CN107469824A - A kind of preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating - Google Patents
A kind of preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating Download PDFInfo
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- CN107469824A CN107469824A CN201710886238.2A CN201710886238A CN107469824A CN 107469824 A CN107469824 A CN 107469824A CN 201710886238 A CN201710886238 A CN 201710886238A CN 107469824 A CN107469824 A CN 107469824A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B01J37/088—Decomposition of a metal salt
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- G—PHYSICS
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- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of preparation method of the hollow crystal nickel oxide ethanol oxidation catalyst of carbon coating, specific preparation process are as follows:1. a certain proportion of glucose and nickel acetate being dissolved in deionized water solution being made, calcining in tube furnace is placed in after drying and obtains nickel carbon solid;2. the hollow crystal nickel oxide catalyst of carbon coating is obtained after nickel carbon solid is calcined in air atmosphere.The hollow crystal nickel oxide catalyst of the carbon coating prepared in the present invention has good electro catalytic activity in alkalescence condition to ethanol, it is simply cheap to prepare raw material used, preparation process is simple, is expected to apply in the field such as ethanol sensor and Direct Ethanol Fuel Cell.
Description
Technical field
The invention belongs to ethanol oxidation catalyst technical field, can apply to alcohol fuel cell and ethanol sensor etc.
In field, and in particular to the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating a kind of.
Background technology
Because the chemical energy of ethanol can directly be converted available electric energy and its reaction product Nonpoisonous, non-environmental-pollution, institute
All paid close attention to always by scientific circles with the research of oxidation of ethanol.At present, ethanol can be applied to fuel cell, sensor and combustion
Expect cell type ethanol sensor.Noble metal because its remarkable electrocatalysis characteristic is widely used in oxidation of ethanol always, but
It is that noble metal has the shortcomings that a lot, such as expensive and easy poisoning etc..In order to solve this problem, many researchs are directed to using
Metal oxide replaces noble metal, and substantial amounts of result of study shows that some metal oxides can improve the reaction of oxidation of ethanol
Activity and stability.Wherein, nickel oxide shows the superior function to oxidation of ethanol, for example is presented in Ethanol Oxidation
High current density, the reactivity worth of quick reaction rate and stabilizer pole.
The crystal structure of catalyst all has a great impact to its catalytic performance and reaction mechanism, and different crystal structure is urged
The reaction mechanism of agent has difference, or even can be completely opposite.For nickel oxide, many researchs, which are directed to preparing, has crystalline substance
The nickel oxide of body structure, the presence of crystal structure can be greatly enhanced the catalytic performance of catalyst.The oxygen prepared in the present invention
Changing Raney nickel has obvious crystal structure, and the nickel oxide of this crystal structure has very superior catalytic performance to ethanol.
On the other hand, the specific surface area of catalyst can be increased by carrying out carbon coating to catalyst, effectively improve catalyst
Electric conductivity and chemical stability.The nontoxic and cheap glucose that selects in the present invention is carbon source, after high-temperature calcination,
Catalyst particle is wrapped in carbon substrate by intact.The structure of carbon coating greatly increases leading for crystal nickel oxide catalyst
The electrical and catalytic performance to oxidation of ethanol.
After nickel carbon catalyst in the present invention is calcined in atmosphere, because Kinkendal Effect is generated with hollow knot
The crystal nickel oxide of structure, this hollow structure shorten the transmitting range of particle and ethanol so as to improve catalyst to ethanol
Catalytic performance.
The hollow crystal nickel oxide catalyst of the carbon coating prepared in the present invention exists to the superior function of oxidation of ethanol, reason
In carbon coating structure, the hollow structure of particle and the synergy of crystal nickel oxide.
The content of the invention
The purpose of the present invention is a kind of system of the ethanol oxidation catalyst for the hollow crystal nickel oxide for being to provide carbon coating
Preparation Method.
The present invention realizes according to the following steps:
Nickel carbon solid will be obtained after the mixed aqueous solution drying and calcining of a certain proportion of glucose and nickel acetate;By nickel carbon
Solid is placed in Muffle furnace and calcined, and the hollow crystal nickel oxide catalyst of carbon coating is obtained after washing and drying.
The catalysis oxidation that the hollow crystal nickel oxide catalyst of prepared carbon coating has brilliance to ethanol in the present invention is lived
Property, this mainly has benefited from the carbon coating structure of prepared catalyst, and the collaboration of the hollow structure and crystal nickel oxide of particle is made
With.The generation of crystal nickel oxide causes catalyst that the catalytic performance of ethanol is significantly increased.The hollow crystal oxygen of carbon coating
Changing Raney nickel has good stability, is expected to be applied in the fields such as ethanol sensor.
Brief description of the drawings
Fig. 1 is the hollow crystal nickel oxide catalyst HR-TEM figures of the carbon coating prepared in embodiment 1;
Fig. 2 is the XRD of the hollow crystal nickel oxide catalyst of the carbon coating prepared in embodiment 1;
Fig. 3 is the hollow crystal nickel oxide catalyst of carbon coating and following for nickel carbon solid catalyst prepared in embodiment 1
Ring volt-ampere curve.
Specific implementation method
The preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating, specific preparation process are as follows:
(1) preparation of nickel carbon solid:
2g glucose and 1.2g nickel acetates are weighed, thing is then mixed and is dissolved in 50mL deionized waters, after stirring 2h
It is placed in air dry oven and 10h is dried at 100 DEG C.The solid being completely dried is placed in tube furnace, in a nitrogen atmosphere, with 3
DEG C/min heating rate calcines in 800 DEG C and is incubated 2h, that is, obtain nickel carbon solid.
(2) preparation of crystal nickel oxide catalyst:
Weigh 1g nickel carbon solids to be placed in crucible, then crucible is placed in Muffle furnace and calcines 2h at 350 DEG C, rise
Warm speed is 1 DEG C/min.Obtained black powder obtains crystal after deionized water is cleaned three times after drying 12h at 40 DEG C
Nickel oxide catalyst.
The result of study of the hollow crystal nickel oxide catalyst of carbon coating:
(1) test result analysis of appearance structure:
Fig. 1 is the HR-TEM photos of prepared catalyst, and the particle of catalyst is wrapped in hollow structure and well
Overlay in amorphous carbon, this special structure greatly increases the electric conductivity of catalyst and increases catalyst and ethanol
Contact area.
(2) test result analysis of crystalline structure:
It can be obtained by Fig. 2, prepared catalyst has apparent lattice structure, and its main lattice structure is face-centered cubic
The nickel oxide of structure.
(3) electrocatalysis characteristic test result analysis:
Fig. 3 shows that hollow the crystal nickel oxide catalyst and nickel carbon solid catalyst of carbon coating are molten to 0.5M ethanol
The cyclic voltammetry figure of liquid catalysis oxidation.Wherein, the electrolyte of this system is 0.5M sodium hydroxide solution.Can from Fig. 3
To find out, the hollow crystal nickel oxide catalyst of carbon coating shows high oxidate current to ethanol, and this explanation is originally
The hollow crystal nickel oxide catalyst of the carbon coating prepared in invention has good electrocatalysis to ethanol.In addition, through peroxide
After change processing, the oxidation of ethanol current density of the hollow crystal nickel oxide catalyst of carbon coating is relative to nickel carbon solid catalyst
Oxidation of ethanol current density be significantly improved, this illustrates that catalysis can be significantly increased in the generation of hollow crystal nickel oxide
Catalytic activity of the agent to ethanol.
The ethanol oxidation catalyst of the hollow crystal nickel oxide of the carbon coating proposed in the present invention is prepared simply and to environment
Pollution-free, catalyst shows outstanding catalytic activity to ethanol, and the research to Catalytic oxidation of ethanol field provides new think of
Road.
Claims (7)
- A kind of 1. preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating, it is characterised in that:(1) nickel carbon solid will be obtained after the mixed aqueous solution drying and calcining of a certain proportion of glucose and nickel acetate;(2) nickel carbon solid is placed in Muffle furnace and calcined, the hollow crystal nickel oxide catalysis of carbon coating is obtained after washing and drying Agent.
- 2. the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating as claimed in claim 1, it is special Levy and be (1) described glucose, the mass ratio of nickel acetate and water is 1: 0.45-0.75: 25.
- 3. the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating as claimed in claim 1, it is special Sign is that the drying temperature described in (1) is 90-100 DEG C, drying time 10-15h.
- 4. the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating as claimed in claim 1, it is special Sign is that the calcination condition described in (1) is as follows:800-1000 is heated to 3-5 DEG C/min heating rate in the case where nitrogen protects gas DEG C and keep 2-5h.
- 5. the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating as claimed in claim 1, it is special Sign is that the calcination condition of the nickel carbon solid described in (2) is as follows:Heated under air conditionses with 1-2 DEG C/min heating rate To 250-400 DEG C and keep 2-5h.
- 6. the preparation method of the ethanol oxidation catalyst of the hollow crystal nickel oxide of carbon coating as claimed in claim 1, it is special Sign is that the washing conditions described in (2) are deionized water, and drying temperature is 40 DEG C.
- 7. the ethanol oxidation catalyst of the hollow crystal nickel oxide of the carbon coating as prepared by claim 1~6, there is uniqueness Structure, and have superior catalytic performance and stability to oxidation of ethanol.
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110193367A (en) * | 2019-05-31 | 2019-09-03 | 东北大学秦皇岛分校 | A kind of new structural iron carbon composite and preparation method thereof |
CN110732327A (en) * | 2019-10-25 | 2020-01-31 | 中南民族大学 | carbon material-coated nickel catalyst and method for preparing primary amine compound by using same |
CN111384365A (en) * | 2018-12-27 | 2020-07-07 | 南京理工大学 | Preparation method of carbon-coated multilayer NiO hollow sphere composite material |
WO2021078113A1 (en) * | 2019-10-21 | 2021-04-29 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nanocomposite, preparation method therefor and application thereof |
CN112762469A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Method for catalytic combustion of volatile organic compounds |
CN112755995A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nanocomposite and preparation method and application thereof |
CN112755780A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Method for catalytic decomposition of nitrous oxide |
CN112755993A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nano composite material and preparation method and application thereof |
CN112755994A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nano composite material and preparation method and application thereof |
CN113751042A (en) * | 2020-06-05 | 2021-12-07 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nano composite material and preparation method and application thereof |
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Cited By (16)
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CN111384365A (en) * | 2018-12-27 | 2020-07-07 | 南京理工大学 | Preparation method of carbon-coated multilayer NiO hollow sphere composite material |
CN110193367A (en) * | 2019-05-31 | 2019-09-03 | 东北大学秦皇岛分校 | A kind of new structural iron carbon composite and preparation method thereof |
CN112755994A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nano composite material and preparation method and application thereof |
CN112755993B (en) * | 2019-10-21 | 2022-07-15 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nanocomposite and preparation method and application thereof |
CN112762469A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Method for catalytic combustion of volatile organic compounds |
CN112755995A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nanocomposite and preparation method and application thereof |
CN112755780A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Method for catalytic decomposition of nitrous oxide |
CN112755993A (en) * | 2019-10-21 | 2021-05-07 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nano composite material and preparation method and application thereof |
EP4049750A4 (en) * | 2019-10-21 | 2023-11-29 | China Petroleum & Chemical Corporation | Carbon-coated nickel oxide nanocomposite material, preparation method therefor and use thereof |
CN112755780B (en) * | 2019-10-21 | 2022-11-15 | 中国石油化工股份有限公司 | Method for catalytic decomposition of nitrous oxide |
CN112762469B (en) * | 2019-10-21 | 2022-04-12 | 中国石油化工股份有限公司 | Method for catalytic combustion of volatile organic compounds |
WO2021078113A1 (en) * | 2019-10-21 | 2021-04-29 | 中国石油化工股份有限公司 | Carbon-coated nickel-aluminum nanocomposite, preparation method therefor and application thereof |
CN110732327A (en) * | 2019-10-25 | 2020-01-31 | 中南民族大学 | carbon material-coated nickel catalyst and method for preparing primary amine compound by using same |
CN113751042B (en) * | 2020-06-05 | 2022-07-15 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nano composite material and preparation method and application thereof |
CN113751042A (en) * | 2020-06-05 | 2021-12-07 | 中国石油化工股份有限公司 | Carbon-coated nickel oxide nano composite material and preparation method and application thereof |
CN115770466A (en) * | 2021-09-06 | 2023-03-10 | 中国石油化工股份有限公司 | Flue gas denitration method |
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