WO2023045312A1 - Membrane microporeuse à uniformité de pores élevée et son procédé de préparation, et batterie - Google Patents

Membrane microporeuse à uniformité de pores élevée et son procédé de préparation, et batterie Download PDF

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Publication number
WO2023045312A1
WO2023045312A1 PCT/CN2022/087611 CN2022087611W WO2023045312A1 WO 2023045312 A1 WO2023045312 A1 WO 2023045312A1 CN 2022087611 W CN2022087611 W CN 2022087611W WO 2023045312 A1 WO2023045312 A1 WO 2023045312A1
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Prior art keywords
microporous membrane
high pore
preparing
uniformity according
pore uniformity
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PCT/CN2022/087611
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English (en)
Chinese (zh)
Inventor
庄志
宫晓明
彭锟
李堃
虞少波
程跃
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Shanghai Energy New Materials Technology Co Ltd
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Shanghai Energy New Materials Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • H01M50/491—Porosity
    • 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

Definitions

  • the invention relates to the technical field of lithium battery separators, in particular to a microporous membrane with high pore uniformity and a preparation method thereof.
  • the diaphragm, polyethylene microporous membrane is mainly used in two ways, one is directly loaded between the positive and negative electrodes as a diaphragm; the other One is used as a diaphragm and then coated with ceramics, boehmite, PVDF, aramid fiber, etc. twice to enhance its own heat resistance, and then loaded between the positive and negative electrodes.
  • the ion channel between the positive and negative electrodes is provided by the polyethylene microporous membrane.
  • the requirement of high energy density of the battery has required the separator to be continuously thinned in recent years, and the polyethylene microporous membrane itself is required to have high acupuncture strength, high tensile strength, low closed cell temperature, etc. to protect the lithium battery.
  • lithium ions will not be precipitated at the negative electrode corresponding to the position with more pores and larger, and accumulate to form the negative electrode Lithium dendrites grow after full-load embedding, thereby piercing the polyethylene microporous membrane to form a short circuit; 2.
  • Lithium dendrites grow after full-load embedding, thereby piercing the polyethylene microporous membrane to form a short circuit; 2.
  • excessive heat will be generated and thermal runaway will occur.
  • the uniformity of the pores of the polyethylene microporous membrane itself is very important.
  • the preparation process includes: heating polyolefin and hole-forming solvent on an extruder until melting. After passing through the T-shaped die head, there are multiple groups of cooling rollers that pass through chilled water/cooling water, and then form thin sheets after cooling. Afterwards, the temperature is raised and stretched along the MD (along the production line direction) direction. Then stretch along the TD (vertical line) direction, remove the porogen, and stretch along at least one axial direction again to obtain a polyethylene microporous membrane. Whether it is MD roller extrusion stretching or TD double-side clamping stretching, they are all high-speed stretching.
  • the polyethylene microporous membrane has an intricate internal pore structure, which is soft and easily damaged at high temperatures.
  • the object of the present invention is to provide a method for preparing a microporous membrane with high pore uniformity, comprising the following steps:
  • the surface of the degreasing roller described in step (3) has a microporous flow channel, and a hollow pipe and a heating coil are arranged in the center; the hollow pipe is connected with the microporous flow channel on the roller surface, and the outside is connected with a vacuum pump; the heating The coils are connected to an external heat exchange station.
  • the pore diameter of the microporous channel is ⁇ 1.0mm.
  • the pore diameter of the microporous channel is ⁇ 0.01mm.
  • the area of the micropore flow channel on the surface of the degreasing roller accounts for ⁇ 50% of the total surface area of the degreasing roller.
  • the area of the micropore flow channel on the surface of the degreasing roller accounts for more than 80% of the total surface area of the degreasing roller.
  • the vacuum degree inside the degreasing roller is ⁇ 0.05Mpa.
  • the vacuum inside the degreasing roller is ⁇ 0.08Mpa.
  • the wrap angle between the surface of the degreasing roller and the sheet is ⁇ 60°.
  • the wrap angle between the surface of the degreasing roller and the sheet is ⁇ 180°.
  • the heating temperature of the degreasing roller is ⁇ 60°C and ⁇ 100°C.
  • the heating temperature of the degreasing roller is ⁇ 80°C and ⁇ 100°C.
  • the number of the degreasing rollers is ⁇ 4.
  • the number of the degreasing rollers is more than or equal to 8.
  • the residual oil rate of the thin slices is ⁇ 20%.
  • step (3) the residual oil rate of the thin slices is ⁇ 2%.
  • an extraction process is also included, and the extraction process is located before or after step (4).
  • the purpose of the present invention is to also provide a microporous membrane with high pore uniformity, the microporous membrane is a polyolefin diaphragm, and the pore diameter is tested by the bubble point method, and the ratio of the maximum pore diameter to the median pore diameter is ⁇ 1.3.
  • the median pore diameter of the polyolefin membrane ranges from 25 to 30 nm.
  • the maximum pore diameter of the polyolefin membrane ranges from 26 to 39 nm.
  • the bubble point method is used to test the pore size, and the ratio of the maximum pore size to the median pore size is ⁇ 1.05.
  • the porosity of the polyolefin membrane is ⁇ 30%.
  • the surface resistivity of the polyolefin membrane is ⁇ 0.05 ⁇ *cm2.
  • polyolefin diaphragm is a single-component polyethylene diaphragm.
  • the purpose of the present invention is also to provide a battery comprising any one of the above-mentioned high-porosity uniform microporous membranes as an element separating positive and negative poles.
  • the present invention has the following beneficial effects:
  • the invention provides a method for preparing a high-porosity uniform microporous membrane.
  • a large amount of pore-forming agent previously extracted in the process can be directly added to the finished product tank of the pore-forming agent for reuse after simple filtration, and can be It greatly reduces the amount of extraction agent used in the later extraction process, and also reduces the energy consumption of the separation of the extraction agent and the pore-forming agent, and avoids the oxidation caused by the secondary thermal processing (MD+TD or SBS) of the pore-forming agent After the quality declines, it cannot be used again, which greatly reduces the production cost and raw material cost.
  • MD+TD or SBS secondary thermal processing
  • Fig. 1 is the structural sectional schematic diagram of oil pumping roller of the present invention
  • Fig. 2 is a side view of the structure of the oil sucking roller of the present invention.
  • Fig. 3 is a flow chart of the oil pumping section of the present invention.
  • Fig. 4 is the normal process flow diagram of diaphragm preparation in the prior art
  • Fig. 5 is a flow chart of a diaphragm preparation process according to an embodiment of the present invention.
  • the specific embodiment of the present invention provides a method for preparing a high-porosity uniform microporous membrane, comprising the following steps:
  • the surface of the degreasing roller 1 described in step (3) has a microporous flow channel 2, and a hollow pipe 3 and a heating coil 4 are arranged in the center;
  • the vacuum machine is connected;
  • the heating coil 4 is connected with an external heat exchange station.
  • the hollow pipe 3 is connected to the microporous flow channel 2 extending to the surface of the degreasing roller 1, and the pipe is borrowed from a vacuum pump to assume a negative pressure state.
  • a heating coil 4 inside the degreasing roller 1, which is connected to an external heat exchange station Roller 1 can be heated.
  • the pore-forming agent inside the sheet in contact with it can be preheated and softened, and after the viscosity is reduced, it is forced to be sucked out.
  • the pore-forming agent is selected from one or more of liquid paraffin, mineral oil, soybean oil, and white oil.
  • the pore diameter of the microporous channel 2 is ⁇ 1.0mm.
  • the pore diameter of the microporous channel 2 is ⁇ 0.01 mm.
  • holes with smaller diameters are preferred, so that the sheet is supported by more structures on the surface of the roller, avoiding excessive suction of a single hole, and more uniform suction, thereby ensuring a smaller probability of force deformation of the sheet and more uniform suction of the pore-forming agent.
  • the area of the micropore channel 2 on the surface of the degreasing roller 1 accounts for ⁇ 50% of the total surface area of the degreasing roller 1 .
  • the area of the microporous channels 2 on the surface of the degreasing roller 1 accounts for ⁇ 80% of the total surface area of the degreasing roller 1 .
  • the degreasing roller 1 has multiple sets of microporous flow channels 2 on the surface, and the area occupied by the larger microporous flow channels 2 is preferred in order to have a larger suction area, thereby ensuring faster suction of the pore forming agent.
  • the vacuum degree inside the degreasing roller 1 is ⁇ 0.05Mpa.
  • the vacuum degree inside the degreasing roller 1 is ⁇ 0.08Mpa.
  • a greater degree of vacuum is preferred to ensure that the sheet receives sufficient suction, thereby ensuring that the porogen is more fully sucked out.
  • the wrap angle between the roll surface of the degreasing roller 1 and the sheet is ⁇ 60°.
  • the wrap angle between the roll surface of the degreasing roller 1 and the sheet is ⁇ 180°.
  • a larger wrap angle is preferred to expand a larger contact area, and at the same rotational speed, increase the extraction time of the porogen.
  • the heating temperature of the degreasing roller 1 is ⁇ 60°C and ⁇ 100°C.
  • the heating temperature of the degreasing roller 1 is ⁇ 80°C and ⁇ 100°C.
  • a higher temperature to preheat the pore-forming agent can reduce the kinematic viscosity of the pore-forming agent, so that the pore-forming agent can be removed more thoroughly under a fixed suction.
  • the number of said degreasing rollers is more than or equal to 4. Preferably, the number of said degreasing rollers is more than or equal to 8.
  • the residual oil rate of the thin slices is ⁇ 20%.
  • the residual oil rate of the thin slice is ⁇ 2%.
  • an extraction process S5 is also included, and the extraction process S5 is located before or after step (4).
  • step (4) is asynchronous biaxial stretching (MD+TD) or synchronous biaxial stretching (SBS).
  • microporous membrane is a polyolefin separator.
  • the pore size of the polyolefin membrane is tested by the bubble point method, and the ratio of the maximum pore size to the median pore size is ⁇ 1.30.
  • the ratio of the maximum pore diameter to the median pore diameter is ⁇ 1.05.
  • the median pore diameter of the polyolefin membrane ranges from 25 to 30 nm.
  • the maximum pore diameter of the polyolefin membrane ranges from 26 to 39 nm.
  • the porosity of the polyolefin membrane is ⁇ 30%.
  • the surface resistivity of the polyolefin membrane is ⁇ 0.05 ⁇ *cm2.
  • the needle punch strength of the polyolefin membrane is between 1000-1500gf.
  • the bidirectional tensile strength of the polyolefin separator is between 4100-4350kgf/cm2.
  • the elongation of the polyolefin separator is 40-70% in the MD direction and 50-65% in the TD direction.
  • the thermal shrinkage rate of the polyolefin separator is ⁇ 2.7% in the MD direction and ⁇ 1.0 in the TD direction under the conditions of 110°C and 1 hour.
  • polyolefin membrane is a single-component polyethylene membrane.
  • the instrument used is Capillary Flow Porometer (CFP 1500AE) from PMI, and the surface tension of the infiltration fluid is 15.9 Dynes/cm.
  • the median pore diameter ( ⁇ mean) is obtained from the semi-dry curve of the "dry-wet method". Both the maximum pore size and the minimum pore size can be obtained from the pore size distribution diagram obtained from this test.
  • the maximum pore size ( ⁇ max) is the last value in the pore size distribution graph data, which is the pore size corresponding to the bubble point.
  • a kinematic viscosity measuring instrument DSY-004 Use a kinematic viscosity measuring instrument DSY-004, set the measurement temperature to 60°C, and measure the kinematic viscosity after stabilizing for 1 hour.
  • Standard ambient temperature for testing (23 ⁇ 2)°C.
  • GB/T 36363-2018 stipulates that the number of tests for each sample is 4. In order to further improve the accuracy, it is stipulated that the number of samples for each test should be no less than 4, generally 5. Cut out 5 diaphragms that match the resistance test mold (slightly larger than the mold size), and put the diaphragm into lithium hexafluorophosphate (LiPF6), ethylene carbonate (EC), ethyl methyl carbonate (EMC) carbonate with a concentration of 1.0mol/L Dimethyl ester (DMC) in the electrolyte solution with a volume of 1:1:1, keep sealed, soak for 2h.
  • LiPF6 lithium hexafluorophosphate
  • EC ethylene carbonate
  • EMC ethyl methyl carbonate
  • R Resistance value of a layer of diaphragm, in ohms ( ⁇ );
  • IR The ionic resistivity of the diaphragm, in ohms per square centimeter ( ⁇ *cm2);
  • R Resistance value of a layer of diaphragm, in ohms ( ⁇ );
  • Polyethylene with Mw of 1.0 ⁇ 10 6 and white oil were used as raw materials. Put 20% polyethylene and 80% white oil into a twin-screw extruder, extrude through a T-die at 150°C, and be cooled by a cold roll at a temperature of 5°C. After that, flakes are formed.
  • the area of the surface micropore flow channel 2 accounts for 50% of the total surface area of the degreasing roller 1, the wrapping angle between the roller surface and the sheet is 60°, and the vacuum degree inside the roller is 0.05.
  • Mpa the degreasing roller 1 with a temperature of 60°C and four rollers, and step S3 thereof. Then enter MD stretching, and perform 10 times stretching at 110°C. Enter TD1 stretching, and perform 10-fold stretching at 110°C. After extraction S5, it enters TD2 stretching S6, and performs 2 times stretching and setting at 120°C.
  • the area of the surface micropore flow channel 2 accounts for 60% of the total surface area of the degreasing roller 1, the wrap angle between the roller surface and the sheet is 80°, and the vacuum degree in the roller is 0.06Mpa, the temperature is 70°C, and the degreasing roller 1 with 5 rollers and its step S3, other experimental conditions are the same as those in Example 1.
  • the area of the surface micropore flow channel 2 accounts for 70% of the total surface area of the degreasing roller 1, the wrap angle between the roller surface and the sheet is 120°, and the vacuum degree in the roller is 0.07Mpa, the temperature is 80°C, and the degreasing roller 1 with 6 rollers and its step S3, other experimental conditions are the same as those in Example 1.
  • the area of the surface micropore flow channel 2 accounts for 80% of the total surface area of the degreasing roller 1, the wrap angle between the roller surface and the sheet is 140°, and the vacuum degree in the roller is 0.08Mpa, the temperature is 90°C, and the degreasing roller 1 with 7 rollers and its step S3, other experimental conditions are the same as those in Example 1.
  • the area of the surface micropore flow channel 2 accounts for 85% of the total surface area of the degreasing roller 1, the wrap angle between the roller surface and the sheet is 160°, and the vacuum degree in the roller is 0.09Mpa, the temperature is 95°C, and the degreasing roller 1 with 8 rollers and its step S3, the other experimental conditions are the same as those in Example 1.
  • the area of the surface micropore flow channel 2 accounts for 90% of the total surface area of the degreasing roller 1, the wrap angle between the roller surface and the sheet is 180°, and the vacuum degree in the roller is 0.09Mpa, the temperature is 100°C, and the degreasing roller 1 with 9 rollers and its step S3, other experimental conditions are the same as those in Example 1.
  • Polyethylene with Mw of 1.0 ⁇ 10 6 and white oil were used as raw materials. Put 20% polyethylene and 80% white oil into a twin-screw extruder, extrude through a T-die at 150°C, and be cooled by a cold roll at a temperature of 5°C. After that, flakes are formed. Enter MD stretching, and perform 10-fold stretching at 110°C. Enter TD1 stretching, and perform 10-fold stretching at 110°C. After extraction S5, it enters TD2 stretching S6, and performs 2 times stretching and setting at 120°C.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

La présente invention concerne le domaine technique des séparateurs de batterie au lithium, et concerne spécifiquement un procédé de préparation d'une membrane microporeuse ayant une uniformité de pores élevée. La méthode comprend les étapes suivantes : (1) mélanger et chauffer une polyoléfine et un agent porogène à un état fondu ; (2) permettre au mélange de passer à travers une tête de filière et être refroidi pour former une feuille ; (3) permettre à la feuille de passer à travers un rouleau d'élimination d'huile pour aspirer l'agent de formation de pores à l'intérieur de la feuille ; (4) chauffer et étirer la feuille dans au moins une direction axiale ; (5) étirer la feuille à nouveau pour la mise en forme dans au moins une direction axiale ; et (6) laminer pour obtenir la membrane microporeuse avec une uniformité de pores élevée. Dans l'étape (3), le rouleau d'élimination d'huile comportant des canaux d'écoulement microporeux dans sa surface, et comportant un tuyau creux et une bobine de chauffage au centre de ceux-ci ; le tuyau creux est relié aux canaux d'écoulement microporeux dans la surface de rouleau, et est relié à l'extérieur à une machine de pompage sous vide ; et la bobine de chauffage est reliée à une station d'échange de chaleur externe. Le séparateur préparé par le procédé présente les caractéristiques d'une faible porosité, d'une uniformité de pores extrêmement élevée, d'un faible taux de résistance de surface et d'une valeur D extrêmement élevée (D = résistance/épaisseur de pénétration des ongles).
PCT/CN2022/087611 2021-09-26 2022-04-19 Membrane microporeuse à uniformité de pores élevée et son procédé de préparation, et batterie Ceased WO2023045312A1 (fr)

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CN113904059A (zh) * 2021-09-26 2022-01-07 上海恩捷新材料科技有限公司 一种高孔均匀性微多孔膜及其制备方法、电池
CN115805717A (zh) * 2022-10-31 2023-03-17 武汉惠强新能源材料科技有限公司 一种湿法隔离膜拉伸防断裂装置

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