CN111060434B - Device and method for detecting liquid retention and gas diffusion performance of AGM separator - Google Patents
Device and method for detecting liquid retention and gas diffusion performance of AGM separator Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
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Abstract
The invention discloses a device and a method for detecting the liquid retention and gas diffusion performance of an AGM separator, wherein the device comprises a clamping mechanism for clamping the AGM separator, the clamping mechanism comprises a first clamping part and a second clamping part which are matched with each other to clamp the separator from two sides during clamping, clamping grooves are formed in the middle parts of clamping surfaces of the two clamping parts, and porous gaskets supported by supporting plates and the bottoms of the clamping grooves are arranged in the two clamping grooves; an oxygen inlet pipe communicated with the clamping groove of the first clamping part is arranged on the first clamping part, an air outlet pipe and an inert gas inlet pipe communicated with the clamping groove of the second clamping part are arranged on the second clamping part, and an outlet of the air outlet pipe is connected with an inlet of the gas sensor; the inlet ends of the oxygen inlet pipe and the inert gas inlet pipe are respectively communicated with the oxygen tank and the inert gas tank; and a heating sleeve is arranged on the oxygen inlet pipe. The invention can solve the problem that the detection of the liquid retention performance and the gas diffusion performance of the AGM separator cannot be conveniently carried out in the prior art.
Description
Technical Field
The invention belongs to the field of AGM separator detection, and particularly relates to a device and a method for detecting liquid retention and gas diffusion performance of an AGM separator.
Background
The AGM separator is one of the key materials of valve-regulated lead-acid storage battery and has the main functions of (1) preventing the short circuit inside the battery caused by the mutual contact of positive and negative plates; (2) the storage battery pole group is tightly assembled, and the deformation and the bending of the pole plate and the falling of the active substance are prevented; (3) the necessary amount of electrolyte is stored in the porous separator between the polar plates to ensure higher conductivity and the requirement of battery reaction; (5) preventing migration and diffusion of some substances harmful to the battery through the separator.
The AGM separator should prevent both the positive and negative electrodes from short-circuiting and not increase the internal resistance of the battery significantly, and therefore, should be porous in nature, allow free diffusion of electrolyte and ion migration, and have a relatively small resistance. Meanwhile, the anode and the cathode should be prevented from short circuit caused by the growth of lead dendrite, so the aperture is small and the flexibility is certain; in addition, it is required that the mechanical strength is good, the resistance to acid corrosion, the resistance to oxidation, and the absence of precipitation of substances harmful to the electrode plate.
For example, chinese patent publication No. CN106257708A discloses an anti-short AGM separator, which is made from the following raw materials in percentage by mass: 3-5% of modified nano vermiculite powder, 3-5% of polyethylene oxide, 5-10% of modified bamboo fibers, 10-15% of water-soluble polyvinyl alcohol fibers, 5-10% of polyimide fibers, 30-35% of high-alkali glass fibers with the diameter of 0.5-0.7 mu m, and the balance of high-alkali glass fibers with the diameter of 3-4 mu m. The technical scheme abandons the traditional pure glass fiber formula, is formed by mixing and interweaving a plurality of fibers, has high porosity, uniform gap and excellent comprehensive performance, and can effectively avoid short circuit caused by that the lead powder of the anode penetrates through the separator to the cathode.
Chinese patent publication No. CN206059490U discloses a high-strength AGM separator, which comprises an intermediate layer, adhesive layers, a strength layer, and a PE mesh layer, wherein the adhesive layers are disposed on the upper and lower surfaces of the intermediate layer, the strength layer is disposed on the surface of the adhesive layers, the PE mesh layer is disposed on the surface of the strength layer, the intermediate layer is formed by interweaving glass fibers, the adhesive layers are formed by interweaving water-soluble polyvinyl alcohol fibers, and the strength layer is a mixed fiber layer formed by interweaving 95-97% by mass of glass fibers and 3-5% by mass of cellulose fibers. According to the technical scheme, the mechanical strength and the puncture resistance of the AGM separator are improved, the AGM separator is not easy to break and break during the assembly of a polar group or acid filling, and is not easy to be penetrated by lead dendrites in the using process, so that the micro short circuit capability of the battery can be effectively prevented.
Valve-regulated lead acid batteries (VRLA) are widely used based on the mechanism of oxygen recombination, specifically, oxygen gas evolved from the positive electrode at the end of charging the VRLA battery will diffuse through the porous separator to the negative electrode plate and react with the negative electrode to be consumed. The glass fiber surface of the AGM separator hinders oxygen transport because it is easily wetted by the electrolyte, which affects the performance and life of the lead acid battery. Thus, for AGM-VRLA batteries, the oxygen recombination efficiency is an important parameter index for evaluating the performance of AGM separators. In addition, the AGM separator is used as an electrolyte storage component of the AGM-VRLA battery, and should maintain a certain electrolyte density during the use of the battery to avoid the increase of the electrolyte density and the reduction of the saturation degree of the separator caused by water loss so as to ensure the discharge performance of the battery. Therefore, it is desirable to design a detection device capable of effectively evaluating the gas diffusion performance and the liquid retention performance of the AGM separator, so as to more conveniently detect the liquid retention performance and the gas diffusion performance of the AGM separator.
Disclosure of Invention
The invention provides a device and a method for detecting liquid retention and gas diffusion of an AGM separator, aiming at solving the problem that the detection of the liquid retention performance and the gas diffusion performance of the AGM separator cannot be conveniently carried out in the prior art.
A device for detecting the liquid retention and gas diffusion performance of an AGM separator comprises a clamping mechanism for clamping the AGM separator, wherein the clamping mechanism comprises a first clamping part and a second clamping part which are matched with each other to clamp the separator from two sides during clamping, clamping grooves are formed in the middle of clamping surfaces of the two clamping parts, and porous gaskets supported by supporting plates and the bottoms of the clamping grooves are arranged in the two clamping grooves; an oxygen inlet pipe communicated with the clamping groove of the first clamping part is arranged on the first clamping part, an air outlet pipe and an inert gas inlet pipe communicated with the clamping groove of the second clamping part are arranged on the second clamping part, and an outlet of the air outlet pipe is connected with an inlet of the gas sensor;
the inlet ends of the oxygen inlet pipe and the inert gas inlet pipe are respectively communicated with the oxygen tank and the inert gas tank; and a heating sleeve is arranged on the oxygen inlet pipe.
By utilizing the device disclosed by the invention, the liquid retention and gas diffusion performance of the AGM separator can be rapidly and accurately evaluated. In use, the clamping mechanism is used to secure the AGM separator and can simulate a compressed state within the battery. One surface of the porous gasket is abutted against two side surfaces of the AGM separator in a state that the AGM separator is clamped by the clamping mechanism, and the other surface of the porous gasket is supported by the bottom of the clamping groove through the supporting plate, so that a cavity structure can be formed between the AGM separator and the clamping groove for temporarily stopping air, and the gas is favorably dispersed and collected.
The outlet of the gas sensor is connected with a tail gas receiving device, and the interior of the gas sensor contains a green and safe oxygen consumption agent to effectively absorb discharged gas.
In order to improve the sealing performance of the clamping mechanism, the clamping mechanism has a certain pressure maintaining function, an annular sealing groove is formed around the clamping groove of the second clamping part, and a sealing bulge matched with the sealing groove is formed in the first clamping part.
In the invention, the support plate and the porous gasket can be of a split structure or an integrated structure, and when the support plate and the porous gasket are of an integrated structure, the support plate is arranged on four side edges of the porous gasket.
The first clamping part and the second clamping part are detachably connected through bolts.
The invention also provides a method for detecting the liquid retention and gas diffusion performance of the AGM separator, which utilizes the device for detection and comprises the following steps:
(1) taking an AGM separator sample to be detected, recording the dry weight m0, placing the AGM separator sample to be detected under a certain pressure, stabilizing for 2-15 min, then adding liquid to the compressed AGM separator to saturate and absorb the AGM separator sample to be detected, taking out, recording the initial weight m1 of the wet AGM separator sample, and obtaining the saturated absorption liquid quantity delta m of the AGM separator under the pressure, which is m1-m 0;
(2) measuring a wet AGM separator sample with saturation of 60% -98% according to the measured saturated imbibition amount, recording the weight m2, fixing the clamping device, opening a valve of an oxygen tank to pre-purge the device for 1-5 min, immediately opening the clamping device, placing the wet AGM separator with certain saturation between a first clamping part and a second clamping part of the clamping device, and sealing and fixing;
(3) opening a pressure reduction control valve of the inert gas tank to enable the inert gas to replace the air in the clamping groove and the AGM partition plate;
(4) closing a valve of an inert gas tank, controlling a heating sleeve to heat an oxygen inlet pipe, opening a pressure reduction control valve of the oxygen tank after the temperature in the oxygen inlet pipe is stable, and recording the time interval from the opening of the valve of the oxygen tank to the detection of oxygen by a gas sensor; closing the oxygen sensor and continuously introducing hot oxygen, closing a pressure reduction control valve of an oxygen pipe after the preset time is reached, taking out a wet AGM partition plate sample, weighing, and recording as the finished weight m 3;
(5) the gas diffusion performance of the wet AGM separator was evaluated according to the time interval, and the liquid retention performance of the AGM separator was evaluated according to the difference between m2 and the end weight m 3.
The method can place different AGM separators in the device for detecting the performance of the separator, further analyze the gas diffusion and liquid retention capacity of the different AGM separators, and provide reference basis for research and development and model selection of the AGM separators.
In the step (1), the AGM separator sample is placed under the pressure of 10-100 kPa, and the added liquid is pure water or dilute sulfuric acid.
In the step (3), the pressure reduction control valve of the inert gas tank is controlled to ensure that the ventilation pressure of the inert gas tank is less than 0.2MPa and the ventilation time is 1-20 min. The ventilation pressure ensures that the air in the clamping groove is not diffused to the other side of the AGM separator.
In the step (4), the heating sleeve is controlled to heat, so that the temperature of the air in the oxygen inlet pipe is kept at 50-60 ℃.
In the step (4), the pressure reduction control valve of the oxygen tank is controlled to ensure that the ventilation pressure of the oxygen tank is less than 0.2 MPa.
Compared with the prior art, the invention has the following beneficial effects:
according to the device, the AGM separator is clamped by the clamping mechanism, the compression state in the battery can be simulated, and the clamping groove and the porous gasket in the clamping mechanism can ensure that a cavity structure can be formed between the AGM separator and the clamping groove for temporarily stopping gas, so that the gas is dispersed and collected; by arranging the oxygen inlet pipe, the inert gas and the gas sensor, the time for the gas to diffuse from one side of the AGM separator to the other side can be accurately calculated; meanwhile, the liquid retention performance of the AGM separator in a wet state can be measured according to the mass change before and after the experiment of weighing the AGM separator, and the whole device is simple in structure and convenient to operate.
Drawings
FIG. 1 is a schematic diagram of the overall structure of an apparatus for detecting the liquid retention and gas diffusion performance of an AGM separator according to the present invention;
FIG. 2 is a schematic structural diagram of a second clamping portion according to an embodiment of the present invention;
FIG. 3 is a schematic structural view of a porous pad according to an embodiment of the present invention;
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples, which are intended to facilitate the understanding of the invention without limiting it in any way.
As shown in fig. 1, a device for detecting liquid retention and gas diffusion performance of an AGM separator comprises a clamping mechanism for clamping the AGM separator, the clamping mechanism comprises a first clamping part 1 and a second clamping part 2 which are matched to clamp the separator from two sides during clamping, clamping grooves are arranged in the middle of clamping surfaces of the two clamping parts, an oxygen inlet pipe 3 communicated with the clamping grooves is arranged on the first clamping part 1, an air outlet pipe 5 and an inert gas inlet pipe 4 communicated with the clamping grooves are arranged on the second clamping part 2, and an outlet of the air outlet pipe 5 is connected with an inlet of a gas sensor 6; the outlet of the gas sensor 6 is connected to an exhaust gas receiving device 8 via a conduit 7. The tail gas receiving device 8 contains a green and safe oxygen consuming agent inside, and effectively absorbs the discharged gas.
In the device, the inlet ends of an oxygen inlet pipe 3 and an inert gas inlet pipe 4 are respectively communicated with an oxygen tank and an inert gas tank; the oxygen inlet pipe 3 is also provided with a heating sleeve 9.
The overall structure of first clamping part 1 and second clamping part 2 is comparatively similar, and the clamping face middle part of two clamping parts all is equipped with the centre gripping groove, all is equipped with the porous gasket that supports through backup pad and centre gripping tank bottom in two centre gripping inslots.
As shown in fig. 2, the clamping mechanism will be further described by taking the second clamping portion 2 as an example. The clamping surface of the second clamping part is provided with a clamping groove 21, an annular sealing groove 22 is arranged around the clamping groove 21, and correspondingly, the first clamping part 1 is provided with a sealing bulge matched with the sealing groove 22. The holding groove 21 is provided with a porous gasket 23 supported by the support plate and the bottom of the holding groove 21.
The support plate and the holding groove may be formed in a separate structure or in an integrated structure, and as shown in fig. 3, the support plate 24 and the porous pad 23 are formed in an integrated structure, and four support plates 24 are disposed on four sides of the porous pad 23.
One surface of the porous gasket is abutted against two side surfaces of the AGM separator in the state that the first clamping part 1 and the second clamping part 2 clamp the AGM separator, and the other surface of the porous gasket is supported with the bottom of the clamping groove through the supporting plate, so that a cavity structure can be formed between the AGM separator and the clamping groove for temporarily stopping gas and facilitating the dispersion and collection of the gas. The first clamping part 1 and the second clamping part 2 can be detachably connected through bolts.
The specific examples of the liquid retention and gas diffusion performance detection by using the device are as follows:
example 1
(1) Cutting an AGM separator to be measured into a regular shape with the diameter of 50 multiplied by 50mm, taking 10 samples to be stacked in order, recording the weight m 0-4.606 g of the samples, placing the samples under a certain pressure of 80kPa for stabilizing for 10min, then adding excessive pure water into the compressed AGM separator to ensure that the AGM separator to be measured fully absorbs liquid, taking out the AGM separator to record the weight m 1-21.172 g of the wet AGM separator sample, and ensuring that the saturated liquid absorption quantity Deltam of the AGM separator under the pressure of 80kPa is 16.566 g;
(2) pre-purging the apparatus for 2min, and then holding a sample of an AGM separator (m2 ═ 20.344g) having a saturation of 95% between the first holding section and the second holding section, and sealing and fixing the sample;
(3) introducing hot oxygen gas into the AGM partition plate clamping device, recording the time of opening a valve of an oxygen tank, closing a pressure reduction control valve of an oxygen pipe after 60min, taking out a wet AGM partition plate sample, and weighing the AGM partition plate sample, wherein the weight m3 is recorded as 19.848 g; the formula for calculating the liquid retention performance of the AGM separator was that a ═ 3.15% (m2-m3)/(m2-m0), and the liquid retention performance was evaluated according to the size of a.
Example 2
(1) Cutting an AGM separator to be measured into a regular shape with the diameter of 50 multiplied by 50mm, taking 10 samples to be stacked in order, recording the weight m 0-4.614 g of the samples, placing the samples under a certain pressure of 80kPa for stabilizing for 10min, then adding excessive pure water into the compressed AGM separator to ensure that the AGM separator to be measured fully absorbs liquid, taking out the AGM separator to record the weight m 1-21.102 g of the wet AGM separator sample, and ensuring that the saturated liquid absorption quantity Deltam of the AGM separator under the pressure of 80kPa is 16.488 g;
(2) closing the oxygen sensor testing device, opening an oxygen pressure reducing valve to pre-purge the device, and clamping an AGM partition board (m2 is 19.453g) sample with the saturation of 90% between the first clamping part and the second clamping part after 2min for sealing and fixing;
(3) opening a pressure reducing valve of the nitrogen gas tank, ventilating for 2min, and replacing oxygen gas in the gas path;
(4) closing a valve of an inert gas tank, opening an oxygen sensor, introducing hot oxygen into the AGM partition plate clamping device, recording the opening time of the valve of the oxygen tank, closing a pressure reduction control valve of an oxygen pipe after the oxygen sensor gives out an alarm sound, recording the time difference (interval time delta t), and evaluating the gas diffusion performance according to the delta t.
Example 3
(1) Cutting an AGM separator to be measured into a regular shape with the diameter of 50 multiplied by 50mm, taking 10 samples to be stacked in order, recording the weight m0 of the samples to be 4.616g, placing the samples under a certain pressure of 80kPa for stabilizing for 10min, then adding excessive pure water into the compressed AGM separator to ensure that the AGM separator to be measured fully absorbs liquid, taking out the AGM separator to record the weight m1 of the wet AGM separator to be 21.132g, and ensuring that the saturated liquid absorption quantity Deltam of the AGM separator under the pressure of 80kPa is 16.516 g;
(2) pre-purging the apparatus for 2min, and then holding a sample of an AGM separator (m2 ═ 19.811g) having a saturation of 92% between the first holding portion and the second holding portion, and sealing and fixing the sample;
(3) after an inert gas inlet pipeline is closed, hot oxygen gas is introduced into the AGM partition plate clamping device, the time delta t of opening a valve of an oxygen tank is recorded, then an oxygen sensor is closed, the hot oxygen gas is continuously introduced, after 60min, a pressure reduction control valve of an oxygen pipe is closed, a wet AGM partition plate sample is taken out and weighed, and the weight m3 is recorded as 19.208 g; the formula for calculating the liquid retention performance of the AGM separator is that a is (m2-m3)/(m2-m0) is 4.01%, and the liquid retention performance is evaluated according to the size of a; meanwhile, the gas diffusion performance was evaluated according to Δ t.
The device can respectively detect the liquid retention performance and the gas diffusion performance, and can simultaneously detect the liquid retention performance and the gas diffusion performance in one detection according to actual needs.
The liquid retention performance of the AGM separator affects the oxygen recombination capacity in the sealed lead acid battery, and the device of the invention can be used for measuring the liquid retention performance of the separator so as to evaluate the relevant performance of the separator. Specifically, the AGM separator to be tested is placed in the clamping mechanism, under the condition that other conditions are the same, the weight changes of different AGM separators in a wet state are compared, the liquid retention performance of different AGM separators is analyzed and evaluated, and meanwhile, the gas diffusion new energy is evaluated according to the detected speed of oxygen, so that a reference basis is provided for the research and development of the AGM separators.
The embodiments described above are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions and equivalents made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for detecting the liquid retention and gas diffusion performance of an AGM separator adopts a clamping mechanism for clamping the AGM separator, and is characterized in that the clamping mechanism comprises a first clamping part and a second clamping part which are matched with each other to clamp the separator from two sides during clamping, clamping grooves are formed in the middle of clamping surfaces of the two clamping parts, and porous gaskets are arranged in the two clamping grooves and supported by supporting plates and the bottoms of the clamping grooves; an oxygen inlet pipe communicated with the clamping groove of the first clamping part is arranged on the first clamping part, an air outlet pipe and an inert gas inlet pipe communicated with the clamping groove of the second clamping part are arranged on the second clamping part, and an outlet of the air outlet pipe is connected with an inlet of the gas sensor;
the inlet ends of the oxygen inlet pipe and the inert gas inlet pipe are respectively communicated with the oxygen tank and the inert gas tank; a heating sleeve is arranged on the oxygen inlet pipe;
the method comprises the following steps:
(1) taking an AGM separator sample to be measured, recording the dry weight m0, placing the AGM separator sample to be measured under a certain pressure, stabilizing for 2-15 min, then adding liquid into the compressed AGM separator to saturate and absorb the AGM separator sample to be measured, taking out, recording the initial weight m1 of the wet AGM separator sample, and obtaining the saturated absorption liquid quantity delta m of the AGM separator under the pressure, which is m1-m 0;
(2) measuring a wet AGM separator sample with saturation of 60% -98% according to the measured saturated imbibition amount, recording the weight m2, fixing the clamping device, opening a valve of an oxygen tank to pre-purge the device for 1-5 min, immediately opening the clamping device, placing the wet AGM separator with certain saturation between a first clamping part and a second clamping part of the clamping device, and sealing and fixing;
(3) opening a pressure reduction control valve of the inert gas tank to enable the inert gas to replace oxygen in the clamping groove and the AGM partition plate;
(4) closing a valve of an inert gas tank, controlling a heating sleeve to heat an oxygen inlet pipe, opening a pressure reduction control valve of the oxygen tank after the temperature in the oxygen inlet pipe is stable, and recording the time interval from the opening of the valve of the oxygen tank to the detection of oxygen by a gas sensor; closing the oxygen sensor and continuously introducing oxygen, closing a pressure reduction control valve of an oxygen pipe after the preset time is reached, taking out a wet AGM partition plate sample, weighing, and recording as the finished weight m 3;
(5) the gas diffusion performance of the wet AGM separator was evaluated according to the length of the time interval, and the liquid retention performance of the AGM separator was evaluated according to the difference between m2 and the end weight m 3.
2. The method according to claim 1, wherein an exhaust gas receiving device is connected to an outlet of the gas sensor.
3. The method according to claim 1, wherein an annular sealing groove is formed around the clamping groove of the second clamping portion, and a sealing protrusion matching with the sealing groove is formed on the first clamping portion.
4. The method according to claim 1, wherein the support plate is integrally formed with the porous pad, and the support plates are disposed on four sides of the porous pad.
5. The method according to claim 1, wherein the first clamping portion and the second clamping portion are detachably connected by a bolt.
6. The method according to claim 1, wherein in step (1), the AGM separator sample is placed under a pressure of 10kPa to 100kPa, and the liquid is pure water or a dilute sulfuric acid solution.
7. The method for testing liquid retention and gas diffusion performance of an AGM separator according to claim 1, wherein in the step (3), the pressure reduction control valve of the inert gas tank is controlled so that the aeration pressure of the inert gas tank is less than <0.2MPa and the aeration time is 1 to 20 min.
8. The method for detecting the liquid retention and gas diffusion performance of an AGM separator according to claim 1, wherein in the step (4), the heating of the heating sleeve is controlled so that the temperature of the air in the oxygen inlet pipe is kept at 50-60 ℃.
9. The method for testing liquid retention and gas diffusion performance of an AGM separator according to claim 1, wherein in the step (4), the pressure reduction control valve of the oxygen tank is controlled so that the aeration pressure of the oxygen tank is less than 0.2 MPa.
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