CN112599776B - Preparation method of calamine cream gel applied to alkaline zinc-manganese battery - Google Patents
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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
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention discloses a preparation method of a calamine cream gel applied to an alkaline zinc-manganese battery, which comprises the steps of adding cationic polyacrylamide and modified diatomite into distilled water, then adding soluble starch, stirring for 10-20 min at room temperature, then concentrating, drying, grinding, freeze-drying a self-made composite gel for 0.5-3 h in a liquid nitrogen environment, then vacuumizing and drying for 3-6 h at 40-45 ℃, adding the product obtained in the step S1 and silicon dioxide into a ball mill, grinding for 4-8 h, and discharging to obtain the gel.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to a preparation method of a zinc paste gel applied to an alkaline zinc-manganese battery.
Background
Alkaline zinc-manganese batteries are the most widely used commercial battery products to date. The calamine cream is used as an important composition material for preparing the alkaline zinc-manganese dioxide battery, and the performance of the calamine cream plays a key role in the discharge capacity and the service life of the alkaline battery. In the zinc paste of the current alkaline zinc-manganese battery, much mercury and lead are contained, which causes the battery to have bad influence on the environment after being discarded. Therefore, there is a strong need to provide a zinc paste for alkaline batteries which has a high discharge capacity, a long service life, and is lead-free and mercury-free.
The zinc paste gel is one of key materials for preparing cathode zinc paste in an alkaline manganese battery. The gelling agent can fix the zinc powder to ensure that the zinc powder is uniformly dispersed; absorbing and fixing the electrolyte to provide enough electrolyte for the reaction of the zinc cathode; the solid-liquid separation of the battery in the storage process is prevented; the surface performance of the zinc powder is improved, and the discharge performance of the battery is improved. At present, for mercury-free alkaline zinc-manganese dioxide batteries, two types of gel are mainly polyacrylic acid type and sodium polyacrylate, wherein the sodium polyacrylate type gel is mainly used for improving the vibration resistance. Because different types of gelling agents are developed and produced according to different requirements and by using different processes, certain differences exist in performance, and the requirements are difficult to completely meet by using one gelling agent, the requirements on the performance of the battery are often met by matching two or more gelling agents with different specifications. And the current battery calamine cream gel has the problems of poor expansion rate, water retention performance and discharge performance.
Disclosure of Invention
Aiming at the problems of poor expansion rate, poor water retention performance and poor discharge performance of the calamine cream gel in the alkaline zinc-manganese dioxide battery in the prior art, the invention aims to provide a preparation method of the calamine cream gel applied to the alkaline zinc-manganese dioxide battery, and the preparation method comprises the following steps:
s1: adding cationic polyacrylamide and modified diatomite into distilled water, then adding soluble starch, stirring at room temperature for 10-20 min, then concentrating, drying and grinding for the next step, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is (0.8-1.3) to (1-1.68) to (0.69-0.88).
S2: and (2) freeze-drying the self-made composite gel for 0.5-3 h in a liquid nitrogen environment, then carrying out vacuum-pumping drying for 3-6 h at 40-45 ℃, adding the self-made composite gel, the product obtained in the step S1 and silicon dioxide into a ball mill, grinding for 4-8 h, and discharging to obtain the gel, wherein the mass ratio of the product obtained in the step S1 to the silicon dioxide is (50-85) to (20-30) to (8-12).
Preferably, the cationic polyacrylamide is selected from polyacrylamide with molecular weight of 800-1000 ten thousand and cationic concentration of 40-60%.
Preferably, the modified diatomite is prepared by the following method:
1) Adding diatomite into distilled water, then adding sodium bisulfate, stirring for 50-80 min at 50-65 ℃, then adding graphene oxide, continuously stirring and reacting for 20-40 min at the temperature, wherein the mass-volume ratio of the diatomite to the distilled water to the sodium bisulfate to the graphene oxide is (2-6) g, (80-150) mL, (1.3-3.2) g, (0.88-1.69) g, and standing for later use.
2) Adding polyacrylic acid into the step 1), stirring and reacting at room temperature for 6-10 h, filtering, drying, grinding, and screening with a 600-mesh screen to obtain the modified diatomite.
More preferably, the amount of polyacrylic acid added in the step 2) is 30 to 45% of the amount of diatomaceous earth.
Preferably, the self-made composite gel is prepared by the following method:
adding sodium polyacrylate into a sodium hydroxide aqueous solution, stirring for 6-15 min at room temperature, then adding a cross-linking agent and sodium bisulfite, continuing to stir for 35-50 min, stopping stirring, and standing for 5-10 h to obtain the self-made gel, wherein the mass-volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, the cross-linking agent and the sodium bisulfite is (1-3) g, (20-40) mL, (0.44-0.86) mL and (0.9-1.15) g.
More preferably, the concentration of the aqueous sodium hydroxide solution is 10 to 15%.
More preferably, the crosslinking agent is propylene glycol.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, (1) the diatomite has high specific surface area and rich groups and charges on the surface, and HSO in sodium hydrogen sulfate is utilized 4 - The anionic free radicals initiate the diatomite to generate free radicals, and the diatomite and polyacrylic acid are subjected to grafting reaction to form a network structure, so that a certain fixing effect on zinc particles is achieved, and meanwhile, the diatomite surface is rich in hydrophilic groups and has a strong water retention effect; (2) The diatomite has certain thickening and bonding properties, has excellent water retention and water locking properties after being compounded with polyacrylamide with high molecular weight and high cation concentration, and the cationic polyacrylamide also has good adsorption property, so that zinc powder particles can be adsorbed and fixed in a gel network to avoid sedimentation; (3) The diatomite is compositely modified by the graphene oxide, the surfaces of the diatomite and the graphene oxide have rich hydroxyl groups and other groups, strong hydrogen bonds are generated, the excellent conductivity of the graphene oxide is utilized, the conductivity between zinc powder particles and particles is improved by a hydrogen bond network, the internal resistance of the battery is reduced, the discharge performance is improved, and the battery performance is further improved by the mutual matching of the zinc powder particles and the cationic polyacrylamide; (4) The gel self-made by sodium polyacrylate forms a network structure after adding the cross-linking agent propylene glycol, and is matched to play a role in water retentionAnd (5) water locking effect.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of a calamine cream gel applied to an alkaline zinc-manganese dioxide battery specifically comprises the following steps:
the modified diatomite is prepared by the following method:
1) Adding diatomite into distilled water, then adding sodium bisulfate, stirring for 50min at 50 ℃, then adding graphene oxide, and continuing to stir at the temperature for 20min, wherein the mass-volume ratio of the diatomite to the distilled water to the sodium bisulfate to the graphene oxide is 2g.
2) Adding polyacrylic acid into the step 1), stirring at room temperature for reaction for 6 hours, filtering, drying, grinding, and sieving with a 600-mesh sieve to obtain the modified diatomite, wherein the amount of the added polyacrylic acid is 30% of the amount of the diatomite.
The self-made composite gel is prepared by the following method:
adding sodium polyacrylate into a 10% sodium hydroxide aqueous solution, stirring at room temperature for 6min, then adding a cross-linking agent and sodium bisulfite, continuing to stir for 35min, stopping stirring, and standing for 5-10 h to obtain a self-made gel, wherein the mass volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, propylene glycol and sodium bisulfite is 1g.
S1: adding cationic polyacrylamide with the molecular weight of 800 ten thousand and the cation concentration of 40% and modified diatomite into distilled water, then adding soluble starch, stirring for 10min at room temperature, then concentrating, drying and grinding, and preparing for the next step, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is 0.8.
S2: and (2) freeze-drying the self-made composite gel for 0.5h in a liquid nitrogen environment, then carrying out vacuum-pumping drying for 3h at 40 ℃, adding the self-made composite gel, the product obtained in the step S1 and silicon dioxide into a ball mill, grinding for 4h, and discharging to obtain the gel, wherein the mass ratio of the self-made composite gel to the product obtained in the step S1 to the silicon dioxide is 50.
Example 2
A preparation method of a calamine cream gel applied to an alkaline zinc-manganese dioxide battery specifically comprises the following steps:
the modified diatomite is prepared by the following method:
1) Adding diatomite into distilled water, then adding sodium bisulfate, stirring at 65 ℃ for 80min, then adding graphene oxide, and continuing to stir at the temperature for 40min, wherein the mass-volume ratio of the diatomite to the distilled water to the sodium bisulfate to the graphene oxide is 6g.
2) Adding polyacrylic acid into the step 1), stirring at room temperature for reaction for 10 hours, filtering, drying, grinding, and sieving with a 600-mesh sieve to obtain the modified diatomite, wherein the amount of the added polyacrylic acid is 45% of the amount of the diatomite.
The self-made composite gel is prepared by the following method:
adding sodium polyacrylate into a 15% sodium hydroxide aqueous solution, stirring at room temperature for 15min, then adding a crosslinking agent and sodium bisulfite, continuing to stir for 50min, stopping stirring, and standing for 10h to obtain a self-made gel, wherein the mass volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, propylene glycol and sodium bisulfite is 3 g.
S1: adding cationic polyacrylamide with the molecular weight of 1000 ten thousand and the cation concentration of 60% and modified diatomite into distilled water, then adding soluble starch, stirring for 20min at room temperature, then concentrating, drying and grinding, and preparing for the next step, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is 1.3.
S2: freeze-drying the self-made composite gel for 3h in a liquid nitrogen environment, then carrying out vacuum-pumping drying for 6h at 45 ℃, adding the self-made composite gel, the product in the step S1 and silicon dioxide into a ball mill to grind for 8h, and discharging to obtain the gel, wherein the mass ratio of the self-made composite gel to the product in the step S1 to the silicon dioxide is 85.
Example 3
A preparation method of a calamine cream gel applied to an alkaline zinc-manganese dioxide battery specifically comprises the following steps:
the modified diatomite is prepared by the following method:
1) Adding kieselguhr into distilled water, then adding sodium bisulfate, stirring at 55 ℃ for 60min, then adding graphene oxide, and continuing to stir at the temperature for reaction for 30min, wherein the mass-volume ratio of the kieselguhr to the distilled water to the sodium bisulfate to the graphene oxide is 3 g.
2) Adding polyacrylic acid into the step 1), stirring at room temperature for reaction for 8 hours, filtering, drying, grinding, and sieving with a 600-mesh sieve to obtain the modified diatomite, wherein the amount of the added polyacrylic acid is 35% of the amount of the diatomite.
The self-made composite gel is prepared by the following method:
adding sodium polyacrylate into a 12% sodium hydroxide aqueous solution, stirring at room temperature for 10min, then adding a cross-linking agent and sodium bisulfite, continuing to stir for 40min, stopping stirring, and standing for 7h to obtain a self-made gel, wherein the mass volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, propylene glycol and sodium bisulfite is 2g.
S1: adding cationic polyacrylamide with the molecular weight of 900 ten thousand and the cation concentration of 50% and modified diatomite into distilled water, then adding soluble starch, stirring for 15min at room temperature, then concentrating, drying and grinding, and preparing for the next step, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is 1.1.
S2: and (2) freeze-drying the self-made composite gel for 2h in a liquid nitrogen environment, then carrying out vacuum-pumping drying for 5h at 42 ℃, adding the self-made composite gel, the product obtained in the step S1 and silicon dioxide into a ball mill, grinding for 6h, and discharging to obtain the gel, wherein the mass ratio of the self-made composite gel to the product obtained in the step S1 to the silicon dioxide is 65.
Example 4
A preparation method of a calamine cream gel applied to an alkaline zinc-manganese dioxide battery specifically comprises the following steps:
the modified diatomite is prepared by the following method:
1) Adding kieselguhr into distilled water, then adding sodium bisulfate, stirring at 60 ℃ for 70min, then adding graphene oxide, and continuing to stir at the temperature for 35min, wherein the mass-volume ratio of the kieselguhr to the distilled water to the sodium bisulfate to the graphene oxide is 5g.
2) Adding polyacrylic acid into the step 1), stirring at room temperature for reaction for 9 hours, filtering, drying, grinding, and sieving with a 600-mesh sieve to obtain the modified diatomite, wherein the amount of the added polyacrylic acid is 40% of the amount of the diatomite.
The self-made composite gel is prepared by the following method:
adding sodium polyacrylate into a 14% sodium hydroxide aqueous solution, stirring at room temperature for 13min, then adding a crosslinking agent and sodium bisulfite, continuing to stir for 45min, stopping stirring, and standing for 9h to obtain a self-made gel, wherein the mass volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, propylene glycol and sodium bisulfite is 2.7 g.
S1: adding cationic polyacrylamide with the molecular weight of 1000 ten thousand and the cation concentration of 55% and modified diatomite into distilled water, then adding soluble starch, stirring for 20min at room temperature, then concentrating, drying, grinding, and using the following steps, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is 1.2.
S2: freeze-drying the self-made composite gel for 2.5h in a liquid nitrogen environment, then carrying out vacuum drying for 5h at 43 ℃, adding the self-made composite gel, the product in the step S1 and silicon dioxide into a ball mill to grind for 7h, and discharging to obtain the gel, wherein the mass ratio of the self-made composite gel to the product in the step S1 to the silicon dioxide is 80.
Comparative example 1
PW-150 type calamine jelly gels were purchased commercially.
Comparative example 2
The cell zinc paste gel produced by a certain science and technology company in Jiangsu province is purchased from the commercial industry.
Experimental example: the calamine cream gels prepared in examples 1-4 were subjected to the following performance tests,
performance test (1) expansion ratio: respectively injecting 200g of test piece into different marked plastic pipes, compacting, injecting liquid paraffin on the test piece, sealing, and reading the height (H) of the test piece 1 ) And paraffin level (H) 2 ) (ii) a Then placing the plastic tube in a constant temperature oven at 70 ℃ for a certain time, taking out the plastic tube from the constant temperature oven, cooling to room temperature, and reading the liquid level height (H) of paraffin 3 ) The expansion ratio can be obtained by the following formula,
expansion ratio (%) = [ (H) 3 -H 2 )/H 1 ]×100％；
(2) Water loss: forced convection environment is temperature 20 ℃, relative humidity is 60%, the speed of wind swept by the upper surface of the battery is 7.0m/s, air inlets and air outlets are respectively arranged at two sides of the experiment box body, the battery of the test piece is connected with a constant current discharge instrument to perform constant current discharge work, the working current is 10A, the time is 2h, the change condition of the voltage of the battery is recorded, and each data point is subjected to four times of repeated experiments respectively, so that the average water loss of the test piece is measured;
(3) Discharge performance: respectively carrying out 1500mA repeated discharge tests on the manufactured batteries for 5 times by adopting a DM-2000 primary battery performance tester; the results of the above tests are shown in table 1,
table 1. Results of performance testing:
as can be seen from Table 1, the expansion ratios of the zinciferous paste gels prepared in examples 1-4 of the present invention were all lower than 11.7%, the water loss was about 0.8g, and the discharge performance was 34.2 or more, which is lower than that of the zinciferous paste gels in comparative examples 1 and 2, and higher than that of the zinciferous paste gels in comparative examples 1-2.
Claims (5)
1. A preparation method of a calamine cream gel applied to an alkaline zinc-manganese dioxide battery is characterized by comprising the following steps:
s1: adding cationic polyacrylamide and modified diatomite into distilled water, adding soluble starch, stirring at room temperature for 10-20min, concentrating, drying, grinding, and using the following steps, wherein the mass ratio of the cationic polyacrylamide to the modified diatomite to the soluble starch is (0.8-1.3) to (1-1.68) to (0.69-0.88);
s2: freeze-drying the self-made composite gel for 0.5 to 3 hours in a liquid nitrogen environment, then carrying out vacuum drying for 3 to 6 hours at the temperature of 40 to 45 ℃, adding the self-made composite gel, the product obtained in the step S1 and silicon dioxide into a ball mill, grinding for 4 to 8 hours, and discharging to obtain the gel, wherein the mass ratio of the self-made composite gel to the product obtained in the step S1 to the silicon dioxide is (50 to 85): (20 to 30): (8 to 12);
wherein, the modified diatomite is prepared by the following method:
1) Adding diatomite into distilled water, then adding sodium bisulfate, stirring for 50-80min at 50-65 ℃, then adding graphene oxide, continuing to react for 20-40 min at 50-65 ℃, wherein the mass-volume ratio of the diatomite to the distilled water to the sodium bisulfate to the graphene oxide is (2~6) g, (80-150) mL, (1.3-3.2) g and (0.88-1.69) g, and standing for later use;
2) Adding polyacrylic acid into the step 1), stirring at room temperature for reaction for 6-10h, filtering, drying, grinding, and airing through a 600-mesh screen to obtain modified diatomite;
the self-made composite gel is prepared by the following method: adding sodium polyacrylate into a sodium hydroxide aqueous solution, stirring for 6-15min at room temperature, then adding a crosslinking agent and sodium bisulfite, continuing stirring for 35-50min, stopping stirring, and standing for 5-10h to obtain a self-made gel, wherein the mass volume ratio of the sodium polyacrylate, the sodium hydroxide aqueous solution, the crosslinking agent and the sodium bisulfite is (1~3) g, (20-40) mL, (0.44-0.86) mL, (0.9-1.15) g.
2. The preparation method of the calamine cream gel applied to the alkaline zinc-manganese dioxide battery as claimed in claim 1, wherein the cationic polyacrylamide is selected from polyacrylamide with molecular weight of 800 to 1000 ten thousand and cationic concentration of 40 to 60%.
3. The method for preparing the calamine cream gel applied to the alkaline zinc-manganese dioxide battery as claimed in claim 1, wherein the amount of the polyacrylic acid added in the step 2) is 30 to 45 percent of the amount of the diatomite.
4. The method for preparing the calamine cream gel applied to the alkaline zinc-manganese dioxide battery as claimed in claim 1, wherein the concentration of the sodium hydroxide aqueous solution is 10-15%.
5. The method of claim 1, wherein the cross-linking agent is propylene glycol.
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| JPH04121961A (en) * | 1990-09-12 | 1992-04-22 | Matsushita Electric Ind Co Ltd | Zinc alloy for zinc alkaline battery and its manufacture and zinc alkaline battery using it |
| CN108777304A (en) * | 2018-05-18 | 2018-11-09 | 田秋珍 | Gel special for battery zinc paste |
| CN109817981A (en) * | 2018-12-25 | 2019-05-28 | 宁波富邦电池有限公司 | Alkaline battery cathode synthesis gel |
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| US9548511B2 (en) * | 2012-07-18 | 2017-01-17 | Nthdegree Technologies Worldwide Inc. | Diatomaceous energy storage devices |
| CN107039645B (en) * | 2017-04-11 | 2020-01-31 | 宁波富邦电池有限公司 | Primary alkaline battery negative electrode material and preparation method thereof |
| CN109666168A (en) * | 2017-10-17 | 2019-04-23 | 翁秋梅 | A kind of self-repairability solid-state hydridization dynamic aggregation object and its application |
| CN207925562U (en) * | 2017-12-15 | 2018-09-28 | 中银（宁波）电池有限公司 | Maintainable alkaline zinc-manganese battery |
| CN108976686B (en) * | 2018-07-03 | 2021-03-02 | 辽宁本特耐科技发展有限公司 | Composite hydrogel, anti-seepage coiled material, preparation method and application thereof |
| CN110534699B (en) * | 2019-08-22 | 2021-07-13 | 江苏大毛牛新材料有限公司 | Preparation method of lithium ion battery negative plate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04121961A (en) * | 1990-09-12 | 1992-04-22 | Matsushita Electric Ind Co Ltd | Zinc alloy for zinc alkaline battery and its manufacture and zinc alkaline battery using it |
| CN108777304A (en) * | 2018-05-18 | 2018-11-09 | 田秋珍 | Gel special for battery zinc paste |
| CN109817981A (en) * | 2018-12-25 | 2019-05-28 | 宁波富邦电池有限公司 | Alkaline battery cathode synthesis gel |
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