CN117401673A - Preparation method of nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material - Google Patents
Preparation method of nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material Download PDFInfo
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- CN117401673A CN117401673A CN202311647181.2A CN202311647181A CN117401673A CN 117401673 A CN117401673 A CN 117401673A CN 202311647181 A CN202311647181 A CN 202311647181A CN 117401673 A CN117401673 A CN 117401673A
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- humic acid
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- biochar
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000004021 humic acid Substances 0.000 title claims abstract description 83
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002791 soaking Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 239000008236 heating water Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 230000003111 delayed effect Effects 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 230000002459 sustained effect Effects 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 45
- 125000000524 functional group Chemical group 0.000 description 9
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000019635 sulfation Effects 0.000 description 3
- 238000005670 sulfation reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001934 delay Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000006182 cathode active material Substances 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- MINVSWONZWKMDC-UHFFFAOYSA-L mercuriooxysulfonyloxymercury Chemical compound [Hg+].[Hg+].[O-]S([O-])(=O)=O MINVSWONZWKMDC-UHFFFAOYSA-L 0.000 description 1
- 229910000371 mercury(I) sulfate Inorganic materials 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000010278 pulse charging Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- 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
- H01M10/06—Lead-acid accumulators
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material, and belongs to the technical field of biological humic acid. The method comprises the following steps: s1, soaking humic acid raw materials in dilute sulfuric acid solution, stirring and soaking for 35-45min, filtering, washing and drying; s2, soaking the humic acid obtained after drying in KOH/EDTA mixtureThe solution is subjected to heat preservation under the water bath heating condition, and then filtered, collected and filtered residues are dried and calcined under the protection of nitrogen to obtain humic acid activated carbon; s3, under the condition of water bath heating, adding H into the humic acid activated carbon 2 O 2 And obtaining the humic acid oxygen-enriched active carbon by the solution. When the humic acid biochar material prepared by the invention is applied to the negative electrode of the lead-carbon battery, the shrinkage of the structure of the active substance of the negative electrode can be delayed, the sustained discharge is facilitated, and the internal resistance of the battery is reduced.
Description
Technical Field
The invention belongs to the technical field of biological humic acid, and particularly relates to a preparation method of a nitrogen-doped humic acid biological carbon lead-carbon battery negative electrode composite material.
Background
For centuries, lead storage batteries have been developed in which corrosion of the positive grid and sulfation of the negative plate have been major causes of affecting their life. Lead sulfate accumulated on the negative plate can obviously reduce the effective surface area of active substances, so that the occurrence of chemical reaction is limited to a certain extent, and in order to improve sulfation of the surface of a lead electrode, a bipolar grid design and pulse charging method are adopted. Since these two methods have high demands on battery design and assembly and charging equipment, the negative plate performance is improved and enhanced mainly by adding an expanding agent.
The organic expansion agent has two main roles in the negative plate: firstly, the surface area shrinkage of the cathode active material during the circulation process is prevented, the materials can be adsorbed on the surface of an electrode, and the system energy is reduced by reducing the surface tension; secondly, the passivation preventing function is that PbSO formed in the discharge process of the cathode is influenced 4 And (5) crystallizing. Humic acid has various forms, structures and elements, can form a humic acid derived carbon material, is used as a cheap and abundant carbon source, is applied to a potential and successful raw material, and is used for preparing an organic expanding agent material for a lead-carbon battery cathode. The main functional groups of humic acid are methoxy, phenolic hydroxyl and carboxyl, and the active functional groups have stronger exchange, complexing, flocculation and adsorption effects, however, the humic acid has poor conductivity and can influence the battery resistance and further influence the battery performance.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material, which aims to solve the problems of overlarge battery resistance and poor battery performance caused by poor conductivity of a humic acid organic expanding agent in the background art.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material comprises the following steps:
s1, soaking a humic acid raw material in a dilute sulfuric acid solution, stirring and soaking at a rotating speed of 200-300rpm for 35-45min, removing metal ion impurities in the humic acid raw material, washing and drying;
s2, soaking the humic acid obtained after drying in a KOH/EDTA mixed solution, preserving heat for 70-100min at 70-100 ℃ in a water bath, filtering, collecting filter residues, drying, placing in a tubular furnace, calcining under the protection of nitrogen, and carrying out pore-forming modification on the humic acid to obtain humic acid activated carbon;
s3, under the condition of water bath heating, adding H into the humic acid activated carbon 2 O 2 And (3) modifying the oxygen-enriched functional groups on the surface of the humic acid activated carbon.
Further, the concentration of the dilute sulfuric acid solution in S1 is 1mol/L.
Further, the solid-to-liquid ratio of the humic acid raw material to the dilute sulfuric acid solution in the step S1 is 1g:10-30mL.
Further, the mass ratio of KOH to EDTA (ethylenediamine tetraacetic acid) in the KOH/EDTA mixed solution in the step S2 is 0.5-2:1.
Further, the mass fraction of the KOH/EDTA mixed solution in the S2 is 1-4%.
Further, the solid-to-liquid ratio of humic acid to KOH/EDTA mixed solution in the step S2 is 1g:20-30mL.
Further, the calcination temperature in the step S2 is 200-400 ℃.
Further, H in S3 2 O 2 The concentration of the solution is 0.5-2.0 mol/L.
Further, humic acid activated carbon and H in the S3 2 O 2 The solid-to-liquid ratio of the solution is 1g:5-20mL.
Further, the water bath heating temperature in the step S3 is 65-75 ℃.
The invention has the beneficial effects that:
the invention provides a preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite materialThe preparation method. The method mainly comprises the steps of soaking humic acid in dilute sulfuric acid to remove metal ion impurities in the humic acid, then dissolving and soaking the humic acid in a mixed solution of potassium hydroxide and EDTA, calcining the humic acid at a high temperature under the protection of nitrogen in a tubular furnace, carrying out porous modification on the humic acid, then carrying out water bath heating treatment in a hydrogen peroxide solution, and carrying out modification on the surface of the humic acid activated carbon by adding oxygen-enriched functional groups. Can be beneficial to the adsorption capacity of humic acid and reduce compact PbSO 4 The formation of the active material delays the structure shrinkage of the anode active material, is favorable for continuous discharge, and simultaneously, part of humic acid is carbonized after being calcined at high temperature to generate a porous structure, and simultaneously, part of the original chemical structure is reserved, so that the conductivity of the lead plaster is favorable, and the internal resistance of the battery is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material comprises the following steps:
s1.80mL of dilute sulfuric acid solution with the concentration of 1mol/L is used for soaking 4g of humic acid raw material, stirring and soaking is carried out for 40min at the rotating speed of 250rpm, metal ion impurities in the humic acid raw material are removed, and washing and drying are carried out;
s2, soaking 2g of humic acid in 40mL of KOH/EDTA mixed solution with the mass fraction of 2.5%, wherein the weight ratio of KOH to EDTA in the KOH/EDTA mixed solution is 1:1, preserving the temperature for 85min under the water bath condition of 85 ℃, filtering, collecting filter residues, drying, placing in a tubular furnace, calcining at 300 ℃ under the protection of nitrogen, and carrying out pore-forming modification on the humic acid to obtain humic acid active carbon;
s3.70 ℃ under the water bath heating condition, 12mL of H with the concentration of 1.2 mol/L is added into 1g of humic acid active carbon 2 O 2 SolutionAnd (3) modifying the oxygen-enriched functional groups on the surface of the humic acid activated carbon.
Example 2
A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material comprises the following steps:
s1.40mL of dilute sulfuric acid solution with the concentration of 1mol/L is used for soaking 4g of humic acid raw material, stirring and soaking is carried out for 42min at the rotating speed of 220rpm, metal ion impurities in the humic acid raw material are removed, and washing and drying are carried out;
s2, soaking 2g of humic acid in 60mL of KOH/EDTA mixed solution with the mass fraction of 1.2%, wherein the weight ratio of KOH to EDTA in the KOH/EDTA mixed solution is 1.8:1, preserving the temperature for 100min under the water bath condition of 70 ℃, filtering, collecting filter residues, drying, placing in a tubular furnace, calcining at 220 ℃ under the protection of nitrogen, and performing pore-forming modification on the humic acid to obtain humic acid activated carbon;
s3.65 ℃ under the water bath heating condition, 6mL of H with the concentration of 1.8 mol/L is added into 1g of humic acid active carbon 2 O 2 And (3) modifying the oxygen-enriched functional groups on the surface of the humic acid activated carbon.
Example 3
A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material comprises the following steps:
s1.110mL of dilute sulfuric acid solution with the concentration of 1mol/L is used for soaking 4g of humic acid raw material, stirring and soaking is carried out for 35min at the rotating speed of 300rpm, metal ion impurities in the humic acid raw material are removed, and washing and drying are carried out;
s2, soaking 2g of humic acid in 24mL of KOH/EDTA mixed solution with the mass fraction of 0.8%, wherein the weight ratio of KOH to EDTA in the KOH/EDTA mixed solution is 0.6:1, preserving the temperature for 75min under the water bath condition of 100 ℃, filtering, collecting filter residues, drying, placing in a tubular furnace, calcining at 400 ℃ under the protection of nitrogen, and performing pore-forming modification on the humic acid to obtain humic acid activated carbon;
s3.75 ℃ under the water bath heating condition, 18mL of H with the concentration of 0.6 mol/L is added into 1g of humic acid active carbon 2 O 2 And (3) modifying the oxygen-enriched functional groups on the surface of the humic acid activated carbon.
Example 4
Performance testing
0.02g of the nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material prepared in examples 1-3 and 0.02g of humic acid are respectively dissolved in 100ml of 0.1 ml/L NaOH solution and then added into the solution with the density of 1.34g/cm 3 The system using sulfuric acid solution as electrolyte, lead plate as working electrode, mercurous sulfate as reference electrode, platinum electrode as counter electrode, test each group of electrochemical impedance value, only add the same amount of NaOH solution as blank electrolyte as control, fit each group of impedance value by using Zs impwi nnew software, as shown in table 1:
TABLE 1
As shown in Table 1, as humic acid is subjected to pore-forming modification and oxygen-enriched functional groups are introduced to the surface of the humic acid, the functional groups and the porous holes have the capacity of synergistically adsorbing lead ions, so that the composite material effectively delays sulfation and reduces internal resistance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized by comprising the following steps of:
s1, soaking a humic acid raw material in a dilute sulfuric acid solution, stirring and soaking at a rotating speed of 200-300rpm for 35-45min, and filtering, washing and drying;
s2, soaking the humic acid obtained after drying in a KOH/EDTA mixed solution, preserving heat for 70-100min under the condition of water bath heating, filtering, collecting filter residues, drying, and calcining under the protection of nitrogen to obtain humic acid activated carbon;
s3, under the condition of water bath heating, adding H into the humic acid activated carbon 2 O 2 And obtaining the humic acid oxygen-enriched active carbon by the solution.
2. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the concentration of a dilute sulfuric acid solution in S1 is 1mol/L.
3. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the solid-liquid ratio of humic acid raw materials to dilute sulfuric acid solution in S1 is 1g:10-30mL.
4. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the mass ratio of KOH to EDTA in a KOH/EDTA mixed solution in S2 is 0.5-2:1.
5. The preparation method of the nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the mass fraction of KOH/EDTA mixed solution in S2 is 1% -4%.
6. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the solid-to-liquid ratio of humic acid to KOH/EDTA mixed solution in S2 is 1g:20-30mL.
7. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized in that the calcination temperature in S2 is 200-400 ℃.
8. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized by comprising the following steps of 2 O 2 The concentration of the solution is 0.5-2.0 mol/L.
9. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized by comprising the steps of 2 O 2 The solid-to-liquid ratio of the solution is 1g:5-20mL.
10. A preparation method of a nitrogen-doped humic acid biochar lead-carbon battery negative electrode composite material is characterized by comprising the following steps of (1) heating water bath in S2 to 70-100 ℃; and the heating temperature of the water bath in the step S3 is 65-75 ℃.
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