CN110155980A - A kind of preparation method of the three-dimensional porous carbon material of honeycomb - Google Patents
A kind of preparation method of the three-dimensional porous carbon material of honeycomb Download PDFInfo
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- CN110155980A CN110155980A CN201910420464.0A CN201910420464A CN110155980A CN 110155980 A CN110155980 A CN 110155980A CN 201910420464 A CN201910420464 A CN 201910420464A CN 110155980 A CN110155980 A CN 110155980A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/96—Carbon-based electrodes
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention provides a kind of preparation method of three-dimensional porous carbon material of honeycomb, this method is using glucose and dicyandiamide as carbon source and nitrogen source presoma, it is added and contains metal (copper, cobalt, nickel or iron etc.) salt saturated sodium chloride solution in, by freeze-drying, high temperature pyrolysis and subsequent washing or the method for pickling are prepared for the three-dimensional porous carbon material of honeycomb.Have benefited from glucose amino abundant on hydroxyl and dicyandiamide abundant and its between crosslinked action, improve pyrolysis carbon forming rate and N doping content；The three-dimensional porous carbon material of honeycomb prepared by this method has the characteristics that abundant pore structure, porosity height, large specific surface area and electrochemical performance, and in fuel cell, the fields such as metal-air battery and lithium battery have significant application value.
Description
Technical field
The invention belongs to porous carbon materials preparation technical fields, and in particular to a kind of three-dimensional porous carbon material of honeycomb it is green
Color high efficiency preparation method.The material can be applied in the new energy devices such as fuel cell, metal-air battery, lithium battery.
Background technique
Fuel cell, metal-air battery are as a kind of green, efficient energy conversion and storage element, in recent decades
In, studied mechanism is in depth studied as key object.Oxygen reduction reaction is electric to fuel cell, metal-air is determined
The performance in pond plays decisive role, and the blunt dynamics of oxygen reduction reaction causes its power density and energy efficiency to receive
It is serious to restrict.Meanwhile Current commercial catalyst is mostly Pt/C, expensive, stability and mithridatism are poor.Thus, it develops
A kind of cheap, excellent performance oxygen reduction catalyst is significantly.In addition, with lithium battery especially high-energy
The appearance of the solid state lithium battery and lithium-sulfur cell of density proposes urgently the three-dimensional carbon material of high conductivity, high porosity
Demand.
Three-dimensional porous carbon material is capable of providing big reaction circle because it is with biggish specific surface area and pore structure abundant
Face, microcell space and quick substance transmission channels, are widely used in fuel cell and metal-air battery catalyst, and
The research of electrode material of lithium battery (matrix).Wherein, the porous carbon materials of N doping because its with graphite mould nitrogen, pyridine type nitrogen,
Metal nitrogen etc. is conducive to improve the positive oxygen reduction reaction current potential of fuel cell, metal-air battery.Patent CN107834078A
By the SiO for being pyrolyzed exotic atom presoma and two kinds of sizes2Mixture, then HF etching wash away SiO2Template obtains hetero atom
Adulterate the classifying porous carbon material of honeycomb.SiO in this method2Template be although conducive to construct hierarchical porous structure, but cost it is expensive and
Acid etch step risk is high, and environmental pollution is big.Patent CN108767272A report a kind of nitrogen co-doped porous carbon materials of cobalt and
It is prepared and application, uses riboflavin for carbon source and nitrogen source, in conjunction with cobalt acetate and sodium chloride template, is carbonized by freeze-drying
The nitrogen co-doped porous carbon materials of cobalt are obtained.It uses sodium chloride as template, at low cost and easily remove and recycle,
But riboflavin (vitamin B2) price costly, limit its Commercial Prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the three-dimensional porous carbon material of honeycomb, this method is at low cost
Honest and clean, easy to operate, the characteristics of can be prepared on a large scale, gained carbon material, which has, enriches sensible three-dimensional porous structure.
The core technical features that the present invention is different from existing method are, using glucose and dicyandiamide as carbon source and nitrogen source,
It is added in the saturated sodium chloride solution containing metal (copper, cobalt, nickel or iron etc.) salt, is pyrolyzed by freeze-drying and subsequent high temperature
Method be prepared for the three-dimensional porous carbon material of honeycomb.Wherein dicyandiamide is as main nitrogen, but simple dicyandiamide had been pyrolyzed
Volatile decomposition, carbon forming rate are very low in journey.And the glucose being added serves not only as main carbon source, and passes through in pyrolytic process
The amino crosslinked action of polyhydroxy and dicyandiamide, improves the content of nitrogen in carbon forming rate and product.In addition, dicyandiamide and glucose
There is good water solubility, helps to be dispersed in saturated sodium chloride solution and uniform in freezing dry process later
It is covered in solid sodium chloride, to facilitate the formation of subsequent three-dimensional porous carbon wall.In brief, this project and by certain
The glucose of ratio and the synergistic effect of dicyandiamide had not only improved carbon material yield, but also have improved effective nitrogen content in catalyst, and
It ensure that relatively rich pore structure.
Specifically, the preparation method of the three-dimensional porous carbon material of honeycomb of the present invention is to be achieved through the following technical solutions
's.
(1) by glucose, dicyandiamide and metal salt (Iron trichloride hexahydrate or CoCL2 6H2O, six water nickel chlorides, copper chloride etc.
Metal salt) it is added in the NaCl solution of saturation with mass ratio for 25 ~ 500:25 ~ 500:1, it stirs evenly to form uniform solution.
It after being freezed solution with liquid nitrogen, is placed in freeze drier and is lyophilized, obtain sodium chloride template-organic precursor.
(2) organic precursor powder is placed in tube furnace and is heat-treated step by step, in the inert atmosphere of argon gas, with 3 ~ 30
DEG C/heating rate of min to 450 ~ 580 DEG C, 0.5 ~ 3 h of constant temperature.Again with the heating rate of 3 ~ 30 DEG C/min to 700 ~
1100 DEG C, 0.5 ~ 5 h of constant temperature.It is cooled to room temperature.
(3) again by porous carbon materials deionized water or 0.5 ~ 1.0 M H2SO4(HCl) 4 ~ 8 h are impregnated, decompression filters,
60 ~ 120 DEG C of 3 ~ 16 h of drying, obtain the three-dimensional porous carbon material of honeycomb.
Various specific chemical names in above-mentioned bracket are to provide specific example, and but not limited to this.
Good effect of the present invention is as follows: (1) using cheap glucose and dicyandiamide, reduce cost of material, glucose
It is provided with good water solubility with dicyandiamide, facilitates the content for reducing water, reduces the workload of later period freezing dry process；
Good water solubility facilitates organic matter precursor being uniformly distributed in sodium chloride template in freeze-drying simultaneously；(2) Portugal
The amino of polyhydroxy and dicyandiamide on grape sugar improves the dispersibility of metal ion, is conducive to metal in carbon material pyrolytic process
The performance of ionic catalysis effect and the distribution for improving active site in products therefrom；(3) pass through control organic precursor glucose
With the mass ratio of dicyandiamide, porous carbon materials yield is on the one hand improved；On the other hand the total of available nitrogen in catalyst is improved
Content.(3) have excellent three-D pore structure, high-specific surface area and chemical property using the carbon material of this method preparation.This
The three-dimensional porous carbon material of honeycomb of invention preparation can be used for fuel cell, metal-air battery, the fields such as lithium battery.
Detailed description of the invention
Fig. 1 is the scanning electron microscope for the three-dimensional porous carbon material of honeycomb (FeN-HPC-900) that in the present invention prepared by embodiment 1
Scheme (SEM).
Fig. 2 is the three-dimensional porous carbon material of honeycomb (FeN-HPC-900) and transmission electron microscope that in the present invention prepared by embodiment 1
Scheme (TEM).
Specific embodiment
Technical characteristic in order to better illustrate the present invention is illustrated below by specific embodiment
Embodiment 1
The NaCl solution of 50 mL saturation will be added in beaker, then is separately added into 2 g glucose, 2 g dicyandiamides and 40 mg
FeCl3·6H2O forms uniform orange solution after being sufficiently stirred.After the liquid nitrogen frozen solution, freeze-drying is placed it in
Diel in machine.Obtained faint yellow solid moves in porcelain boat, and tube furnace high-temperature heat treatment, first constant temperature are used in argon atmosphere
900 DEG C of 2 h of heat treatment, heating rate are 5 DEG C/min again after 550 DEG C of 1 h of heat treatment.After being cooled to room temperature, resulting black
Powder is in 0.5 M H2SO4Middle 6 h of pickling, decompression filters and deionized water is flushed to neutrality and obtains wet toner, then by wet toner
Dry one the whole night in 80 DEG C of vacuum oven, and it is 620 mg that weighing, which obtains quality, and gained sample is denoted as FeN-HPC-900.
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of FeN-HPC-900, and Fig. 2 is the transmission electron microscope picture (TEM) of FeN-HPC-900.Fig. 1 Fig. 2 card
Its honeycomb three-dimensional porous structure constructed by ultra-thin carbon wall is illustrated.
Embodiment 2
The NaCl solution of 50 mL saturation will be added in beaker, then is separately added into 2 g glucose, 2 g dicyandiamides and 40 mg
CoCl2·6H2O forms uniform lightpink solution after being sufficiently stirred.After the liquid nitrogen frozen solution, freeze-drying is placed it in
Diel in machine.Obtained solid moves in porcelain boat, and tube furnace high-temperature heat treatment, 550 DEG C of first constant temperature are used in argon atmosphere
900 DEG C of 2 h of heat treatment again are heat-treated after 1 h, and heating rate is 5 DEG C/min.After being cooled to room temperature, resulting black powder exists
0.5 M H2SO4Middle 6 h of pickling, decompression filters and deionized water is flushed to neutrality and obtains wet toner, then by wet toner 70
DEG C vacuum oven in dry one the whole night, it is 587 mg that weighing, which obtains quality, and gained sample is denoted as CoN-HPC-900.Through than
Surface area test show that the carbon material specific surface area reaches 824 m g-1, show that its surface nitrogen content reaches by XPS characterization
8.5%。
Embodiment 3
The NaCl solution of 500 mL saturation will be added in beaker, then is separately added into 20 g glucose, 20 g dicyandiamides and 500
mg FeCl3·6H2O forms uniform orange solution after being sufficiently stirred.After the liquid nitrogen frozen solution, freezing is placed it in
Diel in drying machine.Obtained faint yellow solid moves in porcelain boat, tube furnace high-temperature heat treatment is used in argon atmosphere, first
1000 DEG C of 2 h of heat treatment are warming up to after 550 DEG C of constant temperature 1 h of heat treatment again, heating rate is 5 DEG C/min.It is cooled to room temperature
Afterwards, resulting black powder impregnates 6 h in deionized water, and decompression filters, and deionized water rinses to obtain wet toner, then will be wet
The whole night, it is 6176 mg that weighing obtains quality to carbon dust for drying one in 80 DEG C of vacuum oven, and gained sample is denoted as FeN-
HPC-1000.It show that the carbon material specific surface area reaches 565 m g-1 through specific surface area test, its table is obtained by XPS characterization
Face nitrogen content is up to 9.3%.
Claims (5)
1. a kind of preparation method of the three-dimensional porous carbon material of honeycomb, it is characterised in that: using glucose and dicyandiamide as carbon source and
Nitrogen source is added in the saturated sodium chloride solution containing metal (copper, cobalt, nickel or iron etc.) salt, by being freeze-dried, high temperature pyrolysis,
And subsequent washing or the method for pickling are prepared for the three-dimensional porous carbon material of honeycomb.
2. a kind of preparation method of the three-dimensional porous carbon material of honeycomb as described in claim 1, wherein glucose, dicyandiamide and
Metal salt (Iron trichloride hexahydrate or CoCL2 6H2O, six water nickel chlorides, copper chloride) mass ratio is 25 ~ 500:25 ~ 500:1.
3. a kind of preparation method of the three-dimensional porous carbon material of honeycomb as described in claim 1, wherein high temperature pyrolysis process is adopted
It is the atmosphere of inert gases of nitrogen or argon gas.
4. a kind of preparation method of the three-dimensional porous carbon material of honeycomb as described in claim 1, wherein high temperature pyrolysis process is adopted
With two sections of temperature programmings, with the heating rate of 3 ~ 30 DEG C/min to 450 ~ 580 DEG C, 0.5 ~ 3 h of constant temperature, then with 3 ~ 30
DEG C/heating rate of min to 700 ~ 1100 DEG C, 0.5 ~ 5 h of constant temperature.
5. a kind of preparation method of the three-dimensional porous carbon material of honeycomb as described in claim 1, wherein abundant on glucose
On hydroxyl and dicyandiamide amino abundant and its between crosslinked action, improve pyrolysis carbon forming rate and N doping content.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911698A (en) * | 2019-12-02 | 2020-03-24 | 济南大学 | Oxygen reduction catalyst and preparation method thereof |
| CN111554945A (en) * | 2020-05-27 | 2020-08-18 | 青岛科技大学 | High-efficiency carbon-based electrocatalyst and preparation method and application thereof |
| CN112063366A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | NiCu composite nitrogen porous carbon material and preparation method and application thereof |
| CN113224321A (en) * | 2021-04-29 | 2021-08-06 | 陕西科技大学 | Vanadium-doped carbon-coated iron carbide multifunctional composite electrocatalyst and preparation method and application thereof |
| CN113363508A (en) * | 2021-02-02 | 2021-09-07 | 井冈山大学 | Electrocatalyst for fuel cell and preparation method thereof |
| CN113430540A (en) * | 2021-06-25 | 2021-09-24 | 北京航空航天大学 | Monoatomic catalyst, preparation method and application thereof |
| CN113943158A (en) * | 2021-12-20 | 2022-01-18 | 杭州德海艾科能源科技有限公司 | Preparation method of graphite felt for flow battery |
| CN115231620A (en) * | 2022-08-02 | 2022-10-25 | 西南交通大学 | Method for improving stability of iron-based three-dimensional porous structure and application |
| CN117486212A (en) * | 2023-11-14 | 2024-02-02 | 东营昆宇电源科技有限公司 | Honeycomb nitrogen-doped porous carbon material and application thereof in sodium-electricity negative electrode |
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| CN110911698B (en) * | 2019-12-02 | 2022-05-27 | 济南大学 | Oxygen reduction catalyst and preparation method thereof |
| CN111554945A (en) * | 2020-05-27 | 2020-08-18 | 青岛科技大学 | High-efficiency carbon-based electrocatalyst and preparation method and application thereof |
| CN112063366A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | NiCu composite nitrogen porous carbon material and preparation method and application thereof |
| CN113363508A (en) * | 2021-02-02 | 2021-09-07 | 井冈山大学 | Electrocatalyst for fuel cell and preparation method thereof |
| CN113224321A (en) * | 2021-04-29 | 2021-08-06 | 陕西科技大学 | Vanadium-doped carbon-coated iron carbide multifunctional composite electrocatalyst and preparation method and application thereof |
| CN113430540A (en) * | 2021-06-25 | 2021-09-24 | 北京航空航天大学 | Monoatomic catalyst, preparation method and application thereof |
| CN113943158A (en) * | 2021-12-20 | 2022-01-18 | 杭州德海艾科能源科技有限公司 | Preparation method of graphite felt for flow battery |
| CN115231620A (en) * | 2022-08-02 | 2022-10-25 | 西南交通大学 | Method for improving stability of iron-based three-dimensional porous structure and application |
| CN115231620B (en) * | 2022-08-02 | 2023-12-05 | 西南交通大学 | Method for improving stability of iron-based three-dimensional porous structure and application |
| CN117486212A (en) * | 2023-11-14 | 2024-02-02 | 东营昆宇电源科技有限公司 | Honeycomb nitrogen-doped porous carbon material and application thereof in sodium-electricity negative electrode |
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Application publication date: 20190823 |