CN117219959A - AGM separator and preparation method and application thereof - Google Patents
AGM separator and preparation method and application thereof Download PDFInfo
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- CN117219959A CN117219959A CN202311296705.8A CN202311296705A CN117219959A CN 117219959 A CN117219959 A CN 117219959A CN 202311296705 A CN202311296705 A CN 202311296705A CN 117219959 A CN117219959 A CN 117219959A
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Abstract
The invention belongs to the technical field of storage battery accessories, and particularly relates to an AGM separator, a preparation method and application thereof. The AGM separator comprises glass fiber cotton, acid-dipped alkali-free cotton and X, wherein the acid-dipped alkali-free cotton is acid-dipped alkali-free cotton; x is selected from chemical fibers and/or glass chopped filaments. The AGM separator has good comprehensive performance, the strength can reach 1.66KN/m, the extensibility can reach 5.99%, the specific surface area can reach 19.5 square meters per gram, the capillary acid absorption height can reach 128mm within 5min, the compression ratio can reach 76.88%, and the dynamic wet rebound resilience can reach 67.21%.
Description
Technical Field
The invention belongs to the technical field of storage battery accessories, and particularly relates to an AGM separator, a preparation method and application thereof.
Background
At present, an ultrafine glass fiber separator (AGM separator) is commonly used in a valve-regulated lead-acid battery, wherein all the fibers in the AGM separator are ultrafine glass fiber cotton, most of the AGM separator is prepared from fine glass fibers with diameters smaller than 1.2um, coarse glass fibers with diameters between 2um and 11um and a small amount of organic fibers by adopting a wet process, the specific surface area is generally low, the specific surface area is generally between 0.8 square meter/g and 2.0 square meter/g, the specific surface area is low, and the comprehensive performance of the AGM separator is relatively poor.
In the prior art, the specific surface area of the AGM separator can be improved to a certain extent by improving the consumption of the fine glass fibers in the AGM separator, but the fine glass fibers are expensive and have higher cost; and the structure, compressibility and fiber composition of the separator have an important effect on the degree to which the unfilled separator receives electrolyte, and the use of a large number of fine glass fibers, after assembly and compression, can make the filling and forming process more difficult, thereby affecting the separator structure and compressibility.
In addition, the specific surface area can be increased by adding inorganic particles in the AGM separator, such as the Chinese patent CN103855346A and the Chinese patent CN104201319A, which are both prepared by adding silica particles. Currently, there are mainly two methods for silica as an AGM separator additive: the first method is that the fumed silica is prepared by a high-temperature combustion method, the specific surface area is 200 square meters per gram to 400 square meters per gram, but the surface hydroxyl is less, the activity of the silica is poor, the binding force with glass fiber is very small, the fumed silica can only be used as a filler in an AGM separator, and particularly the strength of the separator is reduced after the use amount of the silica exceeds 4%, the powder falling is serious, the specific surface area of the separator is not improved, and the glass fiber is not trapped; the second method is silica produced by precipitation, but has a high impurity content (usually around 90%), a non-uniform particle size, a broad particle size distribution, poor activity, a small specific surface area, and serious agglomeration of silica particles, and unstable network structure between particles and fibers. Therefore, the prepared partition plate has corresponding problems when the traditional fumed silica or the silica prepared by a precipitation method is added into the glass fiber partition plate.
Therefore, it is necessary to develop an AGM separator that can increase the specific surface area without affecting the overall performance.
Disclosure of Invention
In order to solve the above problems, it is an object of the present invention to provide an AGM separator with good overall properties, which comprises acid-impregnated alkali-free cotton and glass fiber cotton, and which has a high specific surface area, strength and elongation of the AGM separator.
In order to achieve the above purpose, the present invention may adopt the following technical scheme:
an AGM separator comprises glass fiber cotton and acid-dipped alkali-free cotton, wherein the acid-dipped alkali-free cotton is acid-dipped alkali-free cotton.
Another object of the present invention is to provide a method for preparing the above AGM separator, which is simple to operate, requires no complicated equipment, and can be mass-produced.
In order to achieve the above purpose, the present invention may adopt the following technical scheme:
the preparation method of the AGM separator comprises the following steps: (1) preparation of acid-dipped alkali-free cotton: the preparation method of the pickling alkali-free cotton comprises the following steps: placing the alkali-free cotton in an acid solution with the concentration of 1mol/L to 4mol/L for pickling treatment, cleaning and drying after the pickling treatment is finished to obtain pickled alkali-free cotton; (2) mixing and pulping: mixing AGM separator raw materials, and pulping to obtain pulping liquid, wherein the concentration of the pulping liquid is 1.5% -2.5%; (3) Regulating alkali and deslagging, diluting the slurry with water to enable the concentration of the slurry to be 0.2-0.4%, and regulating the pH value to be 2.5-3.5; (4) And (3) molding and drying, spreading the slurry on a molding net, carrying out suction filtration and dehydration, and in the process, keeping the water content of the separator to be 60% -80%, and drying to obtain the AGM separator.
It is still another object of the present invention to provide a battery in which the AGM separator described above is used in the battery to improve the service life of the battery.
In order to achieve the above purpose, the present invention may adopt the following technical scheme:
a battery comprising an AGM separator as described above.
The beneficial effects of the invention at least comprise:
(1) According to the AGM separator, the specific surface area is increased by adding the acid-leaching alkali-free cotton, the specific surface area is increased by a method of not increasing the content of fine fibers, and the cost is reduced.
(2) According to the invention, the AGM separator is added with the acid-soaking alkali-free cotton, so that layering of electrolyte is improved, meanwhile, the problems of low wet elasticity and poor assembly pressure and holding capacity of the AGM separator are effectively solved, the pore diameter of the separator is greatly reduced, the short circuit prevention performance caused by dendrite puncture can be further improved, capacity decline of a storage battery is slowed down, and the cycle service life of the storage battery is prolonged.
(3) The combination of the acid-impregnated alkali-free cotton and the chemical fiber in the AGM separator can improve the strength and the dynamic wet rebound resilience of the AGM separator, and the chemical fiber is hydrophobic fiber, so that the oxygen recombination efficiency in a battery can be improved.
(4) According to the invention, the AGM separator is added with the chopped fibers, so that the separator plays a role of a framework, the appearance of the separator is optimized, and meanwhile, the leaching content is low, so that the battery performance is not influenced.
Drawings
FIG. 1 is a diagram of an AGM separator without glass chopped strands;
FIG. 2 is a diagram of an AGM separator with 10% common glass chopped strands;
FIG. 3 is a diagram of an AGM separator plate with 10% (Mount Taishan TCR 105-13-12) glass chopped filaments added;
FIG. 4 is a graph of AGM separator plate with 10% glass chopped strands (Mount Taishan TCR 105-13-12) +8% (PE/PET) sheath-core composite fibers.
Detailed Description
The examples are presented for better illustration of the invention, but the invention is not limited to the examples. Those skilled in the art will appreciate that various modifications and adaptations of the embodiments described above are possible in light of the above teachings and are intended to be within the scope of the invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. Unless the context clearly differs, singular forms of expression include plural forms of expression. As used herein, it is understood that terms such as "comprising," "having," "including," and the like are intended to indicate the presence of features, numbers, operations, materials, or combinations. The terms of the present invention are disclosed in the specification and are not intended to exclude the possibility that one or more other features, numbers, operations, materials or combinations thereof may be present or may be added. As used herein, "/" may be interpreted as "and" or "as appropriate.
The embodiment of the invention provides an AGM separator, which comprises glass fiber cotton and acid-soaked alkali-free cotton, wherein the acid-soaked alkali-free cotton is acid-soaked alkali-free cotton.
The specific surface area of the conventional AGM separator is generally low, generally 0.8-2.0 square meters per gram, and the layering phenomenon of the electrolyte can be improved by increasing the specific surface area. The existing method for improving the specific surface area is to improve the consumption of fine glass fibers in the AGM separator, but the fine glass fibers are expensive and have higher cost, the separator structure, the compression degree and the fiber composition have important influence on the electrolyte receiving degree of the unfilled separator, and the application of a large number of fine glass fibers can make the filling and forming process more difficult after the assembly and compression; the adoption of acid-soaking alkali-free cotton to increase the specific surface area does not adopt a large amount of fine fibers, and the filling of electrolyte caused by too small aperture due to compression assembly is not reduced on the basis of increasing the specific surface area; and a large amount of fine glass fiber cotton is not needed, the price is low, and the molding is realized because the fiber is directly sheet-formed, the binding property is good, the specific surface area is large, and the strength is high.
In some embodiments, the preparation method of the acid-impregnated alkali-free cotton may include: and (3) placing the alkali-free cotton in an acid solution with the concentration of 1 mol/L-4 mol/L for pickling treatment, cleaning and drying after the pickling treatment is finished, so as to obtain the pickling alkali-free cotton. The acidic solution may be a solution such as hydrochloric acid or sulfuric acid. The concentration of the acidic solution may be 1mol/L to 4mol/L. For example, the concentration of the acidic solution may be less than or equal to 1.5mol/L, less than or equal to 2.0mol/L, less than or equal to 2.2mol/L, less than or equal to 2.7mol/L, less than or equal to 3.3mol/L, less than or equal to 3.7mol/L, less than or equal to 3.9mol/L, or a combination of the above ranges; wherein, the pickling effect of the pickling alkali-free cotton is best when the concentration of the acid solution is equal to 2mol/L, and the specific surface area can be improved by at least more than 10 percent compared with other concentrations.
In some embodiments, the preparation method of the acid-impregnated alkali-free cotton may further include: pickling: placing the alkali-free cotton in hydrochloric acid with the concentration of 1 mol/L-4 mol/L at 60-100 ℃ and uniformly stirring for 3-6 hours; cleaning: after pickling, cleaning and filtering with clear water, and vacuum filtering until the outflow cleaning liquid is neutral; and (3) drying: drying for 3-6 hours at 150-200 ℃ until the sample is dried; wherein the pickling temperature can be 70-80 ℃, 75-85 ℃ or 80-90 ℃ and the like; the pickling effect is best when the pickling temperature is 75-85 ℃, and the specific surface area can be increased by at least about 8% compared with other pickling methods.
In some embodiments, the alkali-free cotton may be alkali-free microfiber glass cotton as described in standard JC/T978-2012. Alkali-free microfibrous glass wool (alkali-free wool) has a limit to the content of silica and alkali metal oxides in its components, and AGM separators prepared from alkali-free wool not acid-leached or alkali-free cotton after acid-leaching have a large specific surface area and high strength. For example, the alkali-free cotton component can comprise 50 to 60 percent of SiO 2 、13％～16％Al 2 O 3 、MgO<5.5％、15％～24％CaO、0～0.8％Na 2 O、0～0.4％K 2 O、Fe 2 O 3 <0.5％、5.8％～10％B 2 O 3 And 0.5 to 1.5 percent of TiO 2 ，Na 2 O and K 2 The sum of the content of O is less than 1.2 percent of the total content of the alkali-free cotton. It should be understood that the sum of the mass fractions of the components is less than or equal to 100 percent. In some embodiments, the alkali-free cotton component can comprise 13 to 16 percent of Al 2 O 3 、MgO<5.5％、15％～24％CaO、0～0.8％Na 2 O、0～0.4％K 2 O、Fe 2 O 3 <0.5％、5.8％～10％B 2 O 3 、0.5％～1.5％TiO 2 And the balance of SiO 2 . Specifically, for the above component contents, by controlling SiO 2 The mass content of (2) is 50-60%, and the SiO of the AGM separator in the storage battery can be ensured 2 The content is more than or equal to 98 percent, so that the alkali-free cotton is based on SiO 2 A large number of micropores are formed on the surface of the glass, so that the specific surface area of the microfiber glass can be increased to about 300m 2 /g～400m 2 /g (surface area may be 300.1 m) 2 /g、354.1.m 2 /g or 398.6m 2 /g, etc.). By controlling Na 2 O and K 2 The total content of O is less than 1.2%, so that the reaction degree of the microfiber glass and the acid can be further controlled, the microfiber glass is ensured to completely take the shape of root or line, and the strength of the microfiber glass is maintained. For example, 56% -58% SiO by mass percent 2 、Na 2 O and K 2 The total content of O is less than 0.5%; or 57% SiO by mass percent 2 、Na 2 O and K 2 The total content of O is 0.4%. The alkali-free cotton component can also comprise 13 to 18 percent of Al 2 O 3 、2.5％～4.5％MgO、15％～24％CaO、0～0.5％Na 2 O、0～0.5％K 2 O、0.15％～0.4％Fe 2 O 3 、6％～8.5％B 2 O 3 And 0.5 to 1.5 percent of TiO 2 . As another example, the alkali-free cotton component may also include 17% Al by mass percent 2 O 3 、3.5％MgO、21％CaO、0.2％Na 2 O、0.3％K 2 O and 0.15 to 0.4 percent of Fe 2 O 3 ，6％～8.5％B 2 O 3 And 0.5 to 1.5 percent of TiO 2 Other components or unavoidable impurities that are known in the art.
In some embodiments, the alkali-free cotton may have an average diameter of 0.1 μm to 5 μm. For example, the alkali-free cotton may have an average diameter of 0.2 μm to 4 μm, 0.5 μm to 3.5 μm, 0.8 μm to 3.2 μm, 1.2 μm to 2.9 μm, 1.5 μm to 2.9 μm, 1.9 μm to 2.5 μm, 2.1 μm to 2.3 μm or a combination of the above ranges.
In some embodiments, the mass of the acid-impregnated alkali-free cotton in the AGM separator described above is 15% -30%, such as 18%, 20%, 22%, 25% or 28%.
In addition, the AGM separator further comprises X, wherein X is selected from chemical fibers and/or glass chopped filaments.
In some embodiments, when X is selected from chemical fibers, the weight of the acid-impregnated alkali-free cotton may comprise 15% to 30%, such as 15%, 20%, 30%, etc., of the weight of the AGM separator; the chemical fiber may comprise 4% to 20% by weight of the AGM separator, such as 4%, 8%, 15% or 20% by weight; the balance being glass fiber cotton. The optimal combination is that the weight of the acid-soaking alkali-free cotton accounts for 20 percent, the weight of the chemical fiber content accounts for 8 percent, and the balance is high alkali or medium alkali glass fiber cotton. This is because increasing the chemical fiber content can increase the mechanical strength of the battery separator, but the chemical fibers are hydrophobic fibers, and excessive chemical fibers can reduce the absorption of sulfuric acid solution by the separator, reducing the performance of the valve regulated lead acid battery. The weight ratio of the acid-dipped alkali-free cotton to the chemical fiber has an influence on the performance of the prepared AGM separator.
On the basis of adding the acid-leaching alkali-free cotton, the chemical fiber is added to improve the comprehensive performance of the AGM separator, such as the strength, the dynamic wet rebound resilience and the like of the AGM separator; in addition, on the basis of adding acid-soaking alkali-free cotton, the appearance flatness of the AGM separator can be improved by adding the glass chopped filaments. The alkali-free cotton is subjected to pickling treatment, the specific surface area is greatly increased, but the alkali-free cotton subjected to pickling has nano micropores on the surface of the fiber after ion leaching, so that the strength is reduced, the strength of the separator can be improved by increasing chemical fibers, the acid absorption performance of the battery separator can be affected by adding the chemical fibers, the separator prepared from the alkali-free cotton subjected to pickling has large specific surface area and strong capillary acid absorption capacity in the acid absorption process, the defect of adding the chemical fibers is overcome, and the manufactured battery separator has high strength and unaffected acid absorption performance.
In some embodiments, when X is selected from the group consisting of glass chopped strands, the weight of the acid-impregnated alkali-free cotton may comprise 15% to 30%, such as 15%, 20%, 30%, etc., of the weight of the AGM separator; the weight of the glass chopped filaments can be 8% -15% of the weight of the AGM separator, such as 8%, 10%, 15% and the like; the balance being glass fiber cotton. The optimal combination is that the weight of the acid-immersed alkali-free cotton accounts for 20 percent, the weight of the chopped strand content accounts for 10 percent, and the balance is micro glass fiber cotton. The addition of chopped filament acts as the skeleton effect in AGM baffle, improves the fashioned roughness of AGM baffle, promotes partial intensity simultaneously, but too high can reduce AGM's acid absorption performance and elasticity to influence valve accuse type lead acid battery's life.
In some embodiments, when X is selected from the group consisting of chemical fibers and glass chopped strands, the weight of the acid-impregnated alkali-free cotton may comprise 15% to 30%, such as 15%, 20%, 30%, etc., of the weight of the AGM separator; the chemical fiber may comprise 4% to 20% by weight of the AGM separator, such as 4%, 8%, 15% or 20% by weight; the glass chopped filaments can account for 8% -15% of the weight of the AGM separator, such as 8%, 10%, 15% and the like; the balance being glass fiber cotton. The AGM separator prepared by the above four substances in different proportions has different properties, wherein 62% of glass fiber cotton, 20% of acid-dipped alkali-free cotton, 10% of chopped fibers and 8% of chemical fibers are preferable, and the prepared AGM separator has high strength, good mechanical property, large specific surface area, high capillary acid absorption height and best comprehensive properties.
On the basis of adding acid-soaking alkali-free cotton, the strength and the elongation of the AGM separator can be increased by adding chemical fibers and glass chopped fibers, so that the separator is not damaged under industrial production, the puncture resistance of the separator can be improved, and short circuit of a battery caused by the penetration of dendrites in the separator is avoided.
The strength of the separator is mainly derived from friction force generated by contact between fibers; after the glass fiber separator absorbs electrolyte sulfuric acid, contact points among fibers are soaked, so that the strength of the separator is reduced, the separator is relaxed and contracted, and is expanded and compressed by the polar plates, so that the pressure of a polar group is reduced, and the service life of a battery is shortened; in the invention, the chemical fiber and the glass chopped strand are added into the pure glass fiber, so that the problems are overcome to a great extent. In addition, the glass chopped fibers play a role of a framework in the partition board, have high strength, strong acid resistance and large diameter, and are convenient for lap joint formation of fine fibers on the framework. For chemical fibers, particularly the added composite fibers are bicomponent fibers, for example, the inner layer is high-temperature-resistant polyethylene terephthalate (PET), the outer layer is Polyethylene (PE) with lower melting point, when the PE/PET sheath-core composite fibers are treated at the high temperature of 150 ℃, the polyethylene layer of the outer layer of the PE/PET sheath-core composite fibers is melted, and the PET of the inner layer is not melted and deformed, so that the supporting effect is realized; when the separator is cooled to room temperature or the working temperature of the battery, the melted polyethylene can bond the surrounding glass fibers together, so that the glass fibers cannot move freely after being soaked, and the functions of enhancing the tensile strength and the rebound rate of the separator are achieved.
In some embodiments, in the AGM separator described above, the chemical fiber can be a monocomponent fiber, and the monocomponent fiber can have a melting point below 180 ℃; or the chemical fiber can be a bicomponent fiber, wherein the fiber melting point of one component is lower than 180 ℃ and the fiber melting point of the other component is higher than 200 ℃; so that the monocomponent fiber can be partially melted when the AGM separator is dried at 150-180 ℃ to bond the glass fiber together, and the strength is improved; for the bicomponent fiber, the outer layer fiber is melted and bonded with the glass fiber, and the inner layer fiber is not melted to play a supporting role.
In some embodiments, the chemical fiber may be selected from one of sheath-core type fiber (such as PE/PP, PE/PET or PET/PET with different components), side-by-side type fiber, island-in-sea type fiber, orange-peel type fiber or polymer fiber; the polymer fibers comprise one or more combinations of substituted polymers, unsubstituted polymers, saturated polymers, unsaturated polymers (e.g., aromatic polymers), organic polymers, inorganic polymers, linear polymers, branched polymers, homopolymers, or copolymers; specifically, the polymer fibers include polyolefins (such as polyethylene, polypropylene, or polybutylene), polyesters (such as polyethylene terephthalate), polyamides (such as nylon or aromatic polyamides), halogenated polymers (such as polytetrafluoroethylene), and combinations thereof.
The glass fiber cotton is bonded by the action of the chemical fiber, so that the glass fiber cotton is prevented from slipping, has a supporting function, has a hydrophobic property, improves the oxygen recombination efficiency, has a small content of the added chemical fiber, and does not change the pore diameter structure. For example, the PE/PET sheath-core composite fiber with high strength and hydrophobicity can increase the rebound rate of the separator, enhance the tensile strength and improve the oxygen recombination efficiency; the PE/PET sheath-core composite fiber is a rod-shaped fiber with a core-shell structure, and the PE and the PET have stable physical and chemical properties and have melting point difference; the outer layer is a PE layer, has a low melting point and is made of a hydrophobic material; the inner layer is of a PET nuclear structure, and has higher melting point and higher hardness; the outer layer is melted when the treatment is carried out at the high temperature of about 150 ℃ and the glass fiber nearby is bonded; the inner layer structure is unchanged, and the support function is achieved, so that the strength and rebound resilience of the partition plate are improved. In addition, the support fiber PET can increase the gas channel in the separator, so that the oxygen recombination efficiency is improved; because the battery is rich in liquid, the pure glass fiber separator is fully saturated, and the gas channel is basically fully blocked by the electrolyte, the oxygen recombination efficiency is very low; when the acid filling amount is the same, the acid filling speed of the battery assembled by the mixed separator added with the hydrophobic fibers is about 22 percent faster than that of the battery assembled by the AGM separator, the battery capacity is improved by about 2.5 percent, and the service life of the battery is obviously prolonged.
In some embodiments, the average diameter of the glass chopped strands may be 5 μm to 15 μm and the average length may be 6mm to 25mm. For example, the average diameter of the glass chopped strands may be in the range of 6 μm to 12 μm, 8 μm to 12 μm, 7 μm to 13 μm, 9 μm to 13 μm or a combination thereof; the average length may be 7mm to 20mm, 8mm to 19mm, 8mm to 22mm, 9mm to 23mm, or a combination of the above ranges. Too thick short shreds overlap joint with glass fiber or overlap joint with the short shreds of itself can cause the aperture too big, can cause dendrite that positive negative pole formed to pass and cause the short circuit in AGM use, also easily form the inside concentration gradient of battery to influence life-span. The short shreds are too thin to play a small or no role of a framework, are unfavorable for forming, and have poor surface quality of the AGM partition board. The short shreds are too long to be wound in the partition plate, so that the short shreds have unobvious supporting effect and cannot have an effect.
In some specific embodiments, the glass chopped strand component can comprise 58-62% of SiO by mass percent 2 、11％～15％Al 2 O 3 、20％～24％CaO、1％～5％MgO、0.2％～1.5％TiO 2 、0～0.8％R 2 O and 0.1 to 0.6 percent of Fe 2 O 3 Wherein R is 2 O is other oxide impurity. It should be understood that the sum of the mass fractions of the components is less than or equal to 100 percent. In some specific embodiments, the composition may include 11% -15% Al by mass 2 O 3 、20％～24％CaO、1％～5％MgO、0.2％～1.5％TiO 2 、0～0.8％R 2 O、0.1％～0.6％Fe 2 O 3 And the balance of SiO 2 . It is also to be noted that the glass chopped fibers of the components have good acid resistance, and in sulfuric acid solution, fe is less than or equal to 50ppm, cu is less than or equal to 1ppm, co is less than or equal to 1ppm and Cr is less than or equal to 1ppm. The purpose of ion precipitation limitation is to: the micro-battery is prevented from being formed in the lead-acid storage battery, so that the self-discharge process in the battery is avoided, the loss of active substances of a battery polar plate is caused, and the service life of the lead-acid storage battery is influenced; fe (Fe) 2+ 、Fe 3+ At the positive electrode, the chemical reactions of the microbatteries formed at the negative electrode are respectively:
PbO 2 +3H + +HSO 4 - +2Fe 2+ —PbSO 4 +2H 2 O+2Fe 3+ ；Pb+HSO4 - +2Fe 3+ —PbSO 4 +H + +2Fe 2+ in the reaction, the active substances of the anode and the cathode are continuously reduced and oxidized to generate compact PbSO 4 Crystallization results in a decrease in battery capacity until the end of life.
In another aspect, the present invention provides a method for preparing the three AGM separators, which comprises: (1) preparation of acid-dipped alkali-free cotton: the preparation method of the pickling alkali-free cotton comprises the following steps: placing the alkali-free cotton in an acid solution with the concentration of 1mol/L to 4mol/L for pickling treatment, cleaning and drying after the pickling treatment is finished to obtain pickled alkali-free cotton; (2) mixing and pulping: mixing the three AGM separator raw materials and pulping to obtain pulping liquid, wherein the concentration of the pulping liquid is 1.5% -2.5%; (3) Regulating alkali and deslagging, diluting the slurry with water to enable the concentration of the slurry to be 0.2-0.4%, and regulating the pH value to be 2.5-3.5; (4) And (3) molding and drying, spreading the slurry on a molding net, carrying out suction filtration and dehydration, and in the process, keeping the water content of the separator to be 60% -80%, and drying to obtain the AGM separator. The method comprises the following steps:
the first technical scheme is as follows: when the AGM separator comprises glass fiber cotton and acid-impregnated alkali-free cotton, the preparation method comprises the following steps: pulping glass fiber cotton and acid-soaked alkali-free cotton to obtain pulping liquid; regulating pH to 2.5-3.5, and removing residues to obtain slurry; spreading the slurry on a forming net, carrying out suction filtration and dehydration, controlling the water content to be 60% -80%, and drying to obtain the AGM separator.
The second technical scheme is as follows: when the AGM separator includes glass fiber wool, acid-impregnated alkali-free cotton and chemical fiber, the method of preparing the same includes: pulping glass fiber cotton, acid-soaked alkali-free cotton and chemical fibers to obtain pulping liquid; regulating pH to 2.5-3.5, and removing residues to obtain slurry; spreading the slurry on a forming net, carrying out suction filtration and dehydration, controlling the water content to be 60% -80%, and drying to obtain the AGM separator.
The third technical scheme is as follows: and replacing chemical fibers in the raw materials of the AGM separator in the second technical scheme with glass chopped filaments to prepare the AGM separator.
The fourth technical scheme is as follows: and replacing the chemical fibers in the raw materials of the AGM separator in the second technical scheme with the combination of the chemical fibers and the glass chopped filaments to prepare the AGM separator.
The drying may include drying at 130-150 deg.c for 3-5 min to set the separator, drying at 150-200 deg.c for 5-10 min and eliminating excessive water from the separator.
A further embodiment of the invention provides a battery comprising an AGM separator as described above. The AGM separator described above can be used in a battery to improve the service life.
For a better understanding of the present invention, the content of the present invention is further elucidated below in connection with the specific examples, but the content of the present invention is not limited to the examples below.
1. Preparation of acid-soaked alkali-free cotton
First, preparation of acid-leaching alkali-free cotton
(1) Pickling: putting the alkali-free cotton into 2mol/L hydrochloric acid, uniformly stirring for 4 hours at 80 ℃, wherein the alkali-free cotton comprises 14.1% of Al by mass percent 2 O 3 、3.6％MgO、20.6％CaO、Na 2 O<0.001％、0.3％K 2 O、0.3％Fe 2 O 3 、7.0％B 2 O 3 、0.6％TiO 2 And the balance of SiO 2 。
(2) Cleaning: after pickling, cleaning with clear water, and vacuum filtering until the outflow cleaning liquid is neutral;
(3) And (3) drying: oven dried for 6 hours at 177 ℃ until the sample was completely oven dried.
(4) The pickling alkali-free cotton is prepared from the following components in percentage by mass: 0.2% Al 2 O 3 、0.02％MgO、CaO<0.001％、Na 2 O<0.001％、0.001％K 2 O、0.001％Fe 2 O 3 、0.2％B 2 O 3 、0.4％TiO 2 And the balance of SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The specific surface area of the obtained acid-impregnated alkali-free cotton is 398.6m 2 /g。
(II) preparation of second acid-leaching alkali-free cotton
(1) Pickling: putting the alkali-free cotton into 2mol/L hydrochloric acid, and uniformly stirring for 4 hours at 80 ℃, wherein the alkali-free cotton comprises 14.3% of Al by mass percent 2 O 3 、3.7％MgO、20.9％CaO、Na 2 O<0.001％、0.4％K 2 O、0.3％Fe 2 O 3 、7.4％B 2 O 3 And 0.6% TiO 2 And the balance of SiO 2 ；
(2) Cleaning: after pickling, cleaning with clear water, and vacuum filtering until the outflow cleaning liquid is neutral;
(3) And (3) drying: drying for 6 hours at 177 ℃ until the sample is dried;
(4) The pickling alkali-free cotton is prepared from the following components in percentage by mass: 0.4% Al 2 O 3 、0.04％MgO、CaO<0.001％、Na 2 O<0.001％、0.001％K 2 O、0.001％Fe 2 O 3 、0.4％B 2 O 3 、0.8％TiO 2 And the balance of SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The specific surface area of the obtained acid-impregnated alkali-free cotton is 300.1m 2 /g。
(III) preparation of third acid-leaching alkali-free cotton
(1) Pickling: putting the alkali-free cotton into 2mol/L hydrochloric acid, and uniformly stirring for 4 hours at 80 ℃, wherein the alkali-free cotton comprises 14.2% of Al by mass percent 2 O 3 、3.6％MgO、20.7％CaO、Na 2 O<0.001％、0.3％K 2 O、0.3％Fe 2 O 3 、7.2％B 2 O 3 And 0.6% TiO 2 And the balance of SiO 2 ；
(2) Cleaning: after pickling, cleaning with clear water, and vacuum filtering until the outflow cleaning liquid is neutral;
(3) And (3) drying: drying for 6 hours at 177 ℃ until the sample is dried;
(4) The pickling alkali-free cotton is prepared from the following components in percentage by mass: 0.3% Al 2 O 3 、0.03％MgO、CaO<0.001％、Na 2 O<0.001％、0.001％K 2 O、0.001％Fe 2 O 3 、0.3％B 2 O 3 、0.6％TiO 2 And the balance of SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The specific surface area of the obtained acid-impregnated alkali-free cotton is 354.1m 2 /g。
(IV) composition of common alkali-free cotton
The alkali-free cotton comprises 14.2% of Al by mass percent 2 O 3 、3.6％MgO、20.7％CaO、Na 2 O<0.001％、0.3％K 2 O、0.3％Fe 2 O 3 、7.2％B 2 O 3 And 0.6% TiO 2 And the balance of SiO 2 The specific surface area of the alkali-free cotton is 1.2m 2 /g。
2. AGM separator preparation and performance testing
In the following examples, the CA glass wool component comprises 2.4% Al by mass 2 O 3 、2.8％MgO、6.4％CaO、15.4％Na 2 O、0.8％K 2 O、0.1％Fe 2 O 3 、5.5％B 2 O 3 And 0.1% TiO 2 The balance of SiO 2 。
In the following examples, the length of the Mount Taishan TCR105-13-12 and the length of the common glass chopped strands are 10mm, and the average diameter is 12 μm; the ingredients of the common glass chopped strands and the Taishan TCR105-13-12 are shown in Table 1; the common glass chopped strands and the ion precipitation content of the Taishan TCR105-13-12 were tested by referring to the test method of BCI-03A-2015AGM Technical Manual Testing Methods and are shown in Table 2.
TABLE 1 different glass chopped strand compositions
TABLE 2 ion precipitation content (ppm) of various glass chopped strands
In the following examples, the preparation of AGM separators was performed according to the following procedure:
(1) Adding a proper amount of water into a beating machine, keeping the concentration of the slurry at 2%, adjusting the pH value to 2, and then adding all the raw materials for mixing and beating to obtain slurry; and (2) size mixing and deslagging: diluting the slurry with water to make the concentration of the slurry be 0.3%, adjusting the pH value to be 2.5, and then carrying out deslagging treatment to obtain the slurry;
(3) And (3) forming: spreading the slurry on a forming net, and carrying out negative pressure suction filtration and dehydration on the slurry to obtain a wet separator, wherein the water content of the separator is kept at 67%;
(4) And (3) drying: drying the wet separator at 150 ℃ for 3 minutes to shape the separator, drying at 200 ℃ for 5 minutes, and removing excessive water in the separator to obtain a dry separator;
(5) And (3) a finished product: and (5) coiling and cutting to obtain the AGM separator.
In the following examples, AGM separators were prepared by measuring their gram weight (g/. Square meter), strength (KN/m), elongation (%), specific surface area (square meter/g), capillary acid absorption height (mm) for 5min, compression ratio (%) and dynamic wet resilience (%) with reference to "BCI-03A-2015 AGM Technical Manual Testing Methods".
In the examples below, the first refers to the first type of acid-impregnated alkali-free cotton prepared as described above, the second refers to the second type of acid-impregnated alkali-free cotton prepared as described above, and the third refers to the third type of acid-impregnated alkali-free cotton prepared as described above.
AGM separator prepared from acid-impregnated alkali-free cotton with different contents
Based on the raw materials shown in table 3 below, different AGM separators were prepared according to the above-described preparation method of AGM separators.
Table 3 ratio of different content acid-impregnated alkali-free cotton
The prepared different AGM separators were respectively tested for gram weight (g/square meter), strength (KN/m), elongation (%), specific surface area (square meter/g), capillary acid absorption height (mm) for 5min, compression ratio (%) and dynamic wet resilience (%) according to the above-mentioned test methods, and the results are shown in Table 4 below. Oxygen recombination efficiency test (%), mrhaJ, mickaK, jindraJ, etal Oxygencycleinsealediead acidbatteries (J) jpowersource.
TABLE 4 Performance test conditions of AGM separators prepared from acid-and alkali-free cottons having different contents
As can be seen from table 4 above, according to comparison of comparative example 1 and examples 1, 2, 3, the addition of the acid-impregnated alkali-free cotton greatly increases the specific surface area, the specific surface area of the sample is large, and the capillary acid absorption force in the acid absorption process is strong, so that the layering phenomenon of the electrolyte is improved, the burning-through phenomenon of the separator caused by uneven electrolyte is improved, and the service life of the AGM separator is prolonged; although the acid absorption performance of the separator is improved along with the increase of the content of the acid-soaked alkali-free cotton, the cost is increased along with the increase of the content of the alkali-free cotton, so that the content of the alkali-free cotton is controlled to be 15-30%.
(II) preparing AGM separator by using chemical fiber with different contents and acid-leaching alkali-free cotton
Based on the raw materials shown in table 5 below, different AGM separators were prepared according to the above-described preparation method of AGM separators.
Table 5 chemical fibers with different contents + alkali-free cotton ratio of pickling
The prepared different AGM separators were respectively tested for gram weight (g/square meter), strength (KN/m), elongation (%), specific surface area (square meter/g), capillary acid absorption height (mm) for 5min, compression ratio (%) and dynamic wet resilience (%) according to the above-mentioned test methods, and the results are shown in Table 6 below.
TABLE 6 Performance test conditions of AGM separators prepared with different content of chemical fibers+acid-and alkali-free cotton
In table 6 above, it can be seen from comparative examples 6 and 2 that the addition of the bi-component chemical fiber can improve the strength of the AGM separator and greatly improve the performance such as dynamic wet resilience, but the addition of the chemical fiber can reduce the capillary acid absorption height of the separator; as seen in examples 6, 7, 8 and 9, as the content of the chemical fiber increases, the mechanical properties of the separator are improved but the acid absorption performance is lowered; comparing the comprehensive performance, the ratio of chemical fiber with 8 percent (example 7) to other components gives the AGM separator with optimal comprehensive performance.
(III) preparing AGM separator by using glass chopped filaments and acid-pickling alkali-free cotton with different contents
Based on the raw materials shown in table 7 below, different AGM separators were prepared according to the above-described preparation method of AGM separators.
Table 7 ratio of glass chopped strands to acid-impregnated alkali-free cotton with different contents
| Examples | CA glass fiber cotton | Acid-soaked alkali-free cotton | Glass chopped strand |
| Example 2 | 80％ | 20% (third kind) | - |
| Example 10 | 72％ | 20% (third kind) | 8% (Tai TCR 105-13-12) |
| Example 11 | 70％ | 20% (third kind) | 10% (Tai TCR 105-13-12) |
| Example 12 | 65％ | 20% (third kind) | 15% (Tai TCR 105-13-12) |
| Comparative example 3 | 70％ | 20% (third kind) | 10% common glass chopped strand |
The prepared different AGM separators were respectively tested for gram weight (g/square meter), strength (KN/m), elongation (%), specific surface area (square meter/g), capillary acid absorption height (mm) for 5min, compression ratio (%) and dynamic wet resilience (%) according to the above-mentioned test methods, and the results are shown in Table 8 below.
TABLE 8 Performance test cases of different AGM separators
In Table 8 above, it can be seen from comparative examples 2 and 10 that the addition of chopped glass fibers slightly improves the strength of the separator and the performance of the separator, but also reduces the acid absorption of the separator, and the 10% (example 11) content performance is optimal. According to comparative example 3 and example 11, the Mount Taishan TCR105-13-12 glass chopped fibers have good acid resistance and low ion precipitation, so that micro batteries are prevented from being formed in the lead-acid storage battery, self-discharge process in the battery is caused, loss of active substances of battery plates is caused, and the service life of the lead-acid storage battery is influenced.
In addition, the appearance flatness of the AGM separator prepared by adding glass chopped filaments is improved to a certain extent, and specific reference is made to FIGS. 1, 2 and 3, wherein FIG. 1 is an AGM separator graph without glass chopped filaments (example 2), FIG. 2 is an AGM separator graph with 10% common glass chopped filaments (comparative example 3), and FIG. 3 is an AGM separator graph with 10% Taishan TCR105-13-12 glass chopped filaments; it is apparent that the flatness of fig. 2 and 3 is significantly better than that of fig. 1.
(IV) preparing AGM separator by different types of chemical fibers, glass chopped filaments and acid-leaching alkali-free cotton
Table 9 different types of chemical fibers + chopped strands + acid-impregnated alkali-free cotton blends
The prepared different AGM separators were respectively tested for gram weight (g/square meter), strength (KN/m), elongation (%), specific surface area (square meter/g), capillary acid absorption height (mm) for 5min, compression ratio (%) and dynamic wet resilience (%) according to the above-mentioned test methods, and the results are shown in Table 10 below.
TABLE 10 Performance test cases of different AGM separators
As can be seen from the above table 10, according to examples 7, 11 and 13, the separator prepared from chemical fiber, glass chopped strands, acid-free alkali cotton and CA glass fiber cotton has high single performance strength, large compression ratio, good dynamic wet resilience performance, good capillary acid absorption height performance and smooth appearance; of these, example 13 had the best overall performance; FIG. 4 is a drawing showing the AGM separator prepared in example 13.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, 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 and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (14)
1. An AGM separator is characterized by comprising glass fiber cotton and acid-soaked alkali-free cotton, wherein the acid-soaked alkali-free cotton is acid-soaked alkali-free cotton.
2. AGM separator according to claim 1 wherein the specific surface area of the acid-impregnated alkali-free cotton is 300m 2 /g～400m 2 /g。
3. The AGM separator according to any one of claims 1 or 2, wherein the mass of the acid-impregnated alkali-free cotton is 15% to 30%.
4. The AGM separator according to any one of claims 1 or 2, further comprising chemical fibers.
5. The AGM separator according to claim 4, wherein the acid-impregnated alkali-free cotton comprises 15% to 30% by weight of the AGM separator, the chemical fiber comprises 4% to 20% by weight of the AGM separator, and the balance is glass fiber cotton.
6. The AGM separator according to any one of claims 1 or 2, further comprising glass chopped strands.
7. The AGM separator according to claim 6 wherein the weight of the acid-impregnated alkali-free cotton is 15% to 30% of the weight of the AGM separator, the weight of the glass chopped strands is 8% to 15% of the weight of the AGM separator, and the balance is glass fiber cotton.
8. The AGM separator according to any one of claims 1 or 2, further comprising chemical fibers and glass chopped filaments.
9. The AGM separator according to claim 8 wherein the acid-impregnated alkali-free cotton comprises 15% to 30% by weight of the AGM separator, the chemical fiber comprises 4% to 20% by weight of the AGM separator, the glass chopped strands comprise 8% to 15% by weight of the AGM separator, and the balance glass fiber wool.
10. An AGM separator according to claim 5 or 9, wherein the chemical fibre is a bicomponent fibre, one component having a fibre melting point below 180 ℃ and the other component having a fibre melting point above 200 ℃.
11. AGM separator according to claim 10 wherein the bicomponent fibres are preferably PET/PET, PP/PET, PE/PET or PE/PP.
12. AGM separator according to claim 7 or 9 wherein the glass chopped strand composition comprises 58% to 62% SiO 2 、11％～15％Al 2 O 3 、20％～24％CaO、1％～5％MgO、0.2％～1.5％TiO 2 、0～0.8％R 2 O and 0.1 to 0.6 percent of Fe 2 O 3 Wherein R is 2 O is other oxide impurity.
13. The method of manufacturing an AGM separator according to any one of claims 1 to 12, comprising:
(1) Preparing acid-dipped alkali-free cotton: the preparation method of the pickling alkali-free cotton comprises the following steps: placing the alkali-free cotton in an acid solution with the concentration of 1mol/L to 4mol/L for pickling treatment, cleaning and drying after the pickling treatment is finished to obtain pickled alkali-free cotton;
(2) Mixing and pulping: mixing AGM separator raw materials, and pulping to obtain pulping liquid, wherein the concentration of the pulping liquid is 1.5% -2.5%;
(3) Regulating alkali and deslagging, diluting the slurry with water to enable the concentration of the slurry to be 0.2-0.4%, and regulating the pH value to be 2.5-3.5;
(4) And (3) molding and drying, spreading the slurry on a molding net, carrying out suction filtration and dehydration, and in the process, keeping the water content of the separator to be 60% -80%, and drying to obtain the AGM separator.
14. Battery, characterized by comprising an AGM separator according to any of claims 1 to 12.
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