
Step b: precipitating reagent is put into aforesaid reaction vessel, is stirred 10-20min, is mixed precipitating reagent sufficiently uniformly with step a solution It closes, it is quiet to 2-3h under room temperature;
Step c: then filter cake is passed through into temperature through saturated common salt water washing 2-3 times by filtering dehydration acquisition filter cake by upper product Degree carries out high temperature drying 2-3h for 100-200 DEG C of electric heating case;
Step e: the filter cake after above-mentioned drying is gone in the calcining furnace that temperature is 200-500 DEG C and calcines 3-5h;
Step f: calcined filter cake is ground by grinder, and powder crosses 40-60 mesh screen;
Step g: the powder after screening is formed by molding machine, obtains product, as non-precious metal catalyst.
Preferably, precipitating reagent is sodium hydroxide or sodium carbonate in the step b.
Preferably, the temperature of reaction kettle is 60-90 DEG C in the step a.
Preferably, the active carbon is to react 3-6h in the hydrogen tank that temperature is 200-300 DEG C.
Preferably, magnetic stirring apparatus is all made of in the step a, step b to be stirred.
The present invention has the advantage that as follows with good effect:
1. a kind of preparation method of non-precious metal catalyst proposed by the present invention, preparation method is simple, and having can operate more by force Property, it is suitble to large-scale production, and raw material are commercially produced product, it is cheap convenient for purchase, it is produced into reduce This, improves the market competitiveness.
2. the preparation method of a kind of non-precious metal catalyst proposed by the present invention, by carrying out high temperature hydrogen atmosphere in active carbon Processing is enclosed, improves the stability of active carbon, and then improve the catalytic effect of catalyst.
Specific embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following embodiment, it is described in detail It is as follows.
Embodiment 1
A kind of preparation method of non-precious metal catalyst, comprising the following steps:
Step a: it by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stirs Mix 0.5h;
Step b: precipitating reagent is put into aforesaid reaction vessel, is stirred 10min, is mixed precipitating reagent sufficiently uniformly with step a solution, It is quiet to 2h under room temperature;
Step c: then filter cake is passed through into temperature through saturated common salt water washing 2 times by filtering dehydration acquisition filter cake by upper product High temperature drying 2h is carried out for 100 DEG C of electric heating casees;
Step e: the filter cake after above-mentioned drying is gone in the calcining furnace that temperature is 200 DEG C and calcines 3h;
Step f: calcined filter cake is ground by grinder, and powder crosses 40 mesh screens;
Step g: the powder after screening is formed by molding machine, obtains product, as non-precious metal catalyst.
In the present embodiment, precipitating reagent is sodium hydroxide or sodium carbonate in the step b.
In the present embodiment, the temperature of reaction kettle is 60 DEG C in the step a.
In the present embodiment, the active carbon is to react 3h in the hydrogen tank that temperature is 200 DEG C.
In the present embodiment, magnetic stirring apparatus is all made of in the step a, step b and is stirred.
Embodiment 2
A kind of preparation method of non-precious metal catalyst, comprising the following steps:
Step a: it by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stirs Mix 0.7h;
Step b: precipitating reagent is put into aforesaid reaction vessel, is stirred 15min, is mixed precipitating reagent sufficiently uniformly with step a solution, It is quiet to 2.8h under room temperature;
Step c: then filter cake is passed through into temperature through saturated common salt water washing 2.5 times by filtering dehydration acquisition filter cake by upper product Degree carries out high temperature drying 2.5h for 150 DEG C of electric heating case;
Step e: the filter cake after above-mentioned drying is gone in the calcining furnace that temperature is 300 DEG C and calcines 4h;
Step f: calcined filter cake is ground by grinder, and powder crosses 50 mesh screens;
Step g: the powder after screening is formed by molding machine, obtains product, as non-precious metal catalyst.
In the present embodiment, precipitating reagent is sodium hydroxide or sodium carbonate in the step b.
In the present embodiment, the temperature of reaction kettle is 80 DEG C in the step a.
In the present embodiment, the active carbon is to react 5h in the hydrogen tank that temperature is 250 DEG C.
In the present embodiment, magnetic stirring apparatus is all made of in the step a, step b and is stirred.
Embodiment 3
A kind of preparation method of non-precious metal catalyst, comprising the following steps:
Step a: it by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stirs Mix 1h;
Step b: precipitating reagent is put into aforesaid reaction vessel, is stirred 20min, is mixed precipitating reagent sufficiently uniformly with step a solution, It is quiet to 3h under room temperature;
Step c: then filter cake is passed through into temperature through saturated common salt water washing 3 times by filtering dehydration acquisition filter cake by upper product High temperature drying 3h is carried out for 200 DEG C of electric heating casees;
Step e: the filter cake after above-mentioned drying is gone in the calcining furnace that temperature is 500 DEG C and calcines 5h;
Step f: calcined filter cake is ground by grinder, and powder crosses 60 mesh screens;
Step g: the powder after screening is formed by molding machine, obtains product, as non-precious metal catalyst.
In the present embodiment, precipitating reagent is sodium hydroxide or sodium carbonate in the step b.
In the present embodiment, the temperature of reaction kettle is 90 DEG C in the step a.
In the present embodiment, the active carbon is to react 6h in the hydrogen tank that temperature is 300 DEG C.
In the present embodiment, magnetic stirring apparatus is all made of in the step a, step b and is stirred.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form, Any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to In the range of technical solution of the present invention.

Claims (5)

1. a kind of preparation method of non-precious metal catalyst, which comprises the following steps:
Step a: it by metallic compound and active carbon investment equipped in the stainless steel electric heating reacting kettle of a certain amount of ethyl alcohol, persistently stirs Mix 0.5-1h;
Step b: precipitating reagent is put into aforesaid reaction vessel, is stirred 10-20min, is mixed precipitating reagent sufficiently uniformly with step a solution It closes, it is quiet to 2-3h under room temperature;
Step c: then filter cake is passed through into temperature through saturated common salt water washing 2-3 times by filtering dehydration acquisition filter cake by upper product Degree carries out high temperature drying 2-3h for 100-200 DEG C of electric heating case;
Step e: the filter cake after above-mentioned drying is gone in the calcining furnace that temperature is 200-500 DEG C and calcines 3-5h;
Step f: calcined filter cake is ground by grinder, and powder crosses 40-60 mesh screen;
Step g: the powder after screening is formed by molding machine, obtains product, as non-precious metal catalyst.
2. a kind of preparation method of non-precious metal catalyst according to claim 1, which is characterized in that in the step b Precipitating reagent is sodium hydroxide or sodium carbonate.
3. a kind of preparation method of non-precious metal catalyst according to claim 1, which is characterized in that in the step a The temperature of reaction kettle is 60-90 DEG C.
4. a kind of preparation method of non-precious metal catalyst according to claim 1, which is characterized in that the active carbon is 3-6h is reacted in the hydrogen tank that temperature is 200-300 DEG C.
5. a kind of preparation method of non-precious metal catalyst according to claim 1, which is characterized in that the step a, step Magnetic stirring apparatus is all made of in rapid b to be stirred.
CN201810769513.7A 2018-07-13 2018-07-13 A kind of preparation method of non-precious metal catalyst Pending CN109088076A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113481530A (en) * 2021-07-28 2021-10-08 澳门大学 Stainless steel-based catalyst and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102315459A (en) * 2011-09-05 2012-01-11 大连理工大学 Preparation method of porous fuel cell anode material NiCu/C
CN102658133A (en) * 2012-05-09 2012-09-12 杭州凯大催化金属材料有限公司 Method for preparing active carbon carrying precious metal catalyst
CN103285863A (en) * 2012-02-28 2013-09-11 比亚迪股份有限公司 Catalyst for preparing dichlorosilane, preparation method of catalyst and preparation method of dichlorosilane
US20150306574A1 (en) * 2014-04-28 2015-10-29 Celanese International Corporation Hydrogenation Catalysts Comprising a Mixed Oxide Comprising Nickel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102315459A (en) * 2011-09-05 2012-01-11 大连理工大学 Preparation method of porous fuel cell anode material NiCu/C
CN103285863A (en) * 2012-02-28 2013-09-11 比亚迪股份有限公司 Catalyst for preparing dichlorosilane, preparation method of catalyst and preparation method of dichlorosilane
CN102658133A (en) * 2012-05-09 2012-09-12 杭州凯大催化金属材料有限公司 Method for preparing active carbon carrying precious metal catalyst
US20150306574A1 (en) * 2014-04-28 2015-10-29 Celanese International Corporation Hydrogenation Catalysts Comprising a Mixed Oxide Comprising Nickel

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Title
姜瑞霞等: "高温氢气处理对活性炭及钯炭催化剂性能的影响", 《化学反应工程与工艺》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113481530A (en) * 2021-07-28 2021-10-08 澳门大学 Stainless steel-based catalyst and preparation method and application thereof

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