CN109585826A - The nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding - Google Patents

The nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding Download PDF

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Publication number
CN109585826A
CN109585826A CN201811431969.9A CN201811431969A CN109585826A CN 109585826 A CN109585826 A CN 109585826A CN 201811431969 A CN201811431969 A CN 201811431969A CN 109585826 A CN109585826 A CN 109585826A
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Prior art keywords
barium sulfate
sulfate particle
lignin sulfonate
sodium lignin
nanoscale barium
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CN201811431969.9A
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Inventor
刘巍
魏晗
楼志强
杨宝峰
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Shuangdeng Group Co Ltd
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Shuangdeng Group Co Ltd
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Priority to CN201811431969.9A priority Critical patent/CN109585826A/en
Publication of CN109585826A publication Critical patent/CN109585826A/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
    • H01M4/366—Composites as layered products
    • 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
    • H01M10/12—Construction or manufacture
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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

Abstract

The invention discloses a kind of nanoscale barium sulfate particle synthetic methods of sodium lignin sulfonate cladding, it is characterised in that: this method first uses 10~50mL0.5mol/LNaOH and 10~100mL0.25mol/LNa2S2O8It is mixed to get NaOH—Na2S2O8Synthetic solvent is rich in nanoscale barium sulfate particle in this solution.Then with 10~90 mLBaCl2It is added to 10~50min of stirring in 10~50mLLS solution, obtains LS-BaCl2Synthetic solvent, above two synthetic solvent is stirred under the conditions of 50~120 DEG C to 10~50min mixing together again, sediment is taken out when being cooled to room temperature, sediment prepares the nanoscale barium sulfate particle material of sodium lignin sulfonate cladding after conventional centrifugal filtration, washing, drying process.

Description

The nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding
Technical field
The invention belongs to chemosynthesis technical fields, and in particular to a kind of nanoscale barium sulfate of sodium lignin sulfonate cladding Particle synthetic method.
Background technique
Barium sulfate is a kind of important industrial chemicals, and the cathode additive agent that can be used as lead-acid accumulator uses.It is stored in plumbic acid In the discharge process of battery, barium sulfate provides site for the nucleation of sulfuric acid leading crystal, and the crystalline size of lead sulfate is effectively reduced, and protects Card sulfuric acid leading crystal is evenly distributed in porous negative electrode active material, is not generated the passivation lead sulfate of bulky grain, is played and prolong The effect of long lead-acid battery service life cycle.
Common barium sulfate is prepared by liquid-phase precipitation method, i.e., by the solution containing sulfate ion and barium ions or barium ions The solution of complex compound mixes, and obtains the precipitating of lead sulfate.The barium sulfate of smaller particle in order to obtain, researcher is by using each The size and shape of kind means control barium sulfate particle, such as use relevant surfaces activating agent.But it is prepared according to the above method What is obtained is micron order barium sulfate particles, and because its scale is still larger, and the surfactant added may be to subsequent production Performances of the lead-acid battery has an impact, and needs to apply relative complex cleaning process removal associated additives.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of nano barium sulfate synthesis sides of sodium lignin sulfonate cladding Method, the simple synthetic method are implemented to be easy, and obtained product does not need to have saved technique using additional complicated cleaning process Cost.The nano barium sulfate of the sodium lignin sulfonate cladding of preparation has preferably dispersibility, can guarantee that sulfuric acid leading crystal is equal It is distributed in porous negative electrode active material evenly, facilitates the service life cycle for extending lead-acid accumulator.
The present invention is achieved through the following technical solutions technical goal.
The nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding, the improvement is that: this method is first used 10~50mL0.5mol/LNaOH and 10~100mL0.25mol/LNa2S2O8It is mixed to get NaOH—Na2S2O8Synthetic solvent, this Nanoscale barium sulfate particle is rich in solution.Then with 10~90 mLBaCl2Be added in 10~50mLLS solution stirring 10~ 50min obtains LS-BaCl2Synthetic solvent, then by above two synthetic solvent together under the conditions of 50~120 DEG C stirring 10~ 50min mixing, takes out sediment, sediment is prepared after conventional centrifugal filtration, washing, drying process when being cooled to room temperature The nanoscale barium sulfate particle material of sodium lignin sulfonate cladding.
As the scheme of further improvement, the nanoscale barium sulfate particle diameter is 20~50nm.
As the scheme of further improvement, the LS-BaCl2LS/B in solutionaCl2Molar ratio is between 0.1~1.
As the scheme of further improvement, the nanoscale barium sulfate particle preferably under the conditions of 60~100 DEG C, is incited somebody to action NaOH—Na2S2O8LS-B is added dropwise in synthetic solventaCl2In synthetic solvent, 2~5h is persistently stirred.
As the scheme of further improvement, the speed control of the stirring is in 100~500r/min.
As the scheme of further improvement, it is 50~90 DEG C that the drying process, which applies temperature, and drying time is 12~48h.
Compared with prior art, the present invention having the positive effect that.
1, simple synthetic method of the present invention, obtained nanoscale barium sulfate particle do not need additionally to apply complicated scavenger Skill, therefore saved process costs.
2, the nanoscale barium sulfate particle of sodium lignin sulfonate cladding has dispersibility well, particularly suitable as plumbic acid The additive of battery terminal negative uses, and helps to improve the service life cycle of lead-acid accumulator.
Detailed description of the invention
Fig. 1 is the nanoscale barium sulfate particle XRD spectra of sodium lignin sulfonate cladding obtained.
Fig. 2 is the nanoscale barium sulfate particle SEM spectrogram of sodium lignin sulfonate cladding obtained.
Specific embodiment:
The present invention is further illustrated below by embodiment.
Embodiment 1
By 15 mL, 0.25 mol/LNa2S2O850 min are continuously stirred under the conditions of 60 DEG C with 30 mL, 0.5 mol/LNaOH, It is then cooled to room temperature to obtain NaOH-Na2S2O8Solution.In addition by 40 mL BaCl2It is added in 25 mL LS solution and stirs 50 Min obtains LS-BaCl2Solution, wherein LS/BaCl2Molar ratio is 0.2.Finally by NaOH-under the conditions of 60 DEG C, 500 r/min Na2S2O8LS-BaCl is added dropwise in solution2In solution, persistently stir 4 h.The substance of synthesis passes through centrifugal filtration, washing, 50 Dry 18 h obtain sample under the conditions of °C.The XRD spectra of the nano barium sulfate particle samples of the sodium lignin sulfonate package of preparation It is as depicted in figs. 1 and 2 with SEM spectrogram.
Embodiment 2
By 10 mL, 0.25 mol/LNa2S2O870 min are continuously stirred under the conditions of 50 DEG C with 30 mL, 0.5 mol/LNaOH, It is then cooled to room temperature to obtain NaOH-Na2S2O8Solution.In addition by 30 mL BaCl2It is added in 15 mL LS solution and stirs 40 Min obtains LS-BaCl2Solution, wherein LS/BaCl2Molar ratio is 0.4.Finally by NaOH-under the conditions of 50 DEG C, 400 r/min Na2S2O8LS-BaCl is added dropwise in solution2In solution, persistently stir 3 h.The substance of synthesis passes through centrifugal filtration, washing, 60 Dry 24 h obtain sample under the conditions of °C.The XRD spectra of the nano barium sulfate particle samples of the sodium lignin sulfonate package of preparation It is similar to Fig. 1 and Fig. 2 with SEM spectrogram.
Embodiment 3
By 20 mL, 0.25 mol/LNa2S2O840 min are continuously stirred under the conditions of 60 DEG C with 20 mL, 0.5 mol/LNaOH, It is then cooled to room temperature to obtain NaOH-Na2S2O8Solution.In addition by 30 mL BaCl2It is added in 20 mL LS solution and stirs 40 Min obtains LS-BaCl2Solution, wherein LS/BaCl2Molar ratio is 0.3.Finally by NaOH-under the conditions of 50 DEG C, 500 r/min Na2S2O8LS-BaCl is added dropwise in solution2In solution, persistently stir 5 h.The substance of synthesis passes through centrifugal filtration, washing, 50 Dry 24 h obtain sample under the conditions of °C.The XRD spectra of the nano barium sulfate particle samples of the sodium lignin sulfonate package of preparation It is similar to Fig. 1 and Fig. 2 with SEM spectrogram.
Embodiment 4
By 15 mL, 0.25 mol/LNa2S2O830 min are continuously stirred under the conditions of 70 DEG C with 20 mL, 0.5 mol/LNaOH, It is then cooled to room temperature to obtain NaOH-Na2S2O8Solution.In addition by 50 mL BaCl2It is added in 40 mL LS solution and stirs 40 Min obtains LS-BaCl2Solution, wherein LS/BaCl2Molar ratio is 0.5.Finally by NaOH-under the conditions of 50 DEG C, 400 r/min Na2S2O8LS-BaCl is added dropwise in solution2In solution, persistently stir 4 h.The substance of synthesis passes through centrifugal filtration, washing, 60 Dry 48 h obtain sample under the conditions of °C.The XRD spectra of the nano barium sulfate particle samples of the sodium lignin sulfonate package of preparation It is similar to Fig. 1 and Fig. 2 with SEM spectrogram.
Embodiment 5
By 30 mL, 0.25 mol/LNa2S2O860 min are continuously stirred under the conditions of 70 DEG C with 30 mL, 0.5 mol/LNaOH, It is then cooled to room temperature to obtain NaOH-Na2S2O8Solution.In addition by 50 mL BaCl2It is added in 25 mL LS solution and stirs 50 Min obtains LS-BaCl2Solution, wherein LS/BaCl2Molar ratio is 0.6.Finally by NaOH-under the conditions of 50 DEG C, 600 r/min Na2S2O8LS-BaCl is added dropwise in solution2In solution, persistently stir 5 h.The substance of synthesis passes through centrifugal filtration, washing, 70 Dry 48 h obtain sample under the conditions of °C.The XRD spectra of the nano barium sulfate particle samples of the sodium lignin sulfonate package of preparation It is similar to Fig. 1 and Fig. 2 with SEM spectrogram.
Sodium lignin sulfonate is a kind of natural polymers, belongs to anionic surfactant, in aqueous solution With very strong dispersibility, it can be used for the synthesis of aided nano material.In addition, sodium lignin sulfonate is in negative electrode active material Lead surface forms a layers of polymer electrolyte, prevents from generating passivation sulfuric acid lead layer on cathode, this effect helps to extend plumbic acid electricity The service life cycle in pond.
The nanoscale barium sulfate of sodium lignin sulfonate cladding not only still with the property of common barium sulfate, also has common sulphur The unexistent physics of sour barium and chemical characteristic, such as good dispersion performance, compatibility.The particle that the synthetic method obtains is not required to Apply additional complicated cleaning process, to save process costs.The nano barium sulfate of lignin sulfonic acid barium cladding has Preferably dispersibility guarantees that sulfuric acid leading crystal is evenly distributed in porous negative electrode active material, which similarly helps to prolong The service life cycle of long lead-acid accumulator.

Claims (6)

1. a kind of nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding, it is characterised in that: this method first uses 10 ~50mL0.5mol/LNaOH and 10~100mL0.25mol/LNa2S2O8It is mixed to get NaOH—Na2S2O8Synthetic solvent, this is molten Nanoscale barium sulfate particle is rich in liquid；Then with 10~90 mLBaCl2Be added in 10~50mLLS solution stirring 10~ 50min obtains LS-BaCl2Synthetic solvent, then by above two synthetic solvent together under the conditions of 50~120 DEG C stirring 10~ 50min mixing, takes out sediment, sediment is prepared after conventional centrifugal filtration, washing, drying process when being cooled to room temperature The nanoscale barium sulfate particle material of sodium lignin sulfonate cladding.
2. the nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding according to claim 1, feature exist In: the nanoscale barium sulfate particle diameter is 20~50nm.
3. the nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding according to claim 1, feature exist In: the LS-BaCl2LS/B in solutionaCl2Molar ratio is between 0.1~1.
4. the nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding according to claim 1, feature exist In: the nanoscale barium sulfate particle preferably under the conditions of 60~100 DEG C, by NaOH—Na2S2O8Synthetic solvent is added dropwise LS—BaCl2In synthetic solvent, 2~5h is persistently stirred.
5. the nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding according to claim 1 or 4, feature Be: the speed control of the stirring is in 100~500r/min.
6. the nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding according to claim 1, feature exist In: it is 50~90 DEG C that the drying process, which applies temperature, and drying time is 12~48h.
CN201811431969.9A 2018-11-28 2018-11-28 The nanoscale barium sulfate particle synthetic method of sodium lignin sulfonate cladding Withdrawn CN109585826A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116023818A (en) * 2022-12-30 2023-04-28 佛山安亿纳米材料有限公司 Core-shell structured barium sulfate composite material and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116023818A (en) * 2022-12-30 2023-04-28 佛山安亿纳米材料有限公司 Core-shell structured barium sulfate composite material and preparation method and application thereof

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Application publication date: 20190405