CN114539602B - Milk rubber microporous foam battery separator and preparation method thereof - Google Patents
Milk rubber microporous foam battery separator and preparation method thereof Download PDFInfo
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- CN114539602B CN114539602B CN202210244259.5A CN202210244259A CN114539602B CN 114539602 B CN114539602 B CN 114539602B CN 202210244259 A CN202210244259 A CN 202210244259A CN 114539602 B CN114539602 B CN 114539602B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/429—Natural polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/042—Elimination of an organic solid phase
- C08J2201/0422—Elimination of an organic solid phase containing oxygen atoms, e.g. saccharose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- 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
Abstract
The invention discloses a milk rubber microporous foam battery separator which comprises the following raw materials in percentage by mass: 40-90% of latex, 1-10% of vulcanizing bag, 1-15% of foaming agent, 1-10% of antioxidant, 1-50% of fumed silica and 1-2% of color paste. The invention provides a latex rubber microporous foam battery separator which has good elasticity, is favorable for tight assembly of a battery, prevents active substances of a battery polar plate from softening and falling off, and prolongs the cycle life of the battery. The invention also provides a preparation method of the emulsion rubber microporous foam battery separator.
Description
Technical Field
The invention relates to the technical field of battery separators, in particular to a milk rubber microporous foam battery separator and a preparation method thereof.
Background
The battery diaphragm has the function of isolating the anode and the cathode in the battery, can avoid the short circuit of the anode and the cathode in the battery, and meanwhile, the separator can allow conductive ions to pass through, and has the thickness, the porosity, the aperture and the tortuosity degree of the hole, which have important influence on the capacity of the high-rate discharge of the battery and the terminal voltage level, and the stability of the separator directly influences the service life of the battery. For electrolytes alone, the separator is required to have sufficient space and pores to conduct ions therethrough. With the intensive research of batteries, it is continuously recognized that separators play an important role in improving battery performance and prolonging battery life.
The prior battery separator mainly comprises a glass fiber separator, a PVC separator by a sintering method, a polyethylene PE separator and the like. The existing separators have problems, such as small rebound force, mud formation in the later period, weak binding force of electrolyte, layering and insufficient puncture resistance of the glass fiber separator; the porosity of the PVC diaphragm by the sintering method is small; the polyethylene PE separator has the problems of weak oxidation resistance and chemical stability and the like.
Disclosure of Invention
The invention aims to provide a latex rubber microporous foam battery separator which has good reverse elasticity, is favorable for tight assembly of a battery, prevents active substances of a battery polar plate from softening and falling off, and prolongs the cycle life of the battery.
The invention discloses a milk rubber microporous foam battery separator and a preparation method thereof, wherein the technical scheme adopted by the invention is as follows:
the latex rubber microporous foam battery separator comprises the following raw materials in percentage by mass: 40-90% of latex, 1-10% of vulcanizing bag, 1-15% of foaming agent, 1-10% of antioxidant, 1-50% of fumed silica and 1-2% of color paste.
Preferably, the vulcanizing bag comprises sulfur powder and zinc oxide, wherein the mass ratio of the sulfur powder is 1-75%, and the mass ratio of the zinc oxide is 1-75%.
A preparation method of a milk rubber microporous foam battery separator comprises the following steps:
s1, adding various raw materials into a speed-regulating mixer, uniformly mixing, and forming foaming slurry through a foaming machine;
s2, conveying the foaming slurry formed in the step S1 to a coating mechanism through a conveying device, and scraping and coating the foaming slurry on Teflon support cloth through the coating mechanism to form a sheet;
s3, conveying the sheet formed in the S2 to an infrared heating shaping tunnel box through a conveying device, heating and shaping to form a gelatinous sheet, and then entering a vulcanization tunnel box for cross-linking vulcanization to solidify and shape the gelatinous sheet;
s4, heating, vulcanizing and shaping in the step S3, and then washing by a washing machine;
s5, carrying out hot air drying on the sheet after washing in the S4 through a drying tunnel to finally form a microporous rubber elastomer separator, and rolling the separator.
Preferably, the stirring frequency in the step S1 is gradually increased and regulated from 0 to 50 Hz.
Preferably, the infrared temperature range in the S3 is 110-130 ℃.
Preferably, the water washing temperature in the step S4 is 25-35 ℃, and potassium oleate is eluted by water washing.
The invention discloses a milk rubber microporous foam battery separator which has the beneficial effects that: the gas phase silicon dioxide is added into the separator to be embedded into the rubber reticular structure, so that the pore diameter of 0.1-1 micron is formed, the capillary suction function of the separator is increased, the porosity is increased, the pore diameter is regulated by the foaming agent, so that a large pore with the diameter of 20-40 microns is formed, the separator has the channel condition that oxygen generated by the positive electrode reaches the negative electrode for combination, the bent pore formed by the micro pore foaming prevents the migration of lead ions, the 83-87% high porosity is beneficial to the oxygen combination efficiency in the later stage of charging, the decomposition of electrolyte is reduced, the sealing reaction efficiency of the battery is improved, the cycle life of the battery is prolonged, and the separator has an adsorption effect on the electrolyte and has an improvement effect on preventing the electrolyte layering from causing the increase of the sulfuric acid density at the bottom of the electrode plate to corrode the electrode plate.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a separator for a microcellular foam battery of latex rubber in accordance with the present invention.
Detailed Description
The invention is further illustrated and described below in conjunction with the specific embodiments and the accompanying drawings:
the latex rubber microporous foam battery separator comprises the following raw materials in percentage by mass: 40-90% of latex, 1-10% of vulcanizing bag, 1-15% of foaming agent, 1-10% of antioxidant, 1-50% of fumed silica and 1-2% of color paste.
Through adding the gas phase silicon dioxide in the separator, the gas phase silicon dioxide is inlaid in the rubber reticular structure, the pore diameter of 0.1-1 micron is formed, the capillary suction function of the separator is increased, the porosity is increased, the pore diameter is regulated by the foaming agent, so that a large pore with the diameter of 20-40 microns is formed, the separator has the channel condition that oxygen generated by the positive electrode reaches the negative electrode for combination, the bent pore formed by the micro pore foaming prevents the migration of lead ions, the high porosity of 83-87% is beneficial to the oxygen combination efficiency in the later stage of charging, the decomposition of electrolyte is reduced, the sealing reaction efficiency of the battery is improved, and the cycle life of the battery is prolonged.
And because the separator contains silicon dioxide, the separator has an adsorption effect on electrolyte and an improvement effect on preventing the electrolyte from layering to cause the increase of the sulfuric acid density at the bottom of the polar plate to corrode the polar plate.
The vulcanizing bag comprises sulfur powder and zinc oxide, wherein the mass ratio of the sulfur powder is 1-75%, and the mass ratio of the zinc oxide is 1-75%.
In the above scheme, the foaming agent is potassium oleate.
Referring to fig. 1, a method for preparing a separator for a micro-porous foamed latex cell includes the following steps:
s1, adding various raw materials into a speed-regulating mixer to be uniformly mixed, and forming foaming slurry through a foaming machine. After the raw materials are uniformly mixed, the stirring frequency of the speed-regulating mixer is gradually increased and regulated to 0-50 Hz. The foaming treatment is carried out by a foaming machine, so that foaming slurry with bubbles inside is formed, and the subsequent coating processing treatment is facilitated.
S2, conveying the foaming slurry formed in the step S1 to a coating mechanism through a conveying device, and scraping and coating the foaming slurry on Teflon support cloth through the coating mechanism to form a sheet; a sheet with the thickness of 2 mm and the width of 1 m is formed by the coating scraper, and the thickness and the width of the sheet can be kept consistent by adopting the coating scraper, so that the quality of the finally formed product is ensured to be the same.
S3, conveying the sheet formed in the S2 to an infrared heating shaping tunnel box through a conveying device, wherein the infrared temperature range is 110-130 ℃, and the sheet formed by coating is still in a gelatinous sheet, and then, entering a vulcanization tunnel box for cross-linking vulcanization, so that the sheet is solidified and shaped.
S4, after heating, shaping and vulcanizing in the step S3, washing by a washing machine at the temperature of 25-35 ℃, and washing potassium oleate in the sheet by a washing mode.
S5, carrying out hot air drying on the sheet after washing in S4 through a drying tunnel to finally form a microporous rubber elastomer separator, rolling the separator, and drying the water on the surface of the sheet after washing in a drying mode to finish the product.
In the embodiment, 117.3kg of natural latex, 9.75kg of TC02 vulcanizing bag, 6.37 kg of foaming agent, 5.37kg of fumed silica, 2.63kg of color paste and 7.31kg of antioxidant are added into a variable frequency mixer for speed regulation and mixing, and then foaming slurry is formed through a foaming machine.
The foamed slurry was flowed through a pipe onto a doctor blade apparatus and doctor blade coated on a teflon backing to form a 2 mm thick, one meter wide sheet.
The mixed foaming slurry is continuously operated in the coating and scraping process on a coating and scraping machine, the coated and scraped sheet is subjected to infrared 110-degree shaping tunnel, then enters a vulcanizing tank for 100-degree vulcanization, is subjected to water washing by a 30-degree washing machine, finally enters a drying tunnel tank for 80-degree hot air drying, and an open-pore rubber separator is formed, wherein the main pore diameter of the separator is distributed between 1 and 40 microns, and the porosity is above 83%. And the resulting separator test values are shown in the following table:
the test table data shows that the microporous rubber foam separator has the performance indexes of other battery separators and the rebound resilience key indexes which are not possessed by the glass fiber separator, and the performance indexes have positive effects on the tight assembly requirement of the battery pole plate for preventing the active substances from falling off and prolonging the cycle service life of the battery pole plate.
The invention provides a breast rubber microporous foam battery separator, which is characterized in that fumed silica is added in the separator to enable the fumed silica to be inlaid in a rubber reticular structure, so that the pore diameter of 0.1-1 micron is formed, the capillary suction function of the separator is increased, the porosity is increased, and the pore diameter is regulated by a foaming agent, so that a macroporous with the diameter of 20-40 microns is formed, the separator is provided with a channel condition that oxygen generated by an anode reaches a cathode for combination, the migration of lead ions is prevented by a tortuous pore formed by microporous foaming, the oxygen recombination efficiency in the later stage of charging is facilitated by 83-87%, the decomposition of electrolyte is reduced, the sealing reaction efficiency of a battery is improved, the cycle life of the battery is prolonged, and the separator has an adsorption effect on the electrolyte and an improvement effect on preventing the corrosion of a polar plate due to the increase of sulfuric acid density at the bottom of a polar plate caused by electrolyte layering because the silica is contained in the separator.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (1)
1. A milk rubber microporous foam battery separator, wherein the pore diameter is distributed between 1 and 40 microns, and the porosity is more than 83 percent; the preparation raw materials comprise latex, a vulcanization package, a foaming agent, an antioxidant, fumed silica and color paste, wherein the raw materials comprise the following components in percentage by mass: 40-90% of latex, 1-10% of vulcanizing bag, 1-15% of foaming agent, 1-10% of antioxidant, 1-50% of fumed silica and 1-2% of color paste; the vulcanizing bag comprises sulfur powder and zinc oxide, wherein the mass ratio of the sulfur powder is 1-75%, and the mass ratio of the zinc oxide is 1-75%; the method is characterized in that the emulsion rubber microporous foam battery separator is prepared by the following steps:
s1, adding various raw materials into a speed-regulating mixer, uniformly mixing, and forming foaming slurry through a foaming machine; wherein the stirring frequency is 0-50 Hz, and the stirring frequency is gradually increased and adjusted;
s2, conveying the foaming slurry formed in the step S1 to a coating mechanism through a conveying device, and scraping and coating the foaming slurry on Teflon support cloth through the coating mechanism to form a sheet;
s3, conveying the sheet formed in the S2 to an infrared heating shaping tunnel box through a conveying device, heating and shaping to form a gelatinous sheet, and then entering a vulcanization tunnel box for cross-linking vulcanization to solidify and shape the gelatinous sheet; wherein the infrared temperature range is 110-130 ℃;
s4, heating, vulcanizing and shaping in the step S3, and then washing by a washing machine; wherein the water washing temperature is 25-35 ℃, and the foaming agent is washed out by water;
s5, carrying out hot air drying on the sheet after washing in the S4 through a drying tunnel to finally form a microporous rubber elastomer separator, and rolling the separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210244259.5A CN114539602B (en) | 2022-03-14 | 2022-03-14 | Milk rubber microporous foam battery separator and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210244259.5A CN114539602B (en) | 2022-03-14 | 2022-03-14 | Milk rubber microporous foam battery separator and preparation method thereof |
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| Publication Number | Publication Date |
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| CN114539602A CN114539602A (en) | 2022-05-27 |
| CN114539602B true CN114539602B (en) | 2023-09-19 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB658296A (en) * | 1948-09-18 | 1951-10-03 | Dunlop Rubber Co | Improvements in or relating to the manufacture of microporous sheets of hard rubber |
| GB731935A (en) * | 1951-05-09 | 1955-06-15 | Tudor Ab | Improved method for making microporous separators for electric accumulators and cells |
| US5221587A (en) * | 1991-03-09 | 1993-06-22 | W. R. Grace & Co.-Conn. | Lead/sulphuric acid storage battery |
| CN102130314A (en) * | 2010-01-12 | 2011-07-20 | 华南师范大学 | Novel PVC/rubber composite micropore partition board |
| CN103311484A (en) * | 2008-09-03 | 2013-09-18 | 三菱树脂株式会社 | Laminated porous film for separator |
| CN108155326A (en) * | 2017-12-22 | 2018-06-12 | 上海恩捷新材料科技股份有限公司 | A kind of collosol coating diaphragm and its preparation method and application |
| CN111286091A (en) * | 2018-12-10 | 2020-06-16 | 江苏金世缘乳胶制品股份有限公司 | Preparation method of high-elasticity low-density natural latex product |
-
2022
- 2022-03-14 CN CN202210244259.5A patent/CN114539602B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB658296A (en) * | 1948-09-18 | 1951-10-03 | Dunlop Rubber Co | Improvements in or relating to the manufacture of microporous sheets of hard rubber |
| GB731935A (en) * | 1951-05-09 | 1955-06-15 | Tudor Ab | Improved method for making microporous separators for electric accumulators and cells |
| US5221587A (en) * | 1991-03-09 | 1993-06-22 | W. R. Grace & Co.-Conn. | Lead/sulphuric acid storage battery |
| CN103311484A (en) * | 2008-09-03 | 2013-09-18 | 三菱树脂株式会社 | Laminated porous film for separator |
| CN102130314A (en) * | 2010-01-12 | 2011-07-20 | 华南师范大学 | Novel PVC/rubber composite micropore partition board |
| CN108155326A (en) * | 2017-12-22 | 2018-06-12 | 上海恩捷新材料科技股份有限公司 | A kind of collosol coating diaphragm and its preparation method and application |
| CN111286091A (en) * | 2018-12-10 | 2020-06-16 | 江苏金世缘乳胶制品股份有限公司 | Preparation method of high-elasticity low-density natural latex product |
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| CN114539602A (en) | 2022-05-27 |
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Address after: 266000 207, No. 97, Kangtai Road, Wangtai sub district office, Huangdao District, Qingdao City, Shandong Province Applicant after: Qingdao Chuanggao Battery Diaphragm Manufacturing Co.,Ltd. Address before: 266000 207, No. 97, Kangtai Road, Wangtai sub district office, Huangdao District, Qingdao City, Shandong Province Applicant before: Qingdao chuanggao battery diaphragm Technology Co.,Ltd. |
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