CN106981609B - Lead storage battery separator and lead storage battery - Google Patents
Lead storage battery separator and lead storage battery Download PDFInfo
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- CN106981609B CN106981609B CN201710188095.8A CN201710188095A CN106981609B CN 106981609 B CN106981609 B CN 106981609B CN 201710188095 A CN201710188095 A CN 201710188095A CN 106981609 B CN106981609 B CN 106981609B
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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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
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- 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
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Abstract
The invention discloses a lead storage battery separator and a lead storage battery, wherein the lead storage battery separator comprises glass fiber and COPET sea island filament, wherein the COPET sea island filament is obtained by dissolving PA/COPET sea island fiber in the sea. The COPET sea-island filament is added during the preparation of the lead storage battery separator, and is obtained by carrying out sea-dissolving treatment on PA/COPET sea-island fibers. After the sea island fiber is separated, the filament number is fine, which can not be realized by the conventional spinning, so that the sea island fiber has the characteristics which can not be realized by the common fiber. Compared with the common AGM separator, the lead storage battery separator has the advantages of high acid absorption, high durable pressure, high tensile breaking strength and the like, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of lead storage battery production, in particular to a lead storage battery separator and a lead storage battery.
Background
Lead storage batteries have a history of over 150 years now and have a wide range of applications. In recent years, electric vehicles have been rapidly developed in China by virtue of their better mobility, lower storage space requirements and excellent price advantages, and the storage battery industry has also been rapidly developed.
The lead accumulator consists of positive and negative plates, partition, casing, electrolyte and poles. The separator in the lead storage battery not only plays a role of separating a positive plate from a negative plate, but also is required to have the characteristics of high porosity, small aperture, strong oxidation resistance, capability of absorbing and maintaining sufficient electrolyte, good compression resilience and the like. If the aperture of the separator of the lead storage battery is too large, lead dendrite of a polar plate of the storage battery is easy to penetrate through the separator to cause short circuit of the battery, the assembly pressure of the lead storage battery after charging and discharging for a period of time is too low to fail due to poor compression resilience of the separator, and the lead storage battery is lack of acid and fails in the circulation process due to poor acid absorption of the separator. The separators of lead storage batteries are currently basically AGM separators, the main component of which is glass fibers. Because the glass fiber is randomly extracted by a flame method, the fineness and the length of the fiber are different, and the thinnest glass fiber can be made to be 0.8-1.59 mu m at present, the prepared glass fiber separator has larger maximum aperture, uneven aperture distribution and poor compression resilience.
In order to make the performance of the AGM separator more excellent, additives are generally added to the AGM separator. Such as:
the Chinese patent with the publication number of CN103855346B discloses an AGM separator of a storage battery and a preparation method thereof, wherein the AGM separator of the storage battery comprises high-alkali glass wool, medium-alkali glass fiber, bi-component polyester fiber and SiO-containing glass fiber2A glue of particles, the high alkali glass wool, the medium alkali glass fiber, the bi-component polyester fiber, the glue containing SiO2The weight percentage of the glue of the particles is 81-87: 2.8-4.6: 1.8-3.7: 8.3-11.4.
The invention discloses a lead-acid storage battery separator and a preparation method thereof, wherein the separator takes glass fiber as a main component and also comprises 10-20% of polyolefin resin fiber with the melting point of 100-200 ℃.
Chinese patent publication No. CN104852002A discloses a lead-acid battery separator, which comprises 85-95% by mass of superfine glass fiber, 4-10% by mass of polyester fiber, and 1-5% by mass of acetate fiber. The preparation method comprises the steps of pulping the superfine glass fiber for 5-10 minutes, adding the polyester fiber and the acetate fiber, pulping for 8-12 minutes, forming and sheet making, entering a drying system at a constant speed, drying at the temperature of 160-250 ℃, rolling and slitting.
Sea-island fibers are a substance in which one polymer is dispersed in another polymer, the dispersed phase being in the state of "islands" in the fiber section, and the matrix corresponding to "sea", and it is seen from the fiber cross section that one component is surrounded by the other component in a finely dispersed state as if there are many islands in the sea. The island and sea components are distributed continuously, densely and uniformly in the axial direction of the fiber. In the production process, it has the fineness of conventional fiber, but the sea component is dissolved away by using a solvent, so that the superfine fiber bundle in a bundle shape can be obtained. According to the general classification of the fiber, after the sea-island fiber is separated, the filament number is only 0.005D, the fiber belongs to superfine fiber, the conventional spinning can not be carried out, and therefore, the fiber has the characteristics which can not be carried out by the general fiber. The sea-island fiber has unique performance, and has the advantages of good acid resistance, good crimp resilience, good capillary wicking effect and the like.
Disclosure of Invention
The invention provides a lead storage battery separator with small pore diameter, high acid absorption, high durable pressure and high tensile breaking strength, aiming at the problems of large maximum pore diameter, uneven pore diameter distribution and poor compression resilience of an AGM separator in the prior art.
The lead storage battery separator comprises glass fibers and COPET sea-island filaments, wherein the COPET sea-island filaments are obtained by carrying out sea-dissolving treatment on PA/COPET sea-island fibers. The PA/COPET sea-island fiber is sea-island fiber with Polyamide (PA) as the sea component and modified polyester (COPET) as the island component, wherein the PA as the sea component is dissolved to obtain bunched superfine fiber bundles, namely COPET sea-island filament.
Preferably, the specification of the PA/COPET sea-island fiber is as follows: the linear density is 0.6 to 0.7dtex, 40 to 80 islands per root. The linear density is an index for describing the thickness of the fiber, generally expressed by the mass of the fiber under a certain length, the unit is g/km, the unit commonly used for the fiber is tex (tex), the important gram number of the fiber with the length of 1000 meters in the official moisture regain is shown, and one tenth of tex is decitex (dtex); denier (D) is also a commonly used unit to characterize the linear density of a fiber, which represents how many grams, i.e., denier, of the weight of a 9000 meter length of fiber. In a sea-island fiber, a sea component surrounds several tens of islands, and after dissolving the sea, the sea component is removed, and the islands are dispersed, for example, 40 islands of PA/COPET sea-island fiber, and then 40 islands of sea component are present in the middle of the sea component of one sea-island fiber, and after dissolving the sea, the 40 islands are dispersed to form 40 COPET sea-island filaments.
Preferably, the mass percentage content of the COPET sea island filament is 5-25%.
More preferably, the mass percentage content of the COPET sea island filament is 15-25%.
Preferably, the fineness of the COPET sea island filament is 0.005-0.01D.
Further preferably, the fineness of the COPET sea island filament is 0.008-0.01D.
Preferably, the fineness of the glass fiber is 29 to 35 °. The fineness of the glass fiber is generally characterized by a unit of degree, the fiber fineness of the 29-degree glass fiber is about 2.083um, and the fiber fineness of the 35-degree glass fiber is about 1.065 um.
Preferably, the preparation method of the COPET sea island filament comprises the following steps: the method comprises the steps of immersing PA/COPET sea-island fiber into a sulfuric acid solution with the mass concentration of 10% -15%, stirring for 20 minutes, and dissolving sea components to obtain the COPET sea-island filament.
Preferably, the method for preparing the lead storage battery separator comprises the following steps: mixing the COPET sea island filaments and the glass fibers in proportion, adding water to prepare slurry, and carrying out wet forming and drying to prepare the separator.
The invention also provides a lead storage battery prepared by using the lead storage battery separator.
The COPET sea-island filament is added during the preparation of the lead storage battery separator, and is obtained by carrying out sea-dissolving treatment on PA/COPET sea-island fibers. After the sea island fiber is separated, the filament number is fine, which can not be realized by the conventional spinning, so that the sea island fiber has the characteristics which can not be realized by the common fiber. Compared with the common AGM separator, the lead storage battery separator has the advantages of high acid absorption, high durable pressure, high tensile breaking strength and the like, and has good application prospect.
Drawings
FIG. 1 is a graph showing the results of measurement of the liquid absorption amount in example 5.
FIG. 2 is a graph showing the endurance pressure test results in example 6.
FIG. 3 is a graph showing the results of measurement of tensile rupture strength in example 7.
Detailed Description
PA/COPET sea-island fibers of various specifications: purchased from Jiangsu instrumented chemical fiber GmbH;
glass fiber: from Shenyang Dongshong glass fibers, Inc.
Example 1
Weighing 15kg of PA/COPET sea-island fiber with linear density of 0.62dtex and 40 islands/root, and performing acid treatment to obtain superfine fiber, wherein the acid treatment method comprises placing the sea-island fiber in H with concentration of 10%2SO4In the solution, stirring treatment was carried out for 20min to sufficiently contact the sea-island fibers with the acid solution, and "sea" (PA) of the PA/COPET sea-island fibers was dissolved in the acid solution to obtain 8.5kg of a bundle-like modified polyester microfiber bundle (COPET sea-island filaments) made of COPET, wherein the fineness of the dispersed modified polyester sea-island filaments was 0.01D.
Weighing 4.5kg of the prepared COPET sea island filament with the fineness of 0.01D, 25.5kg of glass fiber (wherein the 29-degree glass fiber accounts for 45 percent, and the 35-degree glass fiber accounts for 55 percent), and 30kg of the two (the COPET sea island filament accounts for 15 percent), adding 12 tons of water to mix to prepare slurry, and preparing the sea island/glass fiber type non-woven material by adopting a wet forming process, wherein the drying process is drying at 90 ℃ for 40min, drying at 100 ℃ for 40min, and drying at 120 ℃ for 40min, and the total drying time is 2h, and finally preparing the sea island/glass fiber type lead storage battery separator. The separator had a width of 71.5mm by 0.62mm, and was used for 20AH battery preparation.
Example 2
Weighing 15kg of PA/COPET sea-island fiber with linear density of 0.69dtex and 50 islands/root, and performing acid treatment to obtain superfine fiber, wherein the acid treatment method comprises placing the sea-island fiber into H with concentration of 15%2SO4In the solution, stirring treatment was carried out for 20min to bring the sea-island fibers into full contact with the acid solution, and "sea" (PA) of the PA/COPET sea-island fibers was dissolved in the acid solution to obtain 8.2kg of a bundle-like modified polyester microfiber bundle (COPET sea-island filaments) made of COPET, wherein the fineness of the dispersed modified polyester sea-island filaments was 0.008D.
Weighing 7.5kg of the prepared COPET sea island filament with fineness of 0.008D, 22.5kg of glass fiber (wherein 29-degree glass fiber accounts for 45 percent and 35-degree glass fiber accounts for 55 percent), and 30kg of the two (COPET sea island filament accounts for 25 percent), adding 12 tons of water to mix to prepare slurry, and preparing the sea island/glass fiber type non-woven material by adopting a wet forming process, wherein the drying process is drying at 90 ℃ for 40min, drying at 100 ℃ for 40min, drying at 120 ℃ for 40min, and the total drying time is 2h, and finally preparing the sea island/glass fiber type lead storage battery separator. The separator had a width of 71.5mm by 0.62mm, and was used for 20AH battery preparation.
Example 3
Weighing 15kg of PA/COPET sea-island fiber with linear density of 0.60dtex and 60 islands/root, and performing acid treatment to obtain superfine fiber, wherein the acid treatment method comprises adding 10% H into the sea-island fiber2SO4In the solution, stirring treatment was carried out for 20min to sufficiently contact the sea-island fiber with the acid solution, and "sea" (PA) of the PA/COPET sea-island fiber was dissolved in the acid solution to obtain 8.7kg of a cluster-like modified polyester microfiber bundle (COPET sea-island filament) made of COPET, in which the fineness of the dispersed modified polyester sea-island filament was 0.006D.
Weighing 1.5kg of the prepared COPET sea island filament with the fineness of 0.006D, 28.5kg of glass fiber (wherein 29-degree glass fiber accounts for 45 percent and 35-degree glass fiber accounts for 55 percent), and 30kg of the two (COPET sea island filament accounts for 5 percent), adding 12 tons of water to mix to prepare slurry, and preparing the sea island/glass fiber type non-woven material by adopting a wet forming process, wherein the drying process is drying at 90 ℃ for 40min, drying at 100 ℃ for 40min, drying at 120 ℃ for 40min, and the total drying time is 2h, and finally preparing the sea island/glass fiber type lead storage battery separator. The separator had a width of 71.5mm by 0.62mm, and was used for 20AH battery preparation.
Example 4
Weighing 15kg of PA/COPET sea-island fiber with linear density of 0.70dtex and 80 islands/root, and performing acid treatment to obtain superfine fiber, wherein the acid treatment method comprises placing the sea-island fiber into H with concentration of 15%2SO4In the solution, stirring treatment was carried out for 20min to sufficiently contact the sea-island fibers with the acid solution, and "sea" (PA) of the PA/COPET sea-island fibers was dissolved in the acid solution to obtain 8.6kg of a bundle-like modified polyester microfiber bundle (COPET sea-island filaments) made of COPET, wherein the fineness of the dispersed modified polyester sea-island filaments was 0.005D.
3.0kg of the prepared COPET sea island filament with the fineness of 0.005D, 27.0kg of glass fiber (wherein the 29-degree glass fiber accounts for 45 percent, and the 35-degree glass fiber accounts for 55 percent) and 30kg of the glass fiber (the COPET sea island filament accounts for 10 percent) are weighed and added into 12 tons of water to be mixed to prepare slurry, the sea island/glass fiber type non-woven material is manufactured by adopting a wet forming process, the drying process temperature is 40min at 90 ℃, 40min at 100 ℃, 40min at 120 ℃ and the total drying time is 2h, and finally, the sea island/glass fiber type lead storage battery separator is prepared. The separator had a width of 71.5mm by 0.62mm, and was used for 20AH battery preparation.
Comparative example 1
30kg of 100% glass fiber (wherein the 29 degree accounts for 45%, the 35 degree accounts for 55%) is added into 12 tons of water to prepare a certain slurry, a wet forming process is adopted to manufacture the sea island/glass fiber type non-woven material, the drying process temperature is 90 ℃ for 40min, 100 ℃ for 40min, 120 ℃ for 40min, and the total drying time is 2h, and finally the glass fiber type lead storage battery separator is prepared. The separator had a width of 71.5mm by 0.62mm, and was used for 20AH battery preparation.
Example 5
The separators prepared in examples 1 to 4 and comparative example 1 were examined for the amount of acid absorbed under pressure.
The partition board is cut into 15 pieces of 50mm × 50mm square, dried at 80 ℃ + -2 ℃ for more than 1h, taken out and placed in a dryer to be cooled to room temperature. Measuring the thickness of the sample by using a 10kPa thickness gauge, adding the thickness to obtain the total thickness of the sample to be measured, and weighing the total weight of the sample to be measured to obtain g 1; placing a sample to be measured in the middle of a clamp, adjusting the clamp, measuring the thickness of the sample at the interval of a 50kPa thickness gauge (by using a vernier caliper), placing the clamp and a partition plate into an acid-resistant container filled with a sulfuric acid solution with the density of 1.280g/cm3 +/-0.005 g/cm3 at 25 ℃, taking out after 30min, keeping pressure for 5min, taking out the partition plate, weighing the total mass to obtain g2, and determining the acid absorption X as (g2-g1)/g 1. For each sample, 5 specimens were selected and their endurance pressure was measured, and the average value was determined.
As shown in Table 1 and FIG. 1, the acid absorption of the separators prepared in examples 1 to 4 was improved to a certain extent compared with the separators prepared in comparative example 1, and the improvement range was 6.9% to 10.9%.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | |
| Liquid absorption amount (unit g/g) | 5.88±0.15 | 6.10±0.18 | 5.95±0.21 | 6.05±0.23 | 5.50±0.19 |
Example 6
The separators prepared in examples 1 to 4 and comparative example 1 were subjected to a wet endurance pressure test.
The detection method comprises the following steps:
1) cutting 15 round AGM clapboards with the diameter of 5cm, stacking the circular AGM clapboards orderly, putting the circular AGM clapboards into water to be fully soaked, and taking out and stacking the circular AGM clapboards orderly;
2) measuring the initial thickness of the diaphragm under the pressure of 0kPa and the actual thickness of the diaphragm under the pressure of 100 kPa;
3) calculating the compression amount of the separator (initial thickness-actual thickness);
4) setting a working program of the universal testing machine, standing for 120s after the preset compression amount is reached, returning the clamp to the position where the displacement is zero, and performing the durability test 200 times in such a circulating reciprocating manner;
5) selecting the data point when the separator is kept still for 120s as the durable pressure value of the separator in the current cycle;
6) for each sample, 5 specimens were selected and their endurance pressure was measured, and the average value was determined.
As shown in Table 2 and FIG. 2, the separator plates prepared in examples 1-4 have a certain increase in the endurance pressure compared to the separator plate prepared in comparative example 1, and the increase range is 28.1% -59.4%.
TABLE 2
Example 7
The separators prepared in examples 1 to 4 and comparative example 1 were subjected to tensile breaking strength.
The detection method comprises the following steps:
firstly, cutting 5 samples (5 samples in each sample) along the forming direction of a partition board, wherein the length of each sample is 100mm, the width of each sample is 15mm, a mark with a clamp of 50mm is made on each sample, the samples are clamped on an upper clamp and a lower clamp of a tensile machine, the samples are clamped and cannot slide and damage the samples in the test process, the central line of each clamp is coaxial with the central line of each sample, the samples are stretched at the speed of 100mm/min +/-5 mm/min, and the load of the samples during the damage is recorded, wherein the tensile strength delta is P/b, delta is the tensile strength and is kN/m, and P is the damage load of the samples and is N (cattle); b is the sample width in mm. The tensile break strength of the separators prepared in examples 1 to 4 and comparative example 1 was measured for 5 specimens each and averaged.
As shown in Table 3 and FIG. 3, the tensile rupture strength of the separators prepared in examples 1 to 4 was improved to some extent by 17.9% to 25.6% as compared with that of the separator prepared in comparative example 1.
TABLE 3
Claims (4)
1. A lead storage battery separator is characterized by comprising glass fiber and COPET sea island filament, wherein the COPET sea island filament is obtained by dissolving PA/COPET sea island fiber in sea,
the specification of the PA/COPET sea-island fiber is as follows: a linear density of 0.6 to 0.7dtex, 40 to 80 islands/root,
the mass percentage content of the COPET sea island filament is 15-25 percent,
the fineness of the COPET sea island filament is 0.008-0.01D,
the fineness of the glass fiber is 29-35 degrees.
2. The lead storage battery separator according to claim 1, wherein the COPET sea-island filaments are prepared by the following method: the method comprises the steps of immersing PA/COPET sea-island fiber into a sulfuric acid solution with the mass concentration of 10% -15%, stirring for 20 minutes, and dissolving sea components to obtain the COPET sea-island filament.
3. The lead storage battery separator according to claim 1, characterized in that it is prepared by the following method: mixing the COPET sea island filaments and the glass fibers in proportion, adding water to prepare slurry, and carrying out wet forming and drying to prepare the separator.
4. A lead-acid battery produced by using the lead-acid battery separator as defined in any one of claims 1 to 3.
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| CN107403934B (en) * | 2017-08-27 | 2020-09-18 | 山东金科力电源科技有限公司 | Short fiber for lead-acid storage battery plate |
| CN109004154B (en) * | 2018-07-23 | 2021-06-18 | 广东蒙泰高新纤维股份有限公司 | Method for manufacturing power lithium ion battery diaphragm by wet papermaking process |
| CN109841786A (en) * | 2019-04-02 | 2019-06-04 | 南京林业大学 | Chemical fibre composite diaphragm and its production method |
| CN113279145B (en) * | 2021-05-27 | 2023-04-07 | 天津齐邦新材料有限公司 | Preparation method of degradable superfine mask base cloth |
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| CN1356731A (en) * | 2000-08-10 | 2002-07-03 | 日本维林株式会社 | Partition for battery |
| CN102522513A (en) * | 2011-12-19 | 2012-06-27 | 中材科技股份有限公司 | Glass fiber battery membrane and preparation method thereof |
| CN103088450A (en) * | 2013-02-05 | 2013-05-08 | 济南欣海特种纤维有限公司 | Sea-island fiber preparation process and distributing plate for spinning |
| WO2017031159A1 (en) * | 2015-08-17 | 2017-02-23 | Celgard, Llc | Improved battery separators and related methods |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1356731A (en) * | 2000-08-10 | 2002-07-03 | 日本维林株式会社 | Partition for battery |
| CN102522513A (en) * | 2011-12-19 | 2012-06-27 | 中材科技股份有限公司 | Glass fiber battery membrane and preparation method thereof |
| CN103088450A (en) * | 2013-02-05 | 2013-05-08 | 济南欣海特种纤维有限公司 | Sea-island fiber preparation process and distributing plate for spinning |
| WO2017031159A1 (en) * | 2015-08-17 | 2017-02-23 | Celgard, Llc | Improved battery separators and related methods |
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