CN110416473B - Aramid fiber slurry, preparation method thereof and diaphragm based on aramid fiber slurry - Google Patents
Aramid fiber slurry, preparation method thereof and diaphragm based on aramid fiber slurry Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D177/00—Coating compositions based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Coating compositions based on derivatives of such polymers
- C09D177/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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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
Abstract
The invention discloses aramid fiber slurry, a preparation method thereof and a diaphragm based on the aramid fiber slurry, wherein the preparation method of the aramid fiber slurry comprises the following steps: preparing a first solution and a second solution, mixing the first solution with dimethylacetamide, stirring the mixture evenly, adding water, stirring the mixture evenly, adding isopropanol, stirring the mixture evenly, adding dimethyl carbonate, stirring the mixture evenly, adding the second solution, and stirring the mixture evenly to obtain the aramid fiber slurry.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to aramid fiber slurry, a preparation method of the aramid fiber slurry and a diaphragm based on the aramid fiber slurry.
Background
The lithium ion battery comprises a positive electrode, a negative electrode, a separator and an electrolyte, wherein the separator is one of four main materials of the lithium ion battery, does not participate in electrochemical reaction in the battery, and is a key inner layer component in the lithium battery.
The aramid fiber coated diaphragm has the advantages of good high-temperature resistance, high energy density, excellent wettability, long service life and the like, and is widely concerned by industrial people. When the aramid fiber coating membrane is manufactured, a large amount of solvent is needed for extraction in the coating process, the resource waste cost is high, the extraction waste liquid is difficult to treat, the environment is polluted, and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the aramid fiber slurry.
The invention also aims to provide the aramid pulp obtained by the preparation method.
It is another object of the present invention to provide a separator coated with the aramid pulp.
The invention also aims to provide application of the aramid fiber slurry in improving the pore-forming uniformity.
The purpose of the invention is realized by the following technical scheme.
The preparation method of the aramid fiber slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, stirring for 4-10 hours at 80-100 ℃ in a closed environment to dissolve the meta-aramid fiber in the dimethylacetamide to obtain a first solution, wherein the dimethylacetamide accounts for 70-78 wt% of the first base material, the meta-aramid fiber accounts for 18-22 wt% of the first base material, the chloride salt accounts for 1.2-8 wt% of the first base material, and the chloride salt is lithium chloride or calcium chloride;
the second solution was prepared as follows: uniformly mixing alumina and tripropylene glycol to obtain a second base material, and sanding the second base material by using a sand mill to ensure that the particle size of the second base material is D50: 0.9-1.2 μm and D90: 1.4-1.7 μm to obtain a second solution, wherein the alumina accounts for 45-55 wt% of the second base material by mass fraction;
in the step 1), the method for obtaining the second base stock comprises the following steps: mixing alumina and tripropylene glycol, then putting the mixture into a stirring tank, and stirring the mixture for 3 to 6 hours by adopting a double-planet stirrer, wherein the revolution of the stirring speed is 30 to 40r/min, and the rotation is 2000 to 2500 r/min.
2) Mixing the first solution and dimethylacetamide, stirring uniformly, adding water, stirring uniformly, adding isopropanol, stirring uniformly, adding dimethyl carbonate, stirring uniformly, adding the second solution, and stirring uniformly to obtain the aramid fiber slurry, wherein the first solution accounts for 18-22 wt% of the aramid fiber slurry, the dimethylacetamide accounts for 15-20 wt% of the aramid fiber slurry in the step 2), the water accounts for 5-10 wt% of the aramid fiber slurry, the isopropanol accounts for 5-9 wt% of the aramid fiber slurry, the dimethyl carbonate accounts for 7-10 wt% of the aramid fiber slurry, and the second solution accounts for 34-40 wt% of the aramid fiber slurry.
In the step 2), stirring is performed while adding the water.
In the step 2), mixing the first solution with dimethylacetamide, and stirring for 30-90 min until the mixture is uniform.
In the step 2), water is added and then stirred for at least 30min until the mixture is uniform.
In the step 2), adding isopropanol and stirring for at least 30min until the mixture is uniform.
In the step 2), adding dimethyl carbonate and stirring for at least 30min until the mixture is uniform.
In the step 2), the second solution is added and stirred for at least 60min until the mixture is uniform.
The aramid fiber slurry obtained by the preparation method.
The preparation method of the diaphragm comprises the steps of coating the aramid fiber slurry on a base film, and carrying out water extraction to obtain the diaphragm.
The aramid fiber slurry is applied to improving the pore-forming uniformity.
The aramid fiber slurry contains alcohol, water and ester, the proportion of three non-solvents (alcohol, water and ester) is creatively adjusted, the alcohol, the water and the ester occupy the position of the aramid fiber slurry under the combined action of the three non-solvents, and the non-solvents are uniformly dissolved in water after the aramid fiber is solidified by pure water, so that the extraction effect is achieved, and the pores of the aramid fiber are uniformly formed.
Drawings
FIG. 1 is an electron micrograph of a separator obtained in example 1 of the present invention;
FIG. 2 is an electron micrograph of a separator obtained in comparative example 2;
FIG. 3 is an electron micrograph of the separator obtained in comparative example 1.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The purchase sources of the drugs involved in the following examples are as follows:
dimethyl acetamide: 99.5% of Ci chemical reagent manufacturing Co., Ltd, Tianjin City
Tripropylene glycol: 99.5% of Ci chemical reagent manufacturing Co., Ltd, Tianjin City
Isopropyl alcohol: 99.5% of Ci chemical reagent manufacturing Co., Ltd, Tianjin City
Meta-aramid fiber: japanese Sumitomo
The instruments and models tested in the following examples were as follows:
the agitator tank adopts a double planet mixer (HY-DLH43L)
Example 1
The preparation method of the aramid fiber slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, sealing the first base material in a stirring tank, introducing hot water of 80 ℃ into a jacket of the stirring tank, and stirring at 80 ℃ for 10 hours to dissolve the meta-aramid fiber in dimethylacetamide to obtain a first solution, wherein the stirring speed is 35r/min, and according to mass fraction, the chloride salt is 2 wt% of the first base material, the dimethylacetamide is 78 wt% of the first base material, the meta-aramid fiber is 20 wt% of the first base material, and the chloride salt is lithium chloride;
the second solution was prepared as follows: mixing alumina and tripropylene glycol, putting the mixture into a stirring tank, stirring the mixture for 3 hours by using a double-planet stirrer until the mixture is uniformly mixed (revolution at the stirring speed of 40r/min and rotation at the rotation speed of 2500r/min) to obtain a second base material, and then sanding the second base material for 3 times (the rotation speed of 800r/min) by using a sand mill to ensure that the particle size of the second base material is D50:0.9 mu m and D90:1.4 mu m to obtain a second solution, wherein the alumina accounts for 45 wt% of the second base material in terms of mass fraction;
2) mixing the first solution with dimethylacetamide, stirring for 0.5h to be uniform, adding water and stirring while adding water to prevent a large amount of bulk aramid fibers from being diluted to cause insolubility again. Adding water, stirring for 30min to be uniform, adding isopropanol, stirring for 30min to be uniform, adding dimethyl carbonate, stirring for 30min to be uniform, adding a second solution, stirring for 60min to be uniform, and obtaining aramid fiber slurry, wherein the first solution is 20 wt% of the aramid fiber slurry, the dimethylacetamide in the step 2) is 19 wt% of the aramid fiber slurry, the water is 9 wt% of the aramid fiber slurry, the isopropanol is 9 wt% of the aramid fiber slurry, the dimethyl carbonate is 9 wt% of the aramid fiber slurry, and the second solution is 34 wt% of the aramid fiber slurry.
Example 2
The preparation method of the aramid fiber slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, sealing the first base material in a stirring tank, introducing hot water of 80 ℃ into a jacket of the stirring tank, and stirring at 80 ℃ for 10 hours to dissolve the meta-aramid fiber in dimethylacetamide to obtain a first solution, wherein the stirring speed is 35r/min, and according to mass fraction, the chloride salt accounts for 8 wt% of the first base material, the dimethylacetamide accounts for 72 wt% of the first base material, the meta-aramid fiber accounts for 20 wt% of the first base material, and the chloride salt is lithium chloride;
the second solution was prepared as follows: mixing alumina and tripropylene glycol, putting the mixture into a stirring tank, stirring the mixture for 3 hours by using a double-planet stirrer until the mixture is uniformly mixed (revolution at the stirring speed of 40r/min and rotation at the rotation speed of 2500r/min) to obtain a second base material, and then sanding the second base material for 3 times (the rotation speed of 800r/min) by using a sand mill to ensure that the particle size of the second base material is D50:1 μm and D90:1.5 μm to obtain a second solution, wherein the alumina accounts for 50 wt% of the second base material in terms of mass fraction;
2) mixing the first solution with dimethylacetamide, stirring for 1h to be uniform, adding water and stirring while adding water to prevent a large amount of bulk aramid fibers from being diluted and causing the problem that the aramid fibers cannot be dissolved again. Adding water, stirring for 30min to be uniform, adding isopropanol, stirring for 30min to be uniform, adding dimethyl carbonate, stirring for 30min to be uniform, adding a second solution, stirring for 60min to be uniform, and obtaining aramid fiber slurry, wherein the first solution is 21 wt% of the aramid fiber slurry, dimethylacetamide in the step 2) is 19 wt% of the aramid fiber slurry, water is 10 wt% of the aramid fiber slurry, isopropanol is 7 wt% of the aramid fiber slurry, dimethyl carbonate is 8 wt% of the aramid fiber slurry, and the second solution is 35 wt% of the aramid fiber slurry.
Example 3
The preparation method of the aramid fiber slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, sealing the first base material in a stirring tank, introducing hot water of 80 ℃ into a jacket of the stirring tank, and stirring at 80 ℃ for 10 hours to dissolve the meta-aramid fiber in dimethylacetamide to obtain a first solution, wherein the stirring speed is 35r/min, and according to mass fraction, the chloride salt is 3 wt% of the first base material, the dimethylacetamide is 75 wt% of the first base material, the meta-aramid fiber is 22 wt% of the first base material, and the chloride salt is lithium chloride;
the second solution was prepared as follows: mixing alumina and tripropylene glycol, putting the mixture into a stirring tank, stirring the mixture for 3 hours by using a double-planet stirrer until the mixture is uniformly mixed (revolution at the stirring speed of 40r/min and rotation at the rotation speed of 2500r/min) to obtain a second base material, and then sanding the second base material for 3 times (the rotation speed of 800r/min) by using a sand mill to ensure that the particle size of the second base material is D50:1.2 mu m and D90:1.7 mu m to obtain a second solution, wherein the alumina accounts for 55 wt% of the second base material in terms of mass fraction;
2) mixing the first solution with dimethylacetamide, stirring for 1h to be uniform, adding water and stirring while adding water to prevent a large amount of bulk aramid fibers from being diluted and causing the problem that the aramid fibers cannot be dissolved again. Adding water, stirring for 30min to be uniform, adding isopropanol, stirring for 30min to be uniform, adding dimethyl carbonate, stirring for 30min to be uniform, adding a second solution, stirring for 60min to be uniform, and obtaining aramid fiber slurry, wherein the first solution is 22 wt% of the aramid fiber slurry, dimethylacetamide in the step 2) is 19 wt% of the aramid fiber slurry, water is 6 wt% of the aramid fiber slurry, isopropanol is 7 wt% of the aramid fiber slurry, dimethyl carbonate is 9 wt% of the aramid fiber slurry, and the second solution is 37 wt% of the aramid fiber slurry.
The aramid pulp provided in examples 1 to 3 was coated on a polyethylene-based film (coating speed 8m/min) and then extracted by the following method: the extraction tank is divided into 10 small tanks, the tank depth is about one meter, each tank is filled with pure water, and the polyethylene base film coated with aramid pulp passes through each tank (each polyethylene base film is soaked in each tank for 12 seconds to obtain the diaphragm.
Comparative example 1
A preparation method of slurry is based on example 1, and isopropanol, water and dimethyl carbonate non-solvent are removed, and other steps are unchanged. Namely, the preparation method of the slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, sealing the first base material in a stirring tank, introducing hot water of 80 ℃ into a jacket of the stirring tank, and stirring at 80 ℃ for 10 hours to dissolve the meta-aramid fiber in dimethylacetamide to obtain a first solution, wherein the stirring speed is 35r/min, and according to mass fraction, the chloride salt is 2 wt% of the first base material, the dimethylacetamide is 78 wt% of the first base material, the meta-aramid fiber is 20 wt% of the first base material, and the chloride salt is lithium chloride;
the second solution was prepared as follows: mixing alumina and tripropylene glycol, putting the mixture into a stirring tank, stirring the mixture for 3 hours by using a double-planet stirrer until the mixture is uniformly mixed (revolution at the stirring speed of 40r/min and rotation at the rotation speed of 2500r/min) to obtain a second base material, and then sanding the second base material for 3 times (the rotation speed of 800r/min) by using a sand mill to ensure that the particle size of the second base material is D50:0.9 mu m and D90:1.4 mu m to obtain a second solution, wherein the alumina accounts for 45 wt% of the second base material in terms of mass fraction;
2) and (3) mixing the first solution with dimethylacetamide, stirring for 0.5h until the mixture is uniform, adding a second solution, and stirring for 60min until the mixture is uniform to obtain slurry, wherein the first solution accounts for 30 wt% of the slurry, the dimethylacetamide accounts for 25 wt% of the slurry in the step 2), and the second solution accounts for 45 wt% of the slurry.
Comparative example 2
The preparation method of the traditional aramid fiber slurry comprises the following steps:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, sealing the first base material in a stirring tank, introducing hot water of 80 ℃ into a jacket of the stirring tank, and stirring at 80 ℃ for 10 hours to dissolve the meta-aramid fiber in dimethylacetamide to obtain a first solution, wherein the stirring speed is 35r/min, and according to mass fraction, the chloride salt is 2 wt% of the first base material, the dimethylacetamide is 80 wt% of the first base material, the meta-aramid fiber is 18 wt% of the first base material, and the chloride salt is lithium chloride.
The second solution was prepared as follows: mixing alumina and tripropylene glycol, putting the mixture into a stirring tank, stirring the mixture for 3 hours by using a double-planet stirrer until the mixture is uniformly mixed (revolution at the stirring speed of 40r/min and rotation at the rotation speed of 2500r/min) to obtain a second base material, and then sanding the second base material for 3 times (the rotation speed of 800r/min) by using a sand mill to ensure that the particle size of the second base material is D50:0.9 mu m and D90:1.4 mu m to obtain a second solution, wherein the alumina accounts for 45 wt% of the second base material in terms of mass fraction;
2) mixing the first solution with dimethylacetamide, stirring for 0.5h to be uniform, adding dimethyl carbonate, stirring for 30min to be uniform, adding the second solution, stirring for 60min to be uniform, and obtaining the traditional aramid pulp, wherein the first solution accounts for 20 wt% of the traditional aramid pulp, the dimethylacetamide accounts for 29 wt% of the traditional aramid pulp in the step 2), the dimethyl carbonate accounts for 13 wt% of the traditional aramid pulp, and the second solution accounts for 38 wt% of the traditional aramid pulp.
The slurry/conventional aramid slurry of comparative examples 1-2 was coated on a polyethylene-based film (coating speed 8m/min) and then extracted in the following manner: dividing the extraction tank into 10 small tanks, enabling the polyethylene base membrane coated with the slurry/traditional aramid fiber slurry to penetrate through each tank to obtain a diaphragm, wherein the depth of each tank is about one meter, extracting solutions with different proportions are adopted in the first three tanks, the extracting solutions are mixed solutions of deionized water and DMAC, the proportion of DMAC to water in the first tank is 3:2 (volume ratio), the proportion of DMAC to water in the second tank is 1:1 (volume ratio), the proportion of DMAC to water in the third tank is 2:3 (volume ratio), the process is extracted by three coagulation baths with different concentrations, and the other tanks are extracted by deionized water. Each polyethylene-based film was guaranteed to be immersed for a sufficient 12 seconds in each tank.
Relevant parameters of the separators obtained in examples 1 to 3 and comparative examples 1 and 2 are shown in Table 1. An electron microscope image of the aramid pulp obtained in example 1 and the separator obtained from the pulp obtained in comparative example 2 is shown in fig. 1, an electron microscope image of the separator obtained from the pulp obtained in comparative example 2 is shown in fig. 2, an electron microscope image of the separator obtained from the pulp obtained in comparative example 1 is shown in fig. 3, and it can be seen from fig. 1 that the aramid surface morphology is three-dimensional and the voids are uniform. As can be seen from FIG. 2, the aramid fiber extracted by the traditional solvent has smaller aperture and poorer three-dimensional property of a net structure. It can be seen from fig. 3 that the slurry after removal of water and alcohol shows almost no pore size.
TABLE 1
The data show that the diaphragm obtained from the aramid fiber slurry can uniformly form holes in the aramid fiber, the normal air permeability of the battery diaphragm is guaranteed, on the premise of the same thickness, compared with the diaphragm prepared from the traditional aramid fiber slurry, the diaphragm prepared from the aramid fiber slurry has the advantages that the air permeability increment is small, the shrinkage rate at 130 ℃/h is obviously reduced, the pore-forming effect is more three-dimensional than that of a solvent extraction pore, the manufacturing cost is reduced, and the original performance of the aramid fiber diaphragm can be improved.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The preparation method of the aramid fiber slurry is characterized by comprising the following steps of:
1) preparing a first solution and a second solution, wherein,
the first solution was prepared as follows: dissolving chloride salt in dimethylacetamide, adding meta-aramid fiber to obtain a first base material, stirring for 4-10 hours at 80-100 ℃ in a closed environment to dissolve the meta-aramid fiber in the dimethylacetamide to obtain a first solution, wherein the dimethylacetamide accounts for 70-78 wt% of the first base material, the meta-aramid fiber accounts for 18-22 wt% of the first base material, the chloride salt accounts for 1.2-8 wt% of the first base material, and the chloride salt is lithium chloride or calcium chloride;
the second solution was prepared as follows: uniformly mixing alumina and tripropylene glycol to obtain a second base material, and sanding the second base material by using a sand mill to ensure that the particle size of the second base material is D50: 0.9-1.2 μm and D90: 1.4-1.7 μm to obtain a second solution, wherein the alumina accounts for 45-55 wt% of the second base material by mass fraction;
2) mixing the first solution and dimethylacetamide, stirring uniformly, adding water, stirring uniformly, adding isopropanol, stirring uniformly, adding dimethyl carbonate, stirring uniformly, adding the second solution, and stirring uniformly to obtain the aramid fiber slurry, wherein the first solution accounts for 18-22 wt% of the aramid fiber slurry, the dimethylacetamide accounts for 15-20 wt% of the aramid fiber slurry in the step 2), the water accounts for 5-10 wt% of the aramid fiber slurry, the isopropanol accounts for 5-9 wt% of the aramid fiber slurry, the dimethyl carbonate accounts for 7-10 wt% of the aramid fiber slurry, and the second solution accounts for 34-40 wt% of the aramid fiber slurry.
2. The method for preparing according to claim 1, characterized in that, in the step 1), the second base stock is obtained by: mixing alumina and tripropylene glycol, then putting the mixture into a stirring tank, and stirring the mixture for 3 to 6 hours by adopting a double-planet stirrer, wherein the revolution of the stirring speed is 30 to 40r/min, and the rotation is 2000 to 2500 r/min.
3. The production method according to claim 2, characterized in that in the step 2), stirring is performed while adding the water;
in the step 2), mixing the first solution with dimethylacetamide, and stirring for 30-90 min until the mixture is uniform.
4. The method according to claim 3, wherein in the step 2), water is further added and then stirred for at least 30min until the homogenization.
5. The method according to claim 4, wherein in the step 2), the mixture is stirred for at least 30min after the addition of isopropanol until the homogenization.
6. The method according to claim 5, wherein in the step 2), the mixture is stirred for at least 30min after adding the dimethyl carbonate until the mixture is homogeneous.
7. The method according to claim 6, wherein in the step 2), the second solution is added and then stirred for at least 60min until the homogeneous state.
8. Aramid pulp obtained by the preparation method according to any one of claims 1 to 7.
9. A preparation method of the diaphragm, the aramid fiber slurry of claim 8 is coated on a base film, and water extraction is carried out to obtain the diaphragm.
10. Use of the aramid slurry as defined in claim 8 for improving pore-forming uniformity.
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| CN112490581B (en) * | 2020-10-28 | 2022-12-27 | 河北金力新能源科技股份有限公司 | Meta-aramid fiber and oil PDVF composite coating diaphragm and preparation method thereof |
| CN112909425A (en) * | 2021-01-20 | 2021-06-04 | 河北金力新能源科技股份有限公司 | High-efficiency long-life lithium-sulfur battery diaphragm and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102035043A (en) * | 2009-09-25 | 2011-04-27 | 上海比亚迪有限公司 | Polymer porous membrane, preparation method thereof, polymer electrolyte, polymer battery and preparation method of battery |
| KR20130073195A (en) * | 2011-12-23 | 2013-07-03 | 웅진케미칼 주식회사 | Menufacturing method of meta-aramid based porous membrane for secondary battery and porous membrane thereby |
| CN107170942A (en) * | 2017-06-01 | 2017-09-15 | 青岛中科华联新材料股份有限公司 | A kind of high-temperature resistant aramid fiber lithium ion battery composite separation membrane and preparation method thereof |
| CN108864930A (en) * | 2018-06-13 | 2018-11-23 | 河北金力新能源科技股份有限公司 | Aramid fiber lysate and preparation method thereof and aramid fiber diaphragm coating liquid and preparation method thereof and diaphragm |
| CN109181522A (en) * | 2018-07-17 | 2019-01-11 | 河北金力新能源科技股份有限公司 | Aramid fiber coating liquid, lithium ion battery separator and preparation method thereof |
-
2019
- 2019-07-01 CN CN201910586652.0A patent/CN110416473B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102035043A (en) * | 2009-09-25 | 2011-04-27 | 上海比亚迪有限公司 | Polymer porous membrane, preparation method thereof, polymer electrolyte, polymer battery and preparation method of battery |
| KR20130073195A (en) * | 2011-12-23 | 2013-07-03 | 웅진케미칼 주식회사 | Menufacturing method of meta-aramid based porous membrane for secondary battery and porous membrane thereby |
| CN107170942A (en) * | 2017-06-01 | 2017-09-15 | 青岛中科华联新材料股份有限公司 | A kind of high-temperature resistant aramid fiber lithium ion battery composite separation membrane and preparation method thereof |
| CN108864930A (en) * | 2018-06-13 | 2018-11-23 | 河北金力新能源科技股份有限公司 | Aramid fiber lysate and preparation method thereof and aramid fiber diaphragm coating liquid and preparation method thereof and diaphragm |
| CN109181522A (en) * | 2018-07-17 | 2019-01-11 | 河北金力新能源科技股份有限公司 | Aramid fiber coating liquid, lithium ion battery separator and preparation method thereof |
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