CN111740089A - Preparation method of anode material for water-based zinc ion battery - Google Patents
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- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1235—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]2-, e.g. Li2Mn2O4, Li2[MxMn2-x]O4
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention discloses a preparation method of a polyaniline coating material for a positive electrode of a water system zinc ion battery. Firstly, dissolving zinc acetate dihydrate and manganese acetate tetrahydrate in an ethanol solution, stirring and reacting for 1 hour, then transferring to an autoclave, and placing in a 120 ℃ oven to continue reacting for 12-18 hours to obtain spinel type ZnMn2O4(ii) a Then ZnMn is put into2O4Ammonium persulfate and aniline are mixed in aqueous solution to synthesize polyaniline and para-ZnMn2O4Finally washing and drying the product to obtain the polyaniline-coated ZnMn2O4And (3) a positive electrode material. The preparation method is relatively simple, safe in experiment and low in cost, and the obtained polyaniline-coated ZnMn2O4Compared with pure-ZnMn anode material2O4The electrochemical performance is better, and the assembled zinc ion battery has good application prospect.
Description
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a cathode material of a water-based zinc ion secondary battery.
Background
In recent years, non-alkaline zinc ion water system secondary batteries are regarded as possible substitute products of lithium ion batteries due to the advantages of high relative energy storage, low toxicity, safety, reliability and the like, and are widely concerned by scientific research communities. With the continuous and deep research, more and more positive electrode materials of zinc ion batteries are excavated, and the battery performance is continuously improved, but the currently found positive electrode materials have lower conductivity, and the higher conductivity is more beneficial to the transfer of zinc ions in the charging and discharging processes, so that the transmission speed of carriers is improved. Polyaniline is used as a high polymer material with excellent processing performance and better conductivity, and can be combined with a positive electrode material by an organic-inorganic hybridization method to improve the electrochemical performance of the water system zinc ion battery. Yehong Du et al general V2O5After being compounded with polyaniline, the composite material is used as a positive electrode material of an aqueous zinc ion battery and is found to be 100 mA.g-1Has a current density of 361mAh g-1Compared to pure V2O5The electrochemical performance is obviously improved (materials letters, 10.1016/j. matlet.2020.127813). Thus, we prepared polyaniline-coated ZnMn2O4The positive electrode material and the test result show that: this material is compatible with uncoated ZnMn2O4The cathode material shows more excellent electrochemical performance than the cathode material.
Disclosure of Invention
The invention aims to prepare ZnMn in advance2O4Polyaniline is coated in water environment, and ZnMn coated with polyaniline is prepared by controlling the polymerization temperature and the polymerization time of polyaniline2O4And (3) a positive electrode material to improve the electrical conductivity of the material. The method has the advantages of low cost of raw materials and relatively simple preparation process, and the prepared anode material has good circulation stability and is compatible with pure ZnMn2O4The positive electrode material has a higher reversible capacity than the positive electrode material.
In order to realize the purpose of the invention, the following technical scheme is provided:
(1) dissolving zinc acetate dihydrate and manganese acetate tetrahydrate in a certain amount of alcohol solution according to a molar ratio of 1:2, and reacting for 0.5-1 hour under magnetic stirring;
(2) dropwise adding an alkaline solution into the transparent solution obtained in the step (1) to adjust the pH value to 9-10, gradually blackening the solution, and continuously stirring for 1-2 hours;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12-18 hours, taking out the autoclave after cooling, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki product, and drying the product at 40-60 ℃ overnight to obtain the spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in a certain amount of deionized water, and adding spinel-type ZnMn2O4Placing aniline with the mass ratio of 1: 3-7.5 in an oil bath at 80-120 ℃, stirring at a high speed for 0.5 hour, adding 50g/L ammonium persulfate solution into the solution at a speed of one drop per second, wherein the mass ratio of ammonium persulfate to aniline is 5:2, continuously reacting for 6 hours, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a product, and drying the product at 40-60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O4The material, the conductive agent and the binder are mixed according to the mass ratio of 8:1:1 or 9:0:1, a proper amount of N-methyl pyrrolidone is dripped, the mixture is ground for 3-4 hours by a ball mill, the mixed slurry is coated on a stainless steel foil, and the stainless steel foil is dried for 10-12 hours in vacuum at 100-120 ℃ to obtain the cathode material.
Further, the alcohol in step (1) of claim 1 is at least one of methanol, ethanol or ethylene glycol.
Further, the alkaline solution in the step (2) according to claim 1 is at least one of aqueous ammonia or aqueous sodium hydroxide solution.
Further, in the step (5) of claim 1, the conductive agent is at least one of acetylene black, conductive carbon black, graphene or carbon nanotubes.
Further, in the step (5) of claim 1, the binder is one of polyvinylidene chloride, acrylonitrile multipolymer or styrene butadiene rubber.
Features of the invention
The method has the advantages of relatively simple preparation process, safe production process and low cost, and the obtained cathode material has higher conductivity and better electrochemical performance.
Detailed Description
Example 1:
(1) dissolving 0.878g of zinc acetate dihydrate and 1.96g of manganese acetate tetrahydrate in 40mL of ethanol solution, and reacting for 1 hour under magnetic stirring;
(2) dropwise adding ammonia water into the transparent solution obtained in the step (1) to adjust the pH value to 9, gradually turning the solution black, and continuously stirring for 1 hour;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12 hours, taking out the autoclave after the autoclave is cooled, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki product, and drying the product at 60 ℃ overnight to obtain the spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in 50mL of deionized water, and adding 200
Putting L aniline in an oil bath at the temperature of 80 ℃, stirring at high speed for 0.5 hour, adding 10ml of 50g/L ammonium persulfate solution into the solution at the speed of one drop per second, continuously reacting for 6 hours, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a product, and drying the product at the temperature of 60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O40.8g of material, 0.1g of acetylene black and 0.1g of polyvinylidene fluoride, and dropwise addingAn appropriate amount of N-methylpyrrolidone was ground with a ball mill for 4 hours, and then the mixed slurry was coated on a stainless steel foil and vacuum-dried at 110 ℃ for 12 hours to obtain a positive electrode material.
Example 2:
(1) dissolving 0.878g of zinc acetate dihydrate and 1.96g of manganese acetate tetrahydrate in 40mL of ethanol solution, and reacting for 1 hour under magnetic stirring;
(2) dropwise adding NaOH aqueous solution into the transparent solution obtained in the step (1) to adjust the pH value to 10, gradually blackening the solution, and continuously stirring for 1 hour;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12 hours, taking out the autoclave after the autoclave is cooled, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki product, and drying the product at 60 ℃ overnight to obtain the spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in 50mL of deionized water, and adding 200
L aniline is placed in an oil bath environment at the temperature of 80 ℃, continuously stirred for 1 hour at a high magnetic stirring speed, then 10ml of ammonium persulfate solution of 50g/L is added into the solution at the speed of one drop per second, the reaction is continuously carried out for 6 hours, the lower layer precipitate is alternately washed for a plurality of times by ethanol and deionized water to obtain a product, and then the product is dried at the temperature of 60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O40.9g of the material and 0.1g of polyvinylidene fluoride, and a proper amount of N-methyl pyrrolidone was added dropwise, and after grinding for 4 hours with a ball mill, the mixed slurry was coated on a stainless steel foil, and vacuum-dried at 110 ℃ for 12 hours to obtain a positive electrode material.
Example 3:
(1) dissolving 0.878g of zinc acetate dihydrate and 1.96g of manganese acetate tetrahydrate in 40mL of methanol solution, and reacting for 1 hour under magnetic stirring;
(2) dropwise adding ammonia water into the transparent solution obtained in the step (1) to adjust the pH value to 9, gradually turning the solution black, and continuously stirring for 1 hour;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12 hours, taking out the autoclave after the autoclave is cooled, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki product, and drying the product at 60 ℃ overnight to obtain the spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in 50mL of deionized water, and adding 150 percent
Putting L aniline in an oil bath at the temperature of 80 ℃, stirring at high speed for 0.5 hour, adding 7.5 ml of ammonium persulfate solution of 50g/L into the solution at the speed of one drop per second, continuously reacting for 6 hours, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a product, and drying the product at the temperature of 60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O40.8g of the material, 0.1g of acetylene black and 0.1g of polyvinylidene fluoride, and a proper amount of N-methylpyrrolidone was added dropwise, and after grinding for 4 hours with a ball mill, the mixed slurry was coated on a stainless steel foil, and vacuum-dried at 110 ℃ for 12 hours to obtain a positive electrode material.
Example 4:
(1) dissolving 0.878g of zinc acetate dihydrate and 1.96g of manganese acetate tetrahydrate in 40mL of ethanol solution, and reacting for 1 hour under magnetic stirring;
(2) dropwise adding ammonia water into the transparent solution obtained in the step (1) to adjust the pH value to 9, gradually turning the solution black, and continuously stirring for 1 hour;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12 hours, taking out the autoclave after the autoclave is cooled, and alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki productAnd drying the product at 60 ℃ overnight to obtain spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in 50mL of deionized water, and adding 250
L aniline, placing in an oil bath at 80 ℃, stirring at high speed for 0.5 hour, adding 12.5ml of ammonium persulfate solution of 50g/L into the solution at the speed of one drop per second, continuously reacting for 6 hours, alternately washing the lower-layer precipitate for several times by using ethanol and deionized water to obtain a product, and drying the product at 60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O40.9g of the material and 0.1g of polyvinylidene fluoride, and a proper amount of N-methyl pyrrolidone was added dropwise, and after grinding for 4 hours with a ball mill, the mixed slurry was coated on a stainless steel foil, and vacuum-dried at 100 ℃ for 12 hours to obtain a positive electrode material.
Claims (5)
1. ZnMn coated by conductive polymer polyaniline2O4The preparation method of the water system zinc ion battery positive electrode material is characterized by comprising the following steps:
(1) dissolving zinc acetate dihydrate and manganese acetate tetrahydrate in a certain amount of alcohol solution according to a molar ratio of 1:2, and reacting for 0.5-1 hour under magnetic stirring;
(2) dropwise adding an alkaline solution into the transparent solution obtained in the step (1) to adjust the pH value to 9-10, gradually blackening the solution, and continuously stirring for 1-2 hours;
(3) transferring the black solution obtained in the step (2) into an autoclave, placing the autoclave in a 120 ℃ oven for reaction for 12-18 hours, taking out the autoclave after cooling, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a khaki product, and drying the product at 40-60 ℃ overnight to obtain the spinel type ZnMn2O4；
(4) Spinel type ZnMn obtained in the step (3)2O4Dispersing in a certain amount of deionized water, and adding spinel-type ZnMn2O4Placing aniline with the mass ratio of 1: 3-7.5 in an oil bath at 80-120 ℃, stirring at a high speed for 0.5 hour, adding 50g/L ammonium persulfate solution into the solution at a speed of one drop per second, wherein the mass ratio of ammonium persulfate to aniline is 5:2, continuously reacting for 6 hours, alternately washing the lower-layer precipitate for a plurality of times by using ethanol and deionized water to obtain a product, and drying the product at 40-60 ℃ overnight to obtain polyaniline-coated ZnMn2O4A composite material;
(5) taking ZnMn coated by polyaniline in the step (4)2O4The material, the conductive agent and the binder are mixed according to the mass ratio of 8:1:1 or 9:0:1, a proper amount of N-methyl pyrrolidone is dripped, the mixture is ground for 3-4 hours by a ball mill, the mixed slurry is coated on a stainless steel foil, and the stainless steel foil is dried for 10-12 hours in vacuum at 100-120 ℃ to obtain the cathode material.
2. The polyaniline-coated ZnMn for aqueous zinc-ion batteries according to claim 12O4The preparation method of the cathode material is characterized in that the alcohol in the step (1) is at least one of methanol, ethanol or ethylene glycol.
3. The polyaniline-coated ZnMn for aqueous zinc-ion batteries according to claim 12O4The preparation method of the cathode material is characterized in that the alkaline solution in the step (2) is at least one of ammonia water or sodium hydroxide aqueous solution.
4. The polyaniline-coated ZnMn for aqueous zinc-ion batteries according to claim 12O4The preparation method of the cathode material is characterized in that the conductive agent in the step (5) is at least one of acetylene black, conductive carbon black, graphene or carbon nano tubes.
5. The polyaniline-coated ZnMn for aqueous zinc-ion batteries according to claim 12O4The preparation method of the cathode material is characterized in that the binder in the step (5) is one of polyvinylidene chloride, acrylonitrile multipolymer or styrene butadiene rubber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112421028A (en) * | 2020-12-02 | 2021-02-26 | 齐鲁工业大学 | Preparation method of novel water-based zinc ion battery positive electrode material |
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| CN102097661A (en) * | 2009-12-11 | 2011-06-15 | 清华大学深圳研究生院 | Rechargeable zinc ion battery using zinc manganate as anode |
| KR20170124791A (en) * | 2016-05-03 | 2017-11-13 | 경희대학교 산학협력단 | Anode material of zinc air cell and method for preparing the same |
| CN110498454A (en) * | 2019-07-30 | 2019-11-26 | 复旦大学 | A kind of spinel type nanometer crystalline substance material and its preparation method and application |
| CN110828795A (en) * | 2019-10-29 | 2020-02-21 | 陈璞 | Zinc-manganese-oxygen cathode material and preparation method and application thereof |
| US20200227739A1 (en) * | 2017-07-28 | 2020-07-16 | Research Foundation Of The City University Of New York | Process for making manganese dioxide and its polymorphs reversible |
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| CN102097661A (en) * | 2009-12-11 | 2011-06-15 | 清华大学深圳研究生院 | Rechargeable zinc ion battery using zinc manganate as anode |
| KR20170124791A (en) * | 2016-05-03 | 2017-11-13 | 경희대학교 산학협력단 | Anode material of zinc air cell and method for preparing the same |
| US20200227739A1 (en) * | 2017-07-28 | 2020-07-16 | Research Foundation Of The City University Of New York | Process for making manganese dioxide and its polymorphs reversible |
| CN110498454A (en) * | 2019-07-30 | 2019-11-26 | 复旦大学 | A kind of spinel type nanometer crystalline substance material and its preparation method and application |
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Cited By (1)
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| CN112421028A (en) * | 2020-12-02 | 2021-02-26 | 齐鲁工业大学 | Preparation method of novel water-based zinc ion battery positive electrode material |
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