CN111092195A - Ag-TiO2-MnO2Method for preparing composite material - Google Patents

Ag-TiO2-MnO2Method for preparing composite material Download PDF

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Publication number
CN111092195A
CN111092195A CN201811232721.XA CN201811232721A CN111092195A CN 111092195 A CN111092195 A CN 111092195A CN 201811232721 A CN201811232721 A CN 201811232721A CN 111092195 A CN111092195 A CN 111092195A
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Prior art keywords
parts
stirring
deionized water
solution
manganese dioxide
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CN201811232721.XA
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Chinese (zh)
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不公告发明人
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Haimen Yuanmei Art Pattern Design Co ltd
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Haimen Yuanmei Art Pattern Design Co ltd
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Priority to CN201811232721.XA priority Critical patent/CN111092195A/en
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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
    • H01M4/362—Composites
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses Ag-TiO2‑MnO2The preparation method of the composite material comprises the following steps: dissolving SDS in deionized water, stirring uniformly, adding the mixture into a manganese sulfate solution dropwise, and stirring; preparing an ammonium persulfate solution by using deionized water, stirring, slowly adding a manganese sulfate mixed solution into the ammonium persulfate solution, reacting for 7-9 hours, washing a black precipitate, centrifuging, drying, grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample in an air atmosphere to obtain manganese dioxide; adding manganese dioxide into deionized water, performing ultrasonic treatment, dissolving silver nitrate and titanium dioxide in alcohol, performing ultrasonic treatment, adding into manganese dioxide solution, and stirring until the solvent is evaporatedAnd drying, grinding the obtained powder sample, calcining in an air atmosphere, and cooling to obtain the catalyst. The Ag-TiO prepared by the method2‑MnO2The composite material has large specific discharge capacity under high multiplying power, small load transfer impedance and excellent conductivity.

Description

Ag-TiO2-MnO2Method for preparing composite material
Technical Field
The invention relates to Ag-TiO2-MnO2A method for preparing a composite material.
Background
After decades of development, manganese dioxide has been widely used in the fields of batteries, capacitors, catalysis, etc. Lithium/manganese dioxide batteries have become the least expensive and the best safe battery of the lithium primary battery family. The advantages of manganese dioxide as a battery cathode material are: 1) high specific energy (230 Wh Kg)-1) (ii) a 2) The working voltage is high (2.8V-3.2V); 3) the application temperature range is wide (-40 ℃ to 60 ℃); 4) long storage life (more than 10 years of storage at room temperature); 5) low cost, high safety, but low manganese dioxideThe development of the conductive layer is severely restricted by the conductivity and poor structural stability. Researchers mainly carry out modification research on manganese dioxide by methods of preparing a nano material with a large specific surface area, coating a conductive polymer, compounding with a transition metal element and the like. Among them, transition metal modification is one of the simplest and most effective methods. The research on the composite modification of the transition metal element has important significance on the lithium manganese dioxide primary battery.
Disclosure of Invention
The invention aims to provide Ag-TiO2-MnO2A method for preparing a composite material.
The invention is realized by the following technical scheme:
Ag-TiO2-MnO2The preparation method of the composite material comprises the following steps: dissolving 15-25 parts of SDS (sodium dodecyl sulfate) in 70-80 parts of deionized water, stirring uniformly, dropwise adding into 90-100 parts of manganese sulfate solution with the concentration of 0.1mol/L, and magnetically stirring for 40-50 min; preparing 90-100 parts of ammonium persulfate solution with the concentration of 0.1mol/L by using deionized water, strongly stirring for 35-45min at 65-75 ℃, then slowly adding a mixed solution of manganese sulfate into the ammonium persulfate solution, reacting for 7-9h at 65-75 ℃, sequentially washing black precipitates for 4-6 times by using deionized water and ethanol, centrifuging, drying a filter at 65-75 ℃, then grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample for 11-13h at 370 ℃ in an air atmosphere of 360-; adding 10-20 parts of manganese dioxide into 65-75 parts of deionized water, performing ultrasonic dispersion for 35-45min, dissolving 7-9 parts of silver nitrate as a modifier and 9-15 parts of titanium dioxide into 35-45 parts of alcohol, performing ultrasonic dispersion for 15-25min, then adding the mixture into a manganese dioxide solution, stirring for 5-6h at 34-38 ℃ until the solvent is evaporated to dryness, grinding the obtained powder sample, calcining for 11-13h at 370 ℃ in an air atmosphere, and cooling to obtain the manganese dioxide powder; the raw materials are in parts by weight.
Preferably, in the preparation method, magnetic stirring is carried out for 45 min.
Preferably, in the preparation method, strong stirring is carried out for 40min at 70 ℃.
Preferably, in the preparation method, the reaction is carried out for 8 hours at 70 ℃.
Preferably, in the preparation method, the powder sample is calcined for 12 hours at 365 ℃ in an air atmosphere.
Preferably, in the preparation method, the solvent is stirred for 5.5h at 36 ℃ until the solvent is evaporated to dryness.
The invention has the technical effects that:
the method is simple, convenient, rapid and easy to operate, and the prepared Ag-TiO2-MnO2The composite material has large discharge specific capacity under high multiplying power, small load transfer impedance and excellent conductivity, and can be prepared on a large scale.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
Ag-TiO2-MnO2The preparation method of the composite material comprises the following steps: dissolving 20 parts of SDS (sodium dodecyl sulfate) in 75 parts of deionized water, stirring uniformly, dropwise adding into 95 parts of manganese sulfate solution with the concentration of 0.1mol/L, and magnetically stirring for 45 min; preparing 95 parts of ammonium persulfate solution with the concentration of 0.1mol/L by using deionized water, strongly stirring for 40min at 70 ℃, slowly adding a manganese sulfate mixed solution into the ammonium persulfate solution, reacting for 8h at 70 ℃, sequentially washing black precipitates for 5 times by using the deionized water and ethanol, centrifuging, drying a filter at 70 ℃, grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample for 12h at 365 ℃ in an air atmosphere to obtain manganese dioxide; adding 15 parts of manganese dioxide into 70 parts of deionized water, performing ultrasonic dispersion for 40min, dissolving 8 parts of silver nitrate as a modifier and 12 parts of titanium dioxide into 40 parts of alcohol, performing ultrasonic dispersion for 20min, then adding the mixture into a manganese dioxide solution, stirring for 5.5h at 36 ℃ until the solvent is evaporated to dryness, grinding the obtained powder sample, calcining for 12h at 365 ℃ in an air atmosphere, and cooling to obtain the nano-silver-doped manganese dioxide powder; the raw materials are in parts by weight.
Example 2
Ag-TiO2-MnO2The preparation method of the composite material comprises the following steps: dissolving 15 parts of SDS (sodium dodecyl sulfate) in 70 parts of deionized water, stirring uniformly, dropwise adding the mixture into 90 parts of manganese sulfate solution with the concentration of 0.1mol/L, and stirring by magnetic force40 min; preparing 90 parts of ammonium persulfate solution with the concentration of 0.1mol/L by using deionized water, strongly stirring for 35min at 65 ℃, slowly adding a manganese sulfate mixed solution into the ammonium persulfate solution, reacting for 7h at 65 ℃, sequentially washing black precipitates for 4 times by using the deionized water and ethanol, centrifuging, drying a filter at 65 ℃, grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample for 11h at 360 ℃ in an air atmosphere to obtain manganese dioxide; adding 10 parts of manganese dioxide into 65 parts of deionized water, performing ultrasonic dispersion for 35min, dissolving 7 parts of modifying agent silver nitrate and 9 parts of titanium dioxide into 35 parts of alcohol, performing ultrasonic dispersion for 15min, then adding the mixture into a manganese dioxide solution, stirring for 5h at 34 ℃ until the solvent is evaporated to dryness, grinding the obtained powder sample, calcining for 11h at 360 ℃ in an air atmosphere, and cooling to obtain the nano-silver-doped manganese dioxide; the raw materials are in parts by weight.
Example 3
Ag-TiO2-MnO2The preparation method of the composite material comprises the following steps: dissolving 25 parts of SDS (sodium dodecyl sulfate) in 80 parts of deionized water, stirring uniformly, dropwise adding the mixture into 100 parts of manganese sulfate solution with the concentration of 0.1mol/L, and magnetically stirring for 50 min; preparing 100 parts of ammonium persulfate solution with the concentration of 0.1mol/L by using deionized water, strongly stirring for 45min at 75 ℃, slowly adding a manganese sulfate mixed solution into the ammonium persulfate solution, reacting for 9h at 75 ℃, sequentially washing black precipitates for 6 times by using the deionized water and ethanol, centrifuging, drying a filter at 75 ℃, grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample for 13h at 370 ℃ in an air atmosphere to obtain manganese dioxide; adding 20 parts of manganese dioxide into 75 parts of deionized water, performing ultrasonic dispersion for 45min, dissolving 9 parts of modifier silver nitrate and 15 parts of titanium dioxide into 45 parts of alcohol, performing ultrasonic dispersion for 25min, then adding the mixture into a manganese dioxide solution, stirring the mixture at 38 ℃ for 6h until the solvent is evaporated to dryness, grinding the obtained powder sample, calcining the powder sample at 370 ℃ for 13h in an air atmosphere, and cooling the powder sample to obtain the nano-silver/nano-silver; the raw materials are in parts by weight.
The method is simple, convenient, rapid and easy to operate, and the prepared Ag-TiO2-MnO2The composite material has large specific discharge capacity under high rate, small load transfer impedance and excellent conductivityAnd (3) the preparation method can be used for large-scale preparation.

Claims (6)

1. Ag-TiO2-MnO2The preparation method of the composite material is characterized by comprising the following steps: dissolving 15-25 parts of SDS (sodium dodecyl sulfate) in 70-80 parts of deionized water, stirring uniformly, dropwise adding into 90-100 parts of manganese sulfate solution with the concentration of 0.1mol/L, and magnetically stirring for 40-50 min; preparing 90-100 parts of ammonium persulfate solution with the concentration of 0.1mol/L by using deionized water, strongly stirring for 35-45min at 65-75 ℃, then slowly adding a mixed solution of manganese sulfate into the ammonium persulfate solution, reacting for 7-9h at 65-75 ℃, sequentially washing black precipitates for 4-6 times by using deionized water and ethanol, centrifuging, drying a filter at 65-75 ℃, then grinding by using an agate mortar to obtain a brownish black sample, and calcining the powder sample for 11-13h at 370 ℃ in an air atmosphere of 360-; adding 10-20 parts of manganese dioxide into 65-75 parts of deionized water, performing ultrasonic dispersion for 35-45min, dissolving 7-9 parts of silver nitrate as a modifier and 9-15 parts of titanium dioxide into 35-45 parts of alcohol, performing ultrasonic dispersion for 15-25min, then adding the mixture into a manganese dioxide solution, stirring for 5-6h at 34-38 ℃ until the solvent is evaporated to dryness, grinding the obtained powder sample, calcining for 11-13h at 370 ℃ in an air atmosphere, and cooling to obtain the manganese dioxide powder; the raw materials are in parts by weight.
2. The method of claim 1, wherein: stirring for 45min by magnetic force.
3. The method of claim 1, wherein: stirring vigorously at 70 deg.C for 40 min.
4. The method of claim 1, wherein: the reaction was carried out at 70 ℃ for 8 h.
5. The method of claim 1, wherein: the powder samples were calcined in an air atmosphere at 365 ℃ for 12 h.
6. The method of claim 1, wherein: stirring was carried out at 36 ℃ for 5.5h until the solvent was evaporated to dryness.
CN201811232721.XA 2018-10-23 2018-10-23 Ag-TiO2-MnO2Method for preparing composite material Pending CN111092195A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114497504A (en) * 2022-01-28 2022-05-13 惠州亿纬锂能股份有限公司 Positive electrode active material of lithium primary battery and preparation method and application thereof
EP4299773A1 (en) 2022-06-30 2024-01-03 Fortum Oyj Method for processing manganese containing material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114497504A (en) * 2022-01-28 2022-05-13 惠州亿纬锂能股份有限公司 Positive electrode active material of lithium primary battery and preparation method and application thereof
CN114497504B (en) * 2022-01-28 2023-11-03 惠州亿纬锂能股份有限公司 Lithium primary battery positive electrode active material, and preparation method and application thereof
EP4299773A1 (en) 2022-06-30 2024-01-03 Fortum Oyj Method for processing manganese containing material
WO2024003452A1 (en) 2022-06-30 2024-01-04 Fortum Oyj Method for processing manganese containing material

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