CN112919446B - Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method - Google Patents

Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method Download PDF

Info

Publication number
CN112919446B
CN112919446B CN202110091296.2A CN202110091296A CN112919446B CN 112919446 B CN112919446 B CN 112919446B CN 202110091296 A CN202110091296 A CN 202110091296A CN 112919446 B CN112919446 B CN 112919446B
Authority
CN
China
Prior art keywords
nitrogen
porous carbon
doped porous
electrode material
molybdenum disulfide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110091296.2A
Other languages
Chinese (zh)
Other versions
CN112919446A (en
Inventor
刘春晔
李晓梅
王喜恩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yinuoxin Electric Shenzhen Co ltd
Original Assignee
Yinuoxin Electric Shenzhen Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yinuoxin Electric Shenzhen Co ltd filed Critical Yinuoxin Electric Shenzhen Co ltd
Priority to CN202110091296.2A priority Critical patent/CN112919446B/en
Publication of CN112919446A publication Critical patent/CN112919446A/en
Application granted granted Critical
Publication of CN112919446B publication Critical patent/CN112919446B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to the technical field of lithium ion batteries, and discloses nitrogen-doped porous carbon loaded MoS 2 The method comprises the steps of carrying out cross-linking polymerization reaction on 3,3 '-diaminobenzidine and 1,2,4,5-tetra (4' -aldehyde phenyl) benzene to obtain a benzimidazolyl porous polymer, using an aromatic ring as a carbon source and an imidazole group as a nitrogen source, and carrying out activation and high-temperature carbonization on zinc chloride to obtain a nitrogen-doped porous carbon material, wherein the wettability of the electrode material is improved by nitrogen doping, the electrochemical activity of the porous carbon material is enhanced, in the process of synthesizing the molybdenum disulfide nanoflower sphere by a hydrothermal method, a molybdenum disulfide crystal nucleus is firstly generated, the crystal nucleus gradually grows to form a nanosheet and finally assembles a molybdenum disulfide nanoflower, the molybdenum disulfide nanoflower grows in situ in pores of the porous carbon material, the phenomenon of volume expansion of molybdenum disulfide is avoided, and therefore the cycling stability and the rate performance of the molybdenum disulfide-based electrode material are effectively improved.

Description

Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and its preparation method
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to nitrogen-doped porous carbon loaded MoS 2 An electrode material of nanometer flower and a preparation method.
Background
With the continuous acceleration of the modern construction process, the demand of human beings on fossil energy is higher and higher, however, the continuous use of fossil energy finally leads to resource exhaustion, and simultaneously, environmental problems such as greenhouse effect and air pollution are also caused, so that the social desire for novel clean and renewable energy is more and more urgent, although the solar energy, wind energy, tidal energy and other novel advantages of environmental protection and renewable energy are provided, the novel energy is difficult to exploit, the cost is relatively higher, and large-scale exploitation and use are difficult.
The nano molybdenum disulfide is one of transition metal sulfide semiconductors, has higher electrochemical theoretical capacity and higher safety, is considered to be a negative electrode material capable of replacing graphite to become a new generation of lithium ion battery, and researches show that when the nano molybdenum disulfide is taken as the negative electrode material of the lithium ion battery alone, the poorer conductivity of the nano molybdenum disulfide is difficult to meet the use and development requirements of the current lithium ion battery, and the layered stacking structure of the nano molybdenum disulfide can cause the Li to be frequently subjected to the layered stacking structure + The volume expansion occurs in the process of multiple embedding and releasing, so that the cycling stability and the rate capability of the lithium ion battery are greatly limited, and therefore, the nano molybdenum disulfide needs to be modified, on one hand, the specific surface area of the nano molybdenum disulfide is improved from the morphology of the nano molybdenum disulfide, the electrochemical active sites on the surface of the nano molybdenum disulfide can be increased, the conductivity of the nano molybdenum disulfide is enhanced, on the other hand, the nano molybdenum disulfide can be compounded with a porous carbon material with strong conductivity to form a load type lithium ion battery cathode material, the conductivity, the cycling stability, the rate capability and the like of the nano molybdenum disulfide can be improved, of course, along with the continuous and deep research, the conductivity of the traditional porous carbon material cannot meet the development requirement of the lithium ion battery industry, and therefore, the improvement of the conductivity of the porous carbon material also becomes a research hotspot in recent years.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a nitrogen-doped porous carbon loaded MoS 2 The electrode material of the nanoflower and the preparation method solve the problem that a single nano molybdenum disulfide negative electrode material is poor in conductivity and circulation stability.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: nitrogen-doped porous carbon loaded MoS 2 The nitrogen-doped porous carbon is loaded with MoS 2 The preparation method of the electrode material of the nanoflower comprises the following steps:
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-necked bottle, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, pre-reacting for 10-20h at 20-40 ℃, transferring into an oil bath pot, raising the temperature for cross-linking polymerization reaction, filtering a product, washing with acetone and trichloromethane, and drying to obtain a benzimidazolyl porous polymer;
(3) Adding deionized water, benzimidazolyl porous polymer and zinc chloride into a reactor, ultrasonically dispersing uniformly, evaporating a solvent, transferring into a tubular furnace, raising the temperature for carbonization, centrifuging, washing and drying a product after the reaction is finished, so as to obtain a nitrogen-doped porous carbon material;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material, sodium molybdate, thiourea and citric acid into a three-neck flask, ultrasonically stirring for 20-40min, transferring into a reaction kettle, placing into an oven for hydrothermal reaction, cooling a product, centrifuging, washing and drying to obtain nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Preferably, the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetrakis (4' -aldehydic phenyl) benzene in step (2) is 45-80.
Preferably, the temperature of the crosslinking polymerization reaction in the step (2) is 120-140 ℃, and the reaction is carried out for 60-90h under the condition of constant-temperature stirring in the nitrogen atmosphere.
Preferably, the mass ratio of the benzimidazolyl porous polymer to the zinc chloride in the step (3) is within a range from 100.
Preferably, the carbonization temperature in the step (3) is 800-900 ℃, and the carbonization is carried out for 2-6h in an argon atmosphere.
Preferably, the mass ratio of the nitrogen-doped porous carbon material, the sodium molybdate, the thiourea and the citric acid in the step (4) is (100).
Preferably, the temperature of the hydrothermal reaction in the step (4) is 170-190 ℃ and the time is 10-20h.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the nitrogen-doped porous carbon loaded MoS 2 The electrode material of the nanoflower, namely 3,3 '-amino in diaminobenzidine and 1,2,4,5-tetra (4' -aldehyde phenyl) benzene can be subjected to cross-linking polymerization reaction to obtain a benzimidazolyl porous polymer, an aromatic ring is used as a carbon source, imidazole groups are used as a nitrogen source, and a nitrogen-doped porous carbon material is finally obtained by activation and high-temperature carbonization of zinc chloride + The transmission channel greatly improves the specific surface area of the carbon material, exposes more electrochemical active reaction sites and adsorbs more Li + Increase the contact area between the composite cathode material and the electrolyte and accelerate Li + The transfer and the doping of nitrogen increase the wettability of the electrode material, improve the permeation rate of the electrolyte, simultaneously improve the conductivity of the porous carbon material to a certain extent, further enhance the electrochemical activity of the porous carbon material, and further effectively reduce the application difficulty of the porous carbon material in the field of lithium ion batteries.
The nitrogen-doped porous carbon loaded MoS 2 An electrode material of a nanometer flower, in the process of synthesizing a molybdenum disulfide nanometer flower ball by a hydrothermal method, sodium molybdate is used as a molybdenum source, thiourea is used as a sulfur source, a molybdenum disulfide crystal nucleus is generated firstly, hydroxyl and carboxyl in citric acid can be coordinated with molybdenum to form a stable chelate product, and then the hydrolysis and polymerization speed of molybdenum ions is controlled, so that the nanometer molybdenum disulfide crystal nucleus grows into a nanometer sheet gradually, and finally a molybdenum disulfide nanometer flower is assembledCan slow down the accumulation and agglomeration of the molybdenum disulfide nanoflowers to a certain extent, and can avoid the molybdenum disulfide from accumulating in Li + The problem of volume expansion in the continuous embedding and removing process is solved, so that the cycling stability and the rate capability of the nano molybdenum disulfide-based electrode material are effectively improved.
Drawings
FIG. 1 is a schematic reaction scheme of 3,3 '-diaminobenzidine and 1,2,4,5-tetrakis (4' -aldehydiphenyl) benzene.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: nitrogen-doped porous carbon loaded MoS 2 The preparation method of the electrode material of the nanoflower comprises the following steps:
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 45-80;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100-55-80 into a reactor, performing ultrasonic dispersion uniformly, evaporating a solvent, transferring into a tubular furnace, raising the temperature to 800-900 ℃, carbonizing for 2-6h in an argon atmosphere, centrifuging, washing and drying a product after the reaction is finished, thereby obtaining the nitrogen-doped porous carbon material;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100-130-150, namely, 135-160, sodium molybdate, thiourea and citric acid into a three-neck flask, ultrasonically stirring for 20-40min, transferring into a reaction kettle, placing in an oven, and stirring at 170-190Reacting at the temperature of 10-20h, cooling the product, centrifuging, washing and drying to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Example 1
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 45;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 to 135, sodium molybdate, thiourea and citric acid into a three-necked bottle, ultrasonically stirring for 20min, transferring into a reaction kettle, placing into an oven, reacting for 10h at 170 ℃, cooling, centrifuging, washing and drying a product to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Example 2
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with a molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 54;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100:62 into a reactor, performing ultrasonic dispersion uniformly, evaporating a solvent, transferring into a tubular furnace, raising the temperature to 820 ℃, carbonizing for 3 hours in an argon atmosphere, and centrifuging, washing and drying a product after the reaction is finished to obtain the nitrogen-doped porous carbon material;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 to 135, 142, sodium molybdate, thiourea and citric acid into a three-necked flask, ultrasonically stirring for 25min, transferring into a reaction kettle, placing into an oven, reacting for 12h at 175 ℃, cooling, centrifuging, washing and drying a product to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Example 3
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 62;
(3) Adding deionized water, benzimidazolyl porous polymer with the mass ratio of 100;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 to 222, sodium molybdate, thiourea and citric acid into a three-necked bottle, ultrasonically stirring for 30min, transferring into a reaction kettle, placing into an oven, reacting for 15h at 180 ℃, cooling, centrifuging, washing and drying a product to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Example 4
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with a molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 72, pre-reacting for 18h at 35 ℃, transferring into an oil bath, raising the temperature to 135 ℃, stirring and reacting for 80h at constant temperature in a nitrogen atmosphere, filtering a product, washing with acetone and trichloromethane, and drying to obtain the benzimidazolyl porous polymer;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 to 145,232, sodium molybdate, thiourea and citric acid into a three-necked bottle, ultrasonically stirring for 35min, transferring into a reaction kettle, placing in an oven, reacting for 18h at 185 ℃, cooling, centrifuging, washing and drying a product to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Example 5
(1) Using 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid as catalystReacting under the action to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 80;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100 to 80 into a reactor, performing ultrasonic dispersion uniformly, evaporating a solvent, transferring the solvent into a tubular furnace, raising the temperature to 900 ℃, carbonizing the solvent for 6 hours in an argon atmosphere, and centrifuging, washing and drying a product after the reaction is finished to obtain the nitrogen-doped porous carbon material;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 to 240, sodium molybdate, thiourea and citric acid into a three-necked bottle, ultrasonically stirring for 40min, transferring into a reaction kettle, placing into an oven, reacting for 20h at 190 ℃, cooling, centrifuging, washing and drying a product to obtain the nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower.
Comparative example 1
(1) 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid react under the action of a triphenyl phosphorus palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with a molecular formula of C 34 H 22 O 4 ；
(2) Adding a tetrahydrofuran solvent and 3,3 '-diaminobenzidine into a three-neck flask, mechanically stirring uniformly, then continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, wherein the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 36;
(3) Adding deionized water, a benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100 to 48 into a reactor, performing ultrasonic dispersion uniformly, evaporating a solvent, transferring the solvent into a tubular furnace, raising the temperature to 800 ℃, carbonizing the solvent for 1h in an argon atmosphere, and centrifuging, washing and drying a product after the reaction is finished to obtain the nitrogen-doped porous carbon material;
(4) Adding a deionized water solvent, a nitrogen-doped porous carbon material with a mass ratio of 100 2 Electrode material of nanometer flower.
MoS loaded with nitrogen-doped porous carbon 2 Mixing the electrode material of the nanoflower, acetylene black and polyvinylidene fluoride according to the proportion of 8 6 The mixed solution of ethylene carbonate, dimethyl carbonate and diethyl carbonate is used as electrolyte, sealed and stood, and assembled into a button cell, and the initial discharge capacity and the discharge capacity after 100 cycles of the composite electrode material are tested by using an IviumStat electrochemical workstation.
Figure BDA0002912661030000091
/>

Claims (4)

1. Nitrogen-doped porous carbon loaded MoS 2 The preparation method of the electrode material of the nanoflower comprises the steps of adding a nitrogen-doped porous carbon material, sodium molybdate, thiourea and citric acid into a deionized water solvent, ultrasonically stirring for 20-40min, transferring into a reaction kettle, placing in an oven for hydrothermal reaction, cooling a product, centrifuging, washing and drying to obtain the electrode material, and is characterized in that: the preparation method of the nitrogen-doped porous carbon comprises the following steps:
(1) From 1,2,4,5-tetrabromobenzene and 4-formylphenylboronic acid in trisReacting under the action of a phenylphosporium palladium catalyst to obtain 1,2,4,5-tetra (4' -aldehyde phenyl) benzene with the molecular formula of C 34 H 22 O 4 ；
(2) Adding 3,3 '-diaminobenzidine into tetrahydrofuran solvent, mechanically stirring uniformly, continuously adding 1,2,4,5-tetra (4' -aldehyde phenyl) benzene, pre-reacting at 20-40 ℃ for 10-20h, transferring into an oil bath pot, raising the temperature for cross-linking polymerization reaction, filtering, washing and drying the product to obtain the benzimidazolyl porous polymer;
(3) Adding benzimidazolyl porous polymer and zinc chloride in a mass ratio of 100-80 into deionized water, performing ultrasonic dispersion uniformly, evaporating a solvent, transferring the solvent into a tubular furnace for carbonization, and centrifuging, washing and drying a product after the reaction is finished to obtain the nitrogen-doped porous carbon material.
2. The nitrogen-doped porous carbon-loaded MoS according to claim 1 2 The electrode material of the nanometer flower is characterized in that: in the step (2), the mass ratio of 3,3 '-diaminobenzidine to 1,2,4,5-tetra (4' -aldehyde phenyl) benzene is 45-80.
3. The nitrogen-doped porous carbon-loaded MoS according to claim 1 2 The electrode material of the nanometer flower is characterized in that: the temperature of the cross-linking polymerization reaction in the step (2) is 120-140 ℃, and the reaction is carried out for 60-90h by stirring at constant temperature in the nitrogen atmosphere.
4. The nitrogen-doped porous carbon-loaded MoS according to claim 1 2 The electrode material of the nanometer flower is characterized in that: the carbonization temperature in the step (3) is 800-900 ℃, and the carbonization is carried out for 2-6h in an argon atmosphere.
CN202110091296.2A 2021-01-22 2021-01-22 Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method Active CN112919446B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110091296.2A CN112919446B (en) 2021-01-22 2021-01-22 Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110091296.2A CN112919446B (en) 2021-01-22 2021-01-22 Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method

Publications (2)

Publication Number Publication Date
CN112919446A CN112919446A (en) 2021-06-08
CN112919446B true CN112919446B (en) 2023-04-14

Family

ID=76165224

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110091296.2A Active CN112919446B (en) 2021-01-22 2021-01-22 Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method

Country Status (1)

Country Link
CN (1) CN112919446B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113451054B (en) * 2021-06-28 2022-05-17 鹏盛国能(深圳)新能源集团有限公司 Lithium ion capacitor battery and preparation method thereof
CN114156093B (en) * 2021-12-09 2023-06-20 桂林理工大学 N/O co-doped molybdenum sulfide@porous carbon composite electrode material and preparation method and application thereof
CN114481203A (en) * 2022-01-26 2022-05-13 西北工业大学 Foam nickel loaded nanometer flower-shaped nickel sulfide-molybdenum sulfide catalyst, preparation method and application
CN114538519A (en) * 2022-04-13 2022-05-27 景德镇陶瓷大学 Preparation method of phosphorus-doped amorphous carbon-coated 1T-phase molybdenum disulfide/carbon lithium ion battery composite anode material

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106158430A (en) * 2016-09-06 2016-11-23 上海电力学院 A kind of preparation method of the electrode material for ultracapacitor
CN111446436A (en) * 2020-04-26 2020-07-24 何家均 Carbon-coated lithium vanadium phosphate lithium ion battery positive electrode material and preparation method thereof
CN111681883A (en) * 2020-07-08 2020-09-18 刘栋 N, S co-doped porous carbon supercapacitor electrode material and preparation method thereof
CN111977691A (en) * 2020-08-28 2020-11-24 贵港益乐科技发展有限公司 Nitrogen-doped porous carbon-coated MoS2Lithium ion battery cathode material and preparation method thereof
CN112023950A (en) * 2020-09-10 2020-12-04 樊梦林 Ni-doped MoS2Hydrogen evolution electrocatalyst of nanoflower-porous graphene and preparation method thereof

Also Published As

Publication number Publication date
CN112919446A (en) 2021-06-08

Similar Documents

Publication Publication Date Title
CN112919446B (en) Nitrogen-doped porous carbon loaded MoS 2 Electrode material of nanometer flower and preparation method
CN110627033A (en) Nitrogen and sulfur co-doped multistage porous carbon composite material and preparation method and application thereof
CN112928255B (en) Lithium-sulfur battery composite positive electrode material and preparation method and application thereof
CN108598394B (en) Carbon-coated titanium manganese phosphate sodium microspheres and preparation method and application thereof
CN111235696B (en) Bismuth-phosphorus-sulfur/carbon composite nanofiber negative electrode material for sodium ion battery, preparation method of bismuth-phosphorus-sulfur/carbon composite nanofiber negative electrode material and sodium ion battery
CN110504438B (en) Preparation method and application of hetero-atom-doped carbon-coated two-dimensional metal selenide nanosheet composite material
CN107464938B (en) Molybdenum carbide/carbon composite material with core-shell structure, preparation method thereof and application thereof in lithium air battery
CN111370673A (en) Self-supporting lithium-sulfur battery cathode material with hierarchical structure and preparation method thereof
CN109786742B (en) Se-doped MXene battery negative electrode material and preparation method and application thereof
CN113930866A (en) Supercapacitor electrode material with capsule structure and preparation method and application thereof
CN112551574A (en) Sulfur-nitrogen doped porous carbon-coated Li4Ti5O12Lithium ion battery cathode material and preparation method thereof
CN111276694A (en) Preparation method of polyimide derived carbon/molybdenum disulfide negative electrode material and application of polyimide derived carbon/molybdenum disulfide negative electrode material in potassium ion battery
CN112670494B (en) Vanadate electrode material and preparation method and application thereof
CN113644269A (en) Preparation method of nitrogen-doped hard carbon material, product and application thereof
CN113241431A (en) Preparation method and application of ZnS nanoflower @ NC lithium ion battery anode material
CN110482523B (en) Nitrogen-doped hierarchical porous carbon material and application thereof in preparation of supercapacitor
CN110098398B (en) Preparation method and application of honeycomb-like sulfur-doped carbon material
CN110010893B (en) Sulfur-rich carbon material for sodium ion battery negative electrode and preparation method thereof
CN114751395B (en) Nitrogen-doped porous carbon sphere/S composite material, preparation method thereof and application thereof in lithium-sulfur battery
CN114944480B (en) Preparation method of honeycomb porous tin-carbon composite material
CN110137494B (en) Porous hard carbon microsphere material and preparation method thereof, button cell and preparation method thereof
CN110649250A (en) Preparation method of graphene/sulfur composite material and application of graphene/sulfur composite material in lithium-sulfur battery
CN114122371B (en) Preparation method of lithium ion Chi Fukong silicon-carbon anode material
CN114975920A (en) Electrode material with core-shell structure graphite alkyne coated metal antimony and preparation method and application thereof
CN110828796B (en) Yolk shell structure potassium ion battery negative electrode material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant