CN111081948A - Preparation method of high linear velocity-large width polyethylene diaphragm - Google Patents
Preparation method of high linear velocity-large width polyethylene diaphragm Download PDFInfo
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- CN111081948A CN111081948A CN201911365800.2A CN201911365800A CN111081948A CN 111081948 A CN111081948 A CN 111081948A CN 201911365800 A CN201911365800 A CN 201911365800A CN 111081948 A CN111081948 A CN 111081948A
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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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- 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 belongs to the field of battery diaphragm preparation, and particularly relates to a preparation method of a high linear velocity-large width polyethylene diaphragm, which comprises the following steps: s1, blending and extruding; s2, pre-extraction: soaking the gel sheet obtained in the step S1 in an extracting agent, extracting to remove 20-40% of paraffin oil in micropores of the gel sheet, and drying to remove the extracting agent to obtain a surface pre-extracted gel sheet; s3, biaxial stretching: s4, extraction: soaking the primary membrane in the step S3 in an extracting agent, extracting to remove paraffin oil in micropores of the primary membrane, and then drying to remove the extracting agent; s5, heat setting, rolling and slitting: and (5) carrying out heat setting, rolling and slitting on the diaphragm obtained in the step S4 to obtain a finished product. Through the processes of pre-extraction, biaxial stretching and extraction, the diluent is more completely extracted, the residual quantity is less, the extraction time is greatly shortened, the extraction efficiency is improved, and the production of high linear speed and large-width diaphragms can be met.
Description
Technical Field
The invention relates to the field of battery diaphragm preparation, in particular to a preparation method of a high linear speed-large width polyethylene diaphragm.
Background
In the construction of lithium batteries, the separator is one of the key internal layer components. Most of current battery separators are polyethylene composition films with microporous structures, the performance of the current battery separators determines the interface structure, internal resistance and the like of a battery, the characteristics of the battery such as capacity, circulation and safety performance are directly influenced, and the battery separators with excellent performance play an important role in improving the comprehensive performance of the battery. In the existing preparation method of the polyethylene composition diaphragm, a wet method is commonly used for preparing the diaphragm, high-boiling-point micromolecules are used as a diluent to be added into the polyethylene composition, the mixture is heated and melted into a uniform system, then the temperature is reduced to generate phase separation, the micromolecules are extracted by an organic solvent after the bidirectional stretching, and the mutually communicated microporous diaphragm is prepared.
Chinese patent No. CN201010587499.2 discloses a method and a system for preparing a power lithium ion battery diaphragm, wherein the system for preparing the power lithium ion battery diaphragm comprises a stirring device, an extrusion device, a cooling forming device, a bidirectional stretching device, an extraction device, a transverse stretching device and a heat treatment device, and the stirring device, the extrusion device, the cooling forming device, the bidirectional stretching device, the extraction device, the transverse stretching device and the heat treatment device are sequentially connected. The mineral oil in the diaphragm is extracted by adopting the method, the extraction is easy to be incomplete, and the residual mineral oil on the diaphragm can not be fully volatilized, so that the porosity and the air permeability of the battery diaphragm are low, and the performance of the battery diaphragm and the microporous structure of the diaphragm are influenced; secondly, the diaphragm production line adopts a first-stretching and then-extracting process, so that the speed of the production line is 30-50m/min and the width is about 3-4.5 m due to the limitation of extraction efficiency and the influence of paraffin oil on longitudinal stretching, and the great increase of the production line speed is restricted.
Disclosure of Invention
The invention provides a preparation method of a high linear speed-large width polyethylene diaphragm, which is realized by the following technology.
A preparation method of a polyethylene diaphragm with high linear speed and large width comprises the following steps:
s1, blending and extruding: uniformly mixing polyethylene and a diluent, then carrying out melt extrusion, and cooling and forming to obtain a gel sheet;
s2, pre-extraction: soaking the gel sheet obtained in the step S1 in an extracting agent, extracting to remove 20-40% of paraffin oil in micropores of the gel sheet, and drying to remove the extracting agent to obtain a surface pre-extracted gel sheet;
s3, biaxial stretching: sequentially longitudinally stretching and transversely stretching the surface pre-extraction gel sheet obtained in the step S2 to obtain a primary film;
s4, extraction: soaking the primary membrane in the step S3 in an extracting agent, extracting to remove paraffin oil in micropores of the primary membrane, and then drying to remove the extracting agent;
s5, heat setting, rolling and slitting: and (5) carrying out heat setting, rolling and slitting on the diaphragm obtained in the step S4 to obtain a finished product.
The scheme is adopted: extracting the intercrystalline diluent on the surface of the gel sheet to form micropores through pre-extraction, further enlarging the original micropores through stretching, so that a compact layer on the surface of the diaphragm is broken, and the thickness of a skin layer is effectively reduced; and the inner layer contains a large amount of diluents in the membrane in the stretching process, so that the plasticity is increased, in the stretching process, small droplets of the diluents are gathered into large droplets, and mineral oil is extracted out to form holes after the stretching is finished. Secondly, the pre-extraction firstly removes the intercrystalline diluent on the surface of the gel sheet, the diluent in the spherulites is stretched and transferred, the mobility is increased, and then the secondary extraction is carried out, so that the diluent is more completely extracted, and the residual quantity is less. Moreover, the high diluent content is not beneficial to longitudinal stretching, and the diluent content is properly reduced, so that the longitudinal stretching speed can be increased, and the production speed is increased.
Further, in step S2, 25-35% of paraffin oil in the pores of the gel sheet is removed by extraction.
Further, in step S2, the total volume of the extracting agent is 40-100m3The circulation amount of the extracting agent is 1-8m3/h。
Further, in step S2, step SThe total volume of the extracting agent is 50-80m3The circulation amount of the extracting agent is 2-6m3/h。
The amount of the paraffin oil is accurately removed by controlling the using amount and the circulating amount of the extracting agent, when the using amount of the extracting agent is small or the circulating amount is low, the removing amount of the paraffin oil is lower than 20%, and when the using amount of the extracting agent is large or the circulating amount is high, on one hand, the removing amount of the paraffin oil is higher than 20%, on the other hand, a large amount of waste of the extracting agent is caused, and the production cost is increased.
Further, in step S3, the longitudinal stretching is: continuously stretching at the temperature of 50-130 ℃ at multiple points, wherein the total stretching ratio is 7-20 times, and obtaining a longitudinal stretching film with the thickness of 100-; the length of the roller for longitudinal stretching is 2000mm and the diameter of the roller is 800mm and 250 mm.
Further, in step S3, the transverse stretching is: sequentially stretching at the temperature of 100 ℃ and 130 ℃ in multiple stages, wherein the total stretching ratio is 7-20 times, and obtaining a primary film with the thickness of 5-60 mu m; the track width of the transverse stretching is 500-12000 mm.
The longitudinal and transverse stretching multiplying power is controlled, so that the crystallization orientation uniformity of the polymer chain is improved, the micropore rearrangement homogenization degree is improved, and a net structure with uniform pore size distribution is obtained.
Further, in step S4, the total volume of the extractant is 200-600m3The circulation amount of the extracting agent is 4-15m3/h。
Further, in step S4, the total volume of the extractant is 250-450m3The circulation amount of the extracting agent is 6-12m3/h。
Further, in step S2 and step S4, dichloromethane is used as the extractant.
Further, in step S5, the heat setting temperature is 100-150 ℃, and the heat setting stretching magnification is 1.2-3 times, so as to obtain the polyethylene diaphragm with the thickness of 5-40 μm, and the track width of the transverse stretching is 7000-15000 mm. The secondary crystallization rearrangement is carried out through heat setting to eliminate residual stress, so that the size stability of the micropores is improved, but the fusion of the micropores at high temperature can be caused by overhigh heat setting temperature, the pore diameter and the number of the micropores of the microporous membrane are reduced, and the service performance of the lithium ion battery is influenced, so that the preferable temperature is 120-130 ℃.
Further, in step S5, the winding speed is 300m/min at 100-.
Further, in step S1, the diluent accounts for 60 to 90% of the total weight, and the polyethylene accounts for 10 to 40% of the total weight; wherein the diluent is paraffin oil, and the molecular weight of the paraffin oil is 300-1500; the polyethylene comprises ultra-high molecular weight polyethylene (PE1) with average molecular weight of 1 × 10 and high density polyethylene resin6-4×106High density polyethylene resin (PE2) having an average molecular weight of 5X 105-8×105The addition amount of the PE1 and the PE2 is 5:5-95 in mass ratio.
Further, in step S1, the extrusion temperature is 150 ℃ and 250 ℃, and the melt at 190 ℃ and 250 ℃ is obtained by melt extrusion.
Further, in step S1, the cooling forming process includes: cooling the melt at the temperature of 190-250 ℃ to be a gel sheet at the temperature of 20-50 ℃ by a casting sheet, wherein the length of a casting sheet clamping roller and a casting sheet roller for casting the sheet is 2000mm, the diameter of the roller is 300-1500mm, and the diameter ratio of the casting sheet roller/the casting sheet clamping roller is 1.5-5.0.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the processes of pre-extraction, biaxial stretching and extraction, the diluent on the surface is removed by pre-extraction, the diluent in the interior is stretched and transferred, the mobility is increased, and then secondary extraction is carried out, so that the diluent is more completely extracted, the residual quantity is small, the extraction time is greatly shortened, the extraction efficiency is improved, and the production of the diaphragm with high linear velocity (100 + 300m/min) and large width (5-10m) can be met.
2. Micropores are formed on the surface of the gel sheet through pre-extraction, and the original micropores are further enlarged through stretching, so that the thickness of the skin layer of the diaphragm is effectively reduced; the diluent of the inner layer can better control the size and the shape of the micropores of the surface and the inner layer due to the fact that the occupied space is increased and the size growth range of liquid drops is reduced, so that the pore size distribution of the micropores formed by the whole diaphragm is narrow, the porosity is large, the pore size is uniform, and the porosity and the air permeability of the battery diaphragm are improved.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
S1, mixing 30% of polyethylene and 70% of diluent uniformly, carrying out melt extrusion at 200 ℃ through a double-screw co-rotating extruder to obtain a melt at 220 ℃, then carrying out casting sheet processing through a casting sheet clamping roller and a casting sheet roller to ensure that the melt is cooled into a gel sheet at 35 ℃ after casting sheets, wherein the roller length of the casting sheet clamping roller is 1500mm, the roller diameter is 300mm, the roller length of the casting sheet roller is 1500mm, the roller diameter is 900mm, and the diameter ratio of the casting sheet roller to the casting sheet clamping roller is 3.0;
wherein the diluent is solid or liquid paraffin oil, and the molecular weight of the paraffin oil is 300-1500; the polyethylene comprises ultra-high molecular weight polyethylene (PE1) with average molecular weight of 1 × 10 and high density polyethylene resin6-4×106High density polyethylene resin (PE2) having an average molecular weight of 5X 105-8×105The addition amount of PE1 and PE2 is 5:45 in mass ratio;
s2, the gel sheet in the step S1 passes through mutually communicated extraction grooves in sequence under the traction of a roller, the number of the extraction grooves is 1, 20% of paraffin oil in micropores of the gel sheet is removed by using dichloromethane in the extraction grooves in an extraction mode, dichloromethane is removed by drying, the surface pre-extraction gel sheet is obtained, and the total volume of the dichloromethane in the extraction grooves is 40m3The circulating amount of dichloromethane is 1m3H, the length of a roller in the pre-extraction procedure is 1500mm, and the diameter of the roller is 300 mm;
s3, biaxial stretching: sequentially longitudinally stretching and transversely stretching the surface pre-extraction gel sheet obtained in the step S2 to obtain a primary film; the longitudinal stretching is continuous multipoint stretching at the temperature of 100 ℃, and the total stretching multiplying power is 10 times to obtain a longitudinal stretching film with the thickness of 450 mu m; the length of the longitudinally stretched roller is 1500mm, and the diameter of the roller is 500 mm; the transverse stretching is successive multi-stage stretching at the temperature of 120 ℃, and the total stretching ratio is 10 times to obtain a primary film with the thickness of 45 mu m; the width of the transverse stretching track is 1000 mm;
s4, extraction: the primary membrane of the step S3 passes through mutually communicated extraction tanks in turn under the traction of a roller, the number of the extraction tanks is 15, the paraffin oil in the micropores of the diaphragm is washed by dichloromethane, the dichloromethane is removed by drying, and the total volume of the dichloromethane in the extraction tank is 200m3The circulating amount of dichloromethane is 15m3The length of a roller in the extraction procedure is 10000mm, and the diameter of the roller is 350 mm;
s5, heat setting, rolling and slitting: and (2) performing heat setting and stretching at 150 ℃ on the diaphragm obtained in the step S4 at the temperature of 100-.
Experiments show that the selection of the roller length, the roller diameter and the track width in the steps S1-S5 within the protection range of the invention can realize the preparation of the diaphragm with high linear speed (150-600m/min) and large width (5-10 m); next, when the raw material proportioning, the melt extrusion and cooling molding process in step S1, the longitudinal stretching and transverse stretching process in step S3, and the heat setting process in step S5 are selected within the protection scope of the present invention, the influence on the production efficiency of the separator is small, and therefore, the above parameters are not discussed in the following examples.
Example 2
Example 2 is essentially the same as example 1, except that:
s2, pre-extraction: the number of the extraction tanks is 2, 25 percent of paraffin oil in the micropores of the gel sheet is removed by using dichloromethane extraction in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 50m3The circulating amount of dichloromethane is 2m3/h；
S4, extraction: the number of the extraction tanks is 12, and the total volume of the dichloromethane in the extraction tanks is 250m3The circulating amount of dichloromethane is 12m3/h。
Example 3
Example 3 is essentially the same as example 1, except that:
s2, pre-extraction: the number of the extraction tanks is 1, 30 percent of paraffin oil in the micropores of the gel sheet is removed by using dichloromethane extraction in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 65m3The circulating amount of dichloromethane is 4m3/h；
S4, extraction: the number of the extraction tanks is 10, and the total volume of the dichloromethane in the extraction tanks is 320m3The circulating amount of dichloromethane is 9m3/h。
Example 4
Example 4 is essentially the same as example 1, except that:
s2, pre-extraction: the number of the extraction tanks is 4, 35 percent of paraffin oil in the micropores of the gel sheet is removed by using dichloromethane extraction in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 80m3The circulating amount of dichloromethane is 6m3/h；
S4, extraction: the number of the extraction tanks is 8, and the total volume of the dichloromethane in the extraction tanks is 450m3The circulating amount of dichloromethane is 6m3/h。
Example 5
Example 5 is essentially the same as example 1, except that:
s2, pre-extraction: the number of the extraction tanks is 6, 40 percent of paraffin oil in the micropores of the gel sheet is removed by using dichloromethane extraction in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 100m3The circulating amount of dichloromethane is 8m3/h；
S4, extraction: the number of the extraction tanks is 6, and the total volume of the dichloromethane in the extraction tanks is 600m3The circulating amount of dichloromethane is 4m3/h。
Comparative example 1
Comparative example 1 differs from example 3 in that: step S2 and the pre-extraction process are not needed, and the production line speed adopts the diaphragm width of 3000 and 5000mm and the linear speed of 30-50 m/min.
Comparative example 2
Comparative example 2 differs from example 3 in that: step S2 and the pre-extraction process are not needed, and the production line speed adopts the diaphragm width of 5000-.
Comparative example 3
Comparative example 3 differs from example 3 in that: s2, pre-extraction: the number of the extraction tanks is 3, 10 percent of paraffin oil in the micropores of the gel sheet is removed by extracting with dichloromethane in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 20m3The circulating amount of dichloromethane is 4m3/h。
Comparative example 4
Comparative example 4 differs from example 3 in that: s2, pre-extraction: the number of the extraction tanks is 3, 50 percent of paraffin oil in the micropores of the gel sheet is removed by extracting with dichloromethane in the extraction tanks, and the total volume of the dichloromethane in the extraction tanks is 100m3The circulating amount of dichloromethane is 4m3/h。
Application example
The performance of the polyethylene separators prepared in examples 1 to 5 and comparative examples 1 to 4 was measured; the residual oil rate is determined by a weighing method; the porosity aperture size is tested by adopting a JW-BK200 type aperture tester; air permeability Using a Gurley model 4110 air permeameter, according to ASTM D726, at a pressure of 20Kgf/cm2Air permeability is characterized according to the time taken to pass through a volume of 100mL of air under the conditions; the results are shown in Table 1.
Table 1 performance test results of polyethylene separator
The size and the form of the micropore structure are closely related to the content and the distribution condition of paraffin oil, and the method 1-5 is adopted, namely, the diaphragm prepared when the content of the pre-extracted paraffin oil accounts for 20-40 percent, the formed micropores have narrow pore size distribution, the average pore size is 0.05-0.5 mu m, the porosity is 50-60 percent, the pore size is uniform, the porosity is high, and the air permeability is good; most of the residual paraffin oil exists in the spherulites, a certain plasticizing effect is presented in the stretching process, the stretching stress is reduced, the diaphragm is easy to stretch, and the production line speed is greatly improved; preferably, the pre-extracted paraffin oil content is 25-35%. When the pre-extracted paraffin oil content is high, such as increased to the range of comparative example 4, that is, the residual paraffin oil content is low, the required stress is higher when the stretching degree is the same as that of example 3 due to the low paraffin oil content and the large longitudinal stretching and transverse stretching stress, and the spherulite stretching deformation occurs at high multiplying power; and the support of paraffin oil is lacked, so that the hole collapse phenomenon is easy to occur, and the pore size distribution range is wide. When the content of the pre-extracted paraffin oil is low, if the content is reduced to the range of the comparative example 3, the thickness of the skin layer is large, the pore diameters of the surface layer and the inner layer are inconsistent, and after the production is finished, the content of the residual paraffin oil of the diaphragm is slightly high, so that the performance of the diaphragm is not improved. Therefore, only if the pre-extracted paraffin oil content is in a proper range, a diaphragm with good performance can be obtained, and meanwhile, the production speed is improved. Compared with the examples 1-5, the production is carried out under the conventional speed condition, and the cost of the diaphragm is higher; when the production speed is increased, like the comparative example 2, under the same extraction time, the paraffin oil of the comparative example 2 is incompletely extracted, part of micropores are blocked by the paraffin oil, the pore distribution is not uniform, the air permeability of the diaphragm is poor, and when the extraction efficiency similar to that of the example 3 is to be achieved, the extraction time is greatly prolonged and is about 2 times of the total extraction time of the example 3, and the consumption of the extracting agent is also greatly increased.
Claims (10)
1. A preparation method of a polyethylene diaphragm with high linear speed and large width is characterized by comprising the following steps:
s1, blending and extruding: uniformly mixing polyethylene and a diluent, then carrying out melt extrusion, and cooling and forming to obtain a gel sheet;
s2, pre-extraction: soaking the gel sheet obtained in the step S1 in an extracting agent, extracting to remove 20-40% of paraffin oil in micropores of the gel sheet, and drying to remove the extracting agent to obtain a surface pre-extracted gel sheet;
s3, biaxial stretching: sequentially longitudinally stretching and transversely stretching the surface pre-extraction gel sheet obtained in the step S2 to obtain a primary film;
s4, extraction: soaking the primary membrane in the step S3 in an extracting agent, extracting to remove paraffin oil in micropores of the primary membrane, and then drying to remove the extracting agent;
s5, heat setting, rolling and slitting: and (5) carrying out heat setting, rolling and slitting on the diaphragm obtained in the step S4 to obtain a finished product.
2. The method for preparing a polyethylene separator having high line speed and large width according to claim 1, wherein 25-35% of paraffin oil in the pores of the gel sheet is removed by extraction in step S2.
3. The method for preparing polyethylene membrane with high linear velocity and large breadth according to claim 1, wherein in step S2, the total volume of the extractant is 40-100m3The circulation amount of the extracting agent is 1-8m3/h。
4. The method for preparing polyethylene membrane with high linear velocity and large breadth according to claim 3, wherein in step S2, the total volume of the extractant is 50-80m3The circulation amount of the extracting agent is 2-6m3/h。
5. The method for preparing a polyethylene separator having high line speed and large width according to claim 1, wherein the longitudinal stretching in step S3 is: continuously stretching at the temperature of 50-130 ℃ at multiple points, wherein the total stretching ratio is 7-20 times, and obtaining the longitudinal stretching film with the thickness of 100-.
6. The method for preparing a high line speed-large width polyethylene separator according to claim 1, wherein in step S3, the transverse stretching is: sequentially stretching at the temperature of 100-130 ℃ in multiple stages with the total stretching ratio of 7-20 times to obtain an initial film with the thickness of 5-60 mu m, wherein the track width of the transverse stretching is 500-12000 mm.
7. The method for preparing polyethylene diaphragm with high linear velocity and large width as claimed in claim 1, wherein in step S4, the total volume of the extractant is 200-600m3The circulation amount of the extracting agent is 4-15m3/h。
8. The method for preparing high linear velocity-large width polyethylene membrane as claimed in claim 7, wherein in step S4, the total volume of the extractant is 250-450m3The circulation amount of the extracting agent is 6-12m3/h。
9. The method for preparing the high linear velocity-large width polyethylene membrane as claimed in claim 1, wherein in step S5, the heat setting temperature is 100-150 ℃, the heat setting stretching ratio is 1.2-3 times, and a polyethylene membrane with the thickness of 5-40 μm is obtained, and the track width of the transverse stretching is 7000-15000 mm.
10. The method for preparing a high linear velocity-large width polyethylene membrane as claimed in claim 1, wherein the winding speed is 100-300m/min, the slitting speed is 150-600m/min, and the speed ratio of the slitting speed to the winding speed is 1.5-5.0.
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