CN110527450B - Polypropylene film, preparation method thereof, aluminum plastic film and lithium battery - Google Patents
Polypropylene film, preparation method thereof, aluminum plastic film and lithium battery Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/10—Homopolymers or copolymers of propene
- C09J123/14—Copolymers of propene
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/29—Laminated material
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/33—Applications of adhesives in processes or use of adhesives in the form of films or foils for batteries or fuel cells
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2423/00—Presence of polyolefin
- C09J2423/10—Presence of homo or copolymers of propene
- C09J2423/106—Presence of homo or copolymers of propene in the substrate
Abstract
The polypropylene film provided by the invention sequentially comprises a heat sealing layer, a supporting layer and an adhesive layer from the inner side to the outer side; the heat-sealing layer comprises 100 parts by mass of first polypropylene and 5-20 parts by mass of polyolefin elastomer; the support layer comprises 100 parts of a second polypropylene; the adhesive layer comprises 100 parts of third polypropylene and 5-20 parts of maleic anhydride modified polypropylene; at least one of the heat sealing layer, the supporting layer and the bonding layer also comprises 0.01-5 parts of mesoporous material loaded with rare earth salt. The mesoporous material loaded with the rare earth salt can improve the capability of the polypropylene film layer for capturing fluorine ions in hydrofluoric acid so as to prevent the hydrofluoric acid from passing through the polypropylene film layer; meanwhile, the puncture resistance of the polypropylene film can be improved. The preparation method of the polypropylene film provided by the invention is simple, does not need to change the existing preparation equipment, and is easy to popularize; the aluminum-plastic film provided by the invention has higher corrosion resistance and puncture resistance; the lithium battery provided by the invention has higher use safety.
Description
Technical Field
The invention relates to the technical field of preparation of polypropylene films special for aluminum plastic films, in particular to a polypropylene film and a preparation method thereof, an aluminum plastic film containing the polypropylene film and a lithium battery containing the aluminum plastic film.
Background
The aluminum-plastic film structure sequentially comprises a nylon layer, an aluminum foil layer and a polypropylene film layer from the outer side to the inner side, and an adhesive for bonding is arranged between the adjacent layers; the electrolyte of the lithium battery generally consists of an organic solvent and lithium hexafluorophosphate, which is a substance very easy to react with water and generates gaseous hydrofluoric acid with strong corrosiveness; after the hydrofluoric acid penetrates through the polypropylene film layer, the adhesive and the aluminum foil are easy to corrode, so that the aluminum foil and the polypropylene film layer are separated from each other and peeled off, the aluminum foil is perforated, and the like, and the whole lithium battery is scrapped.
The existing thought for improving the corrosion resistance of the aluminum-plastic film is to perform passivation treatment on an aluminum foil, but the method can only improve the corrosion resistance to a certain extent. Hydrofluoric acid generated from the inside of the cell continuously penetrates through the polypropylene film layer to reach the adhesive and the aluminum foil, thereby continuously corroding the aluminum foil. Therefore, preventing hydrofluoric acid from penetrating through the polypropylene film layer is a method for improving the corrosion resistance of the aluminum plastic film. In the process of preparing the aluminum-plastic film, burrs on the aluminum foil easily pierce the inner film to cause liquid leakage and short circuit, so that the battery is scrapped. The existing polypropylene film layer has general puncture resistance and is easy to cause potential safety hazards.
Disclosure of Invention
The invention aims to solve the technical problem of providing a polypropylene film and a preparation method thereof, so as to improve the capturing capability of the polypropylene film on fluorine ions in hydrofluoric acid and the puncture resistance strength of the polypropylene film; in addition, the invention also provides an aluminum plastic film containing the polypropylene film, so as to improve the corrosion resistance of the aluminum plastic film; the invention also provides a lithium battery comprising the aluminum-plastic film, so that the use safety of the lithium battery is improved.
In order to solve the technical problem, the application adopts a technical scheme that: providing a polypropylene film, wherein the polypropylene film sequentially comprises a heat sealing layer, a supporting layer and an adhesive layer from the inner side to the outer side; the heat-sealing layer comprises 100 parts by mass of first polypropylene and 5-20 parts by mass of polyolefin elastomer; the support layer comprises 100 parts of a second polypropylene; the adhesive layer comprises 100 parts of third polypropylene and 5-20 parts of maleic anhydride modified polypropylene; at least one of the heat sealing layer, the supporting layer and the bonding layer further comprises 0.01-5 parts of mesoporous material loaded with rare earth salt.
Preferably, the first polypropylene, the second polypropylene and the third polypropylene are selected from any one or two of binary copolymer polypropylene and ternary copolymer polypropylene.
Preferably, the thickness ratio of the heat sealing layer to the supporting layer to the bonding layer is (1-2) to (4-8): (1-2).
Preferably, the mesoporous material is any one or combination of mesoporous silica and mesoporous alumina; and/or
The particle size range of the mesoporous material is 0.1-5 mu m, the pore size distribution range is 2-50 nm, and the specific surface area range is 150-500 m2(ii)/g; and/or
The rare earth salt is any one or a combination of more of lanthanum chloride, lanthanum nitrate, cerium chloride and cerium nitrate.
Preferably, the mass of the rare earth salt accounts for 0.01-5% of the total mass of the rare earth salt-loaded mesoporous material.
More preferably, the rare earth salt-supported mesoporous material is prepared by the following steps of:
dipping the mesoporous material in 0.05-0.5 mol/L rare earth salt solution, and carrying out ultrasonic treatment for 0.3-1 h;
and after ultrasonic treatment, sequentially vacuumizing, filtering and drying to obtain the mesoporous material loaded with the rare earth salt.
In order to solve the above technical problem, another technical solution adopted by the present application is: the preparation method of the polypropylene film comprises the following steps:
respectively and uniformly mixing the components contained in the heat-sealing layer, the supporting layer and the bonding layer, and then respectively carrying out melting plasticization in three extruders to respectively obtain melts of the heat-sealing layer, the supporting layer and the bonding layer;
carrying out three-layer co-extrusion on the melt of the heat sealing layer, the supporting layer and the bonding layer in a three-layer co-extrusion die head, and then cooling on a cooling roller to form a film;
and annealing the cooled film to obtain the polypropylene film.
Preferably, the step of respectively uniformly mixing the components contained in the heat-sealing layer, the supporting layer and the bonding layer, and then respectively performing melt plasticization in three extruders to respectively obtain melts of the heat-sealing layer, the supporting layer and the bonding layer comprises:
uniformly mixing the components contained in the heat-sealing layer, and then heating the mixture in a first extruder in three stages, wherein the temperature of the first stage is 150-170 ℃, the temperature of the second stage is 170-190 ℃, the temperature of the third stage is 190-220 ℃, and a molten mass of the heat-sealing layer is obtained after the heating in the three stages is finished; and
uniformly mixing the components contained in the supporting layer, and then heating in a second extruder in three stages: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three sections are heated; and
uniformly mixing the components contained in the bonding layer, and then heating in a third extruder in three stages: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated; and/or
The temperature setting range of the cooling roller is 20-35 ℃; and/or
The temperature setting range of the annealing treatment is 40-60 ℃.
In order to solve the above technical problem, another technical solution adopted by the present application is: an aluminum plastic film is provided, and the aluminum plastic film comprises the polypropylene film.
In order to solve the above technical problem, another technical solution adopted by the present application is: a lithium battery is provided, and the lithium battery comprises the aluminum plastic film.
Compared with the prior art, the polypropylene film provided by the invention contains the mesoporous material loaded with the rare earth salt, the mesoporous material loaded with the rare earth salt can improve the capturing capacity of the polypropylene film layer on fluorine ions in hydrofluoric acid so as to prevent the hydrofluoric acid from penetrating through the polypropylene film layer and prevent the hydrofluoric acid from corroding the adhesive and the aluminum foil, and meanwhile, the mesoporous material loaded with the rare earth salt can also improve the mechanical property of the polypropylene film and improve the puncture resistance of the polypropylene film, so that the use safety of the aluminum-plastic film containing the polypropylene film is comprehensively improved; the preparation method of the polypropylene film provided by the invention is simple, the mesoporous material loaded with the rare earth salt is directly mixed with other components in each layer of the polypropylene film, and then the polypropylene film is prepared by using the existing preparation equipment, the existing preparation equipment is not required to be changed, and the preparation method is easy to popularize; the aluminum-plastic film provided by the invention has higher corrosion resistance and puncture resistance; the lithium battery provided by the invention has higher use safety due to the aluminum plastic film.
Drawings
FIG. 1 is a schematic structural diagram of a polypropylene film according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the description of the present disclosure more complete and complete, the following description is given for illustrative purposes with respect to the embodiments and examples of the present invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments are intended to cover the features of the various embodiments as well as the method steps and sequences for constructing and operating the embodiments. However, other embodiments may be utilized to achieve the same or equivalent functions and step sequences.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a polypropylene film according to an embodiment of the present invention. Fig. 1 shows that the polypropylene film sequentially comprises a heat sealing layer 2, a supporting layer 3 and an adhesive layer 4 from bottom to top, the heat sealing layer 2 is arranged close to the electric core side (i.e. close to the inner side of the battery), and the adhesive layer 4 is arranged away from the electric core side and close to the aluminum foil side (i.e. close to the outer side of the battery), i.e. when hydrofluoric acid is generated, the heat sealing layer 2 is firstly contacted, and then the supporting layer 3 and the adhesive layer 4 are sequentially contacted.
According to some embodiments of the present invention, at least one of the heat-sealing layer 2, the supporting layer 3 and the adhesive layer 4 contains a mesoporous material loaded with a rare-earth salt; the rare earth salt contains metal ions capable of forming complexes with fluorine ions, and is loaded on the mesoporous material and then added into at least one layer of the polypropylene film. The porous structure of the mesoporous material can increase the contact area of rare earth salt and hydrofluoric acid so as to enhance the capturing capability of the polypropylene film layer on fluorine ions, thereby preventing the hydrofluoric acid from penetrating through the polypropylene film layer and preventing the hydrofluoric acid from corroding the adhesive and the aluminum foil. Meanwhile, due to the addition of the mesoporous material, the mechanical property of the polypropylene film can be improved, and the puncture resistance of the polypropylene film is improved.
Since the heat-sealing layer 2 is firstly contacted with hydrofluoric acid, in some preferred embodiments of the present invention, only the mesoporous material loaded with rare-earth salt is contained in the heat-sealing layer 2, that is, fluorine ions in the hydrofluoric acid are captured in the heat-sealing layer, so as to achieve the effect of preventing the hydrofluoric acid from passing through the polypropylene film layer; in other preferred embodiments of the present invention, the heat sealing layer 2 and the supporting layer 3 both contain mesoporous materials loaded with rare earth salts to sufficiently capture fluorine ions in hydrofluoric acid, so as to achieve the effect of preventing hydrofluoric acid from passing through the polypropylene film layer.
Specifically, in other embodiments of the present invention, the amount of the mesoporous material loaded with the rare earth salt is 0.01 to 5 parts by mass, and the amount of the mesoporous material is controlled within the range to improve the hydrofluoric acid penetration resistance of the polypropylene film layer and the puncture resistance of the polypropylene film layer. It should be noted that when the addition amount is less than 0.01 part, the prepared polypropylene film has low capturing capability on fluorine ions, and the effect of preventing hydrofluoric acid from passing through the polypropylene film layer is difficult to realize; when the amount is more than 5 parts, mechanical properties of the resulting polypropylene film, such as a decrease in tensile strength, a decrease in elongation at break, and the like, may be affected. More specifically, in some preferred embodiments of the present invention, the amount of the mesoporous material loaded with the rare earth salt is 0.02 to 3 parts by mass, and more preferably 0.02 to 2 parts by mass, and the capability of the polypropylene film layer to prevent hydrofluoric acid from passing through and the puncture resistance of the polypropylene film layer can be improved by controlling the amount of the mesoporous material loaded with the rare earth salt within the above range.
Specifically, in other embodiments of the present invention, the heat-seal layer 2 includes 100 parts by mass of the first polypropylene and 5 to 20 parts by mass of the polyolefin elastomer; support layer 3 comprises 100 parts of a second polypropylene; the bonding layer 4 comprises 100 parts of third polypropylene and 5-20 parts of maleic anhydride modified polypropylene; the polyolefin elastomer contained in the heat-sealing layer 2 can improve the heat-sealing strength of the heat-sealing layer; the maleic anhydride modified polypropylene contained in the adhesive layer 4 can enhance the adhesion of the polypropylene film to the aluminum foil.
More specifically, the first polypropylene, the second polypropylene and the third polypropylene are all selected from any one or two combinations of binary copolymer polypropylene and ternary copolymer polypropylene; the binary copolymer polypropylene has higher mechanical strength, so that the puncture resistance of the polypropylene film is improved, and the ternary copolymer polypropylene is favorable for reducing the heat sealing temperature of the heat sealing layer; thus, in some preferred embodiments, the first polypropylene contained in heat-seal layer 2 is a combination of binary co-polypropylene and ternary co-polypropylene, and the sum of the parts of binary co-polypropylene and ternary co-polypropylene is 100; more preferably, 100 parts of the first polypropylene in the heat-sealing layer 2 comprises 60-90 parts of binary copolymer polypropylene and 10-40 parts of ternary copolymer polypropylene; in some preferred embodiments, the second polypropylene contained in the support layer 3 and the third polypropylene contained in the adhesive layer 4 are both binary copolymer polypropylene to improve the puncture resistance of the polypropylene film.
According to other embodiments of the invention, the heat sealing layer 2 further comprises 0.5-2 parts of slipping agent and 0.5-1.5 parts of anti-blocking agent; the adhesive layer 4 further comprises 0.5-2 parts of slipping agent and 0.5-1.5 parts of anti-blocking agent, and any suitable slipping agent and anti-blocking agent in the field can be used for the slipping agent and the anti-blocking agent, and for the sake of brevity, the details are not repeated herein.
According to some embodiments of the invention, the thickness ratio of the heat sealing layer 2, the supporting layer 3 and the bonding layer 4 is (1-2) to (4-8): (1-2). The thicknesses of the polypropylene films which are commercially available at present are 80 μm and 40 μm, and the polypropylene films provided by the invention can be prepared according to the two thickness specifications; it is understood that the greater the thickness of the polypropylene film, the better its effect of preventing hydrofluoric acid from passing therethrough without affecting the performance of the battery.
Mesoporous materials any suitable mesoporous material known in the art may be used, and according to some embodiments of the present invention, the mesoporous material is selected from either or a combination of mesoporous silica or mesoporous alumina; according to other embodiments of the present invention, the particle size of the mesoporous material is controlled to be 0.1 to 5 μm, preferably 0.1 to 3 μm; if the particle size of the mesoporous material is less than 0.1 μm, the mesoporous material is not beneficial to dispersion in the polypropylene film and is easy to agglomerate, so that the total contact area of the rare earth salt and the hydrofluoric acid is small, the prepared polypropylene film has low capturing capability on fluorine ions, and the effect of preventing the hydrofluoric acid from passing through the polypropylene film layer is difficult to realize; if the particle size of the mesoporous material is larger than 5 μm, the mechanical properties of the obtained polypropylene film, such as a decrease in tensile strength and a decrease in elongation at break, may be affected. According to the bookIn other embodiments of the present invention, it is further required to control the pore size distribution range of the mesoporous material to be 2 to 50nm, and the specific surface area range to be 150 to 500m2(ii)/g; if the pore diameter of the mesoporous material is too large, the corresponding specific surface area of the mesoporous material with the same particle diameter is small, so that the prepared polypropylene film has low capability of capturing fluorine ions, and hydrofluoric acid directly passes through the corresponding added layer due to the large pore diameter, but the hydrofluoric acid is promoted to pass through the polypropylene film layer, so that the opposite effect is achieved.
The rare earth salt can be any suitable rare earth salt in the art, and according to some embodiments of the invention, the rare earth salt is any one or a combination of lanthanum chloride, lanthanum nitrate, cerium chloride and cerium nitrate; lanthanum ions and cerium ions can form complexes with fluorine ions, so that the fluorine ions are captured, and hydrofluoric acid is prevented from penetrating through the polypropylene film layer; according to other embodiments of the invention, the loading amount of the rare earth salt accounts for 0.01-5% of the total mass of the mesoporous material loaded with the rare earth salt, and the capacity of the polypropylene film layer for preventing hydrofluoric acid from passing through is improved by controlling the loading amount within the range, wherein when the loading amount is lower than 0.01%, the prepared polypropylene film has low capability of capturing fluorine ions, and the effect of preventing hydrofluoric acid from passing through the polypropylene film layer is difficult to realize; when the loading is higher than 5%, the raw material cost is higher due to the use of more rare earth salts. Specifically, in some preferred embodiments of the present invention, the loading amount of the rare earth salt accounts for 0.05 to 2% of the total mass of the mesoporous material loaded with the rare earth salt, and the capability of the polypropylene film layer for preventing hydrofluoric acid from passing through can be improved by controlling the loading amount within this range, and the raw material cost is not high.
The rare earth salt can be loaded on the mesoporous material by any suitable means in the art, and in some embodiments of the present invention, the mesoporous material is fully dispersed in the rare earth salt solution by immersing the mesoporous material in 0.05-0.5 mol/L rare earth salt solution and performing ultrasonic treatment for 0.3-1 h, preferably 0.4-0.6 h; after ultrasonic treatment, sequentially vacuumizing (negative pressure adsorption), filtering and drying to obtain the mesoporous material loaded with the rare earth salt, wherein the loading capacity of the rare earth salt can be calculated according to the mass of the mesoporous material before and after impregnation; in other embodiments of the present invention, the mesoporous material loaded with rare earth salt can be obtained by drying and then calcining.
The polypropylene film provided by the invention contains the mesoporous material loaded with the rare earth salt, the mesoporous material loaded with the rare earth salt can improve the capturing capacity of the polypropylene film layer on fluorine ions in hydrofluoric acid so as to prevent the hydrofluoric acid from penetrating through the polypropylene film layer and prevent the hydrofluoric acid from corroding the adhesive and the aluminum foil, and meanwhile, the mesoporous material loaded with the rare earth salt can also improve the mechanical property of the polypropylene film and improve the puncture resistance of the polypropylene film, so that the use safety of the aluminum plastic film containing the polypropylene film is comprehensively improved.
In this regard, the present invention also provides a method of preparing the above-described polypropylene film, which, according to some embodiments of the present invention, comprises the steps of: weighing the components contained in the heat-sealing layer, the supporting layer and the bonding layer in sequence, respectively uniformly mixing, and then respectively carrying out melting plasticization in three extruders to respectively obtain melts of the heat-sealing layer, the supporting layer and the bonding layer; then filtering the melt of the heat sealing layer, the supporting layer and the bonding layer by a filter, performing three-layer co-extrusion in a three-layer co-extrusion die head, and casting the melt onto a cooling roller with a smooth surface to rapidly cool and form a film, wherein the temperature setting range of the cooling roller is 20-35 ℃; and finally, annealing the cooled film to obtain the polypropylene film, wherein the temperature setting range of the annealing treatment is 40-60 ℃. According to further embodiments of the present invention, the method of preparing further comprises: and carrying out corona and edge cutting treatment on the polypropylene film obtained after annealing treatment, and finally rolling.
The heat-sealing layer, the supporting layer and the adhesive layer are melted and plasticized at different temperatures, and in some embodiments of the present invention, the step of preparing the melt of the heat-sealing layer, the supporting layer and the adhesive layer may further include: uniformly mixing the components contained in the heat-sealing layer, and then heating in a first extruder in three stages: the temperature range of the first section is 150-170 ℃, the temperature range of the second section is 170-190 ℃, the temperature range of the third section is 190-220 ℃, and a molten mass of the heat sealing layer is obtained after the three-section heating is finished; uniformly mixing the components contained in the supporting layer, and then heating in a second extruder in three stages: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three-section heating is finished; uniformly mixing the components contained in the bonding layer, and then heating in a third extruder in three stages: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated.
The preparation method of the polypropylene film provided by the invention is simple, the mesoporous material loaded with the rare earth salt is directly mixed with other components in each layer of the polypropylene film, and then the polypropylene film is prepared by using the existing preparation equipment, the existing preparation equipment is not required to be changed, and the preparation method is easy to popularize.
Based on the above, the invention also provides an aluminum plastic film comprising the polypropylene film, and the aluminum plastic film has higher corrosion resistance and puncture resistance.
Based on the above, the invention also provides a lithium battery comprising the aluminum plastic film, and the lithium battery has higher use safety due to the aluminum plastic film.
Example 1
1. Preparing mesoporous silica loaded with 1% of cerium nitrate by mass:
weighing a proper amount of mesoporous silicon oxide product and adding the mesoporous silicon oxide product into a pre-prepared cerium nitrate solution with the concentration of 0.2 mol/L; and (3) carrying out ultrasonic treatment for 30min to fully disperse the mesoporous silicon oxide in the cerium nitrate solution. Vacuumizing the mixed solution, and filtering, drying, roasting and the like to finally obtain the mesoporous silicon oxide loaded with 1% of cerium nitrate by mass; wherein the mesoporous silica has a particle size of 0.1 μm and a specific surface area of 489m2(ii)/g, pore diameter 5 nm; the loading amount of the cerium nitrate is calculated according to the mass of the mesoporous silicon oxide before and after loading.
2. Preparing a special polypropylene film for a lithium battery flexible package aluminum plastic film:
the adhesive layer comprises the following components: 100 parts of binary copolymer polypropylene, 20 parts of maleic anhydride modified polypropylene, 1 part of slipping agent and 0.5 part of anti-blocking agent; the support layer comprises the following components: 100 parts of binary copolymerization polypropylene and 1 part of mesoporous silica loaded with 1% of cerium nitrate by mass percent, prepared in the step 1; the heat-sealing layer comprises the following components: 60 parts of binary copolymer polypropylene, 40 parts of ternary copolymer polypropylene, 5 parts of polyolefin elastomer, 1 part of slipping agent, 0.5 part of anti-blocking agent and 1 part of mesoporous silica loaded with 1% of cerium nitrate by mass percent and prepared in the step 1;
weighing the components in sequence, mixing the components uniformly by using a high-speed mixer respectively, adding the components into three extruders for melting and plasticizing, wherein each component contained in the heat-sealing layer is subjected to three-section heating in the first extruder: the temperature range of the first section is 150-170 ℃, the temperature range of the second section is 170-190 ℃, the temperature range of the third section is 190-220 ℃, and a molten mass of the heat sealing layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the support layer in a second extruder: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the bonding layer in a third extruder: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated;
filtering the obtained melts of the heat sealing layer, the supporting layer and the bonding layer by a filter, feeding the filtered melts into a three-layer co-extrusion die head, and casting the extruded melts onto a cooling roller with a smooth surface to rapidly cool and form a film; wherein, the total thickness of the polypropylene film is set to be 80 μm, and the adhesive layer: a support layer: the thickness ratio of the heat-sealing layer is 1:8:1, and the temperature of the cooling roller is 20 ℃; annealing the cooled film at 60 ℃; then corona treatment and edge cutting treatment are carried out, and finally the polypropylene film A is obtained by rolling.
Example 2
1. Preparing mesoporous alumina loaded with 0.5% of lanthanum nitrate by mass fraction:
weighing a proper amount of mesoporous alumina product and adding the mesoporous alumina product into the product prepared in advanceIn 0.1mol/L lanthanum nitrate solution; ultrasonic treatment is carried out for 30min to fully disperse the mesoporous alumina in the lanthanum nitrate solution. Vacuumizing the mixed solution, and finally obtaining mesoporous alumina loaded with 0.5% of lanthanum nitrate through the working procedures of filtering, drying, roasting and the like; wherein the grain diameter of the mesoporous alumina is 0.5 μm, and the specific surface area is 260m2(ii)/g, pore diameter 19 nm; the loading amount of the lanthanum nitrate is calculated according to the mass difference before and after loading of the mesoporous alumina.
2. Preparing a special polypropylene film for a lithium battery flexible package aluminum plastic film:
the adhesive layer comprises the following components: 100 parts of binary copolymer polypropylene, 5 parts of maleic anhydride modified polypropylene, 2 parts of slipping agent and 0.5 part of anti-blocking agent; the support layer comprises the following components: 100 parts of binary copolymerized polypropylene; the heat-sealing layer comprises the following components: 70 parts of binary copolymer polypropylene, 30 parts of ternary copolymer polypropylene, 10 parts of polyolefin elastomer, 2 parts of slipping agent, 0.5 part of anti-blocking agent and 0.5 part of mesoporous alumina loaded with 0.5% of lanthanum nitrate prepared in the step 1;
weighing the components in sequence, mixing the components uniformly by using a high-speed mixer respectively, adding the components into three extruders for melting and plasticizing, wherein each component contained in the heat-sealing layer is subjected to three-section heating in the first extruder: the temperature range of the first section is 150-170 ℃, the temperature range of the second section is 170-190 ℃, the temperature range of the third section is 190-220 ℃, and a molten mass of the heat sealing layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the support layer in a second extruder: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the bonding layer in a third extruder: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated;
filtering the obtained melts of the heat sealing layer, the supporting layer and the bonding layer by a filter, feeding the filtered melts into a three-layer co-extrusion die head, and casting the extruded melts onto a cooling roller with a smooth surface to rapidly cool and form a film; wherein, the total thickness of the polypropylene film is set to be 80 μm, and the adhesive layer: a support layer: the thickness ratio of the heat-sealing layer is 1:6:1, and the temperature of the cooling roller is 30 ℃; annealing the cooled film, wherein the annealing temperature is 50 ℃; then corona treatment and edge cutting treatment are carried out, and finally the polypropylene film B is obtained by rolling.
Example 3
1. Preparing mesoporous alumina loaded with 2% of cerium nitrate by mass:
weighing a proper amount of mesoporous alumina product and adding the mesoporous alumina product into a pre-prepared cerium nitrate solution with the concentration of 0.4 mol/L; and (3) performing ultrasonic treatment for 30min to fully disperse the mesoporous alumina in the cerium nitrate solution. Vacuumizing the mixed solution, and then filtering, drying, roasting and the like to finally obtain the mesoporous alumina loaded with 2 mass percent of cerium nitrate; wherein the grain diameter of the mesoporous alumina is 5 μm, and the specific surface area is 158m2(ii)/g, pore diameter is 50 nm; the loading amount of the cerium nitrate is calculated according to the mass difference before and after loading of the mesoporous alumina.
2. Preparing a special polypropylene film for a lithium battery flexible package aluminum plastic film:
the adhesive layer comprises the following components: 100 parts of binary copolymer polypropylene, 10 parts of maleic anhydride modified polypropylene, 0.5 part of slipping agent and 1 part of anti-blocking agent; the support layer comprises the following components: 100 parts of binary copolymerization polypropylene and 2 parts of mesoporous alumina loaded with 2% of cerium nitrate by mass percent, prepared in the step 1; the heat-sealing layer comprises the following components: 90 parts of binary copolymer polypropylene, 10 parts of ternary copolymer polypropylene, 20 parts of polyolefin elastomer, 0.5 part of slipping agent, 1 part of anti-blocking agent and 2 parts of mesoporous alumina loaded with 2% of cerium nitrate in mass percentage prepared in the step 1;
weighing the components in sequence, mixing the components uniformly by using a high-speed mixer respectively, adding the components into three extruders for melting and plasticizing, wherein each component contained in the heat-sealing layer is subjected to three-section heating in the first extruder: the temperature range of the first section is 150-170 ℃, the temperature range of the second section is 170-190 ℃, the temperature range of the third section is 190-220 ℃, and a molten mass of the heat sealing layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the support layer in a second extruder: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the bonding layer in a third extruder: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated;
filtering the obtained melts of the heat sealing layer, the supporting layer and the bonding layer by a filter, feeding the filtered melts into a three-layer co-extrusion die head, and casting the extruded melts onto a cooling roller with a smooth surface to rapidly cool and form a film; wherein, the total thickness of the polypropylene film is set to be 40 μm, and the adhesive layer: a support layer: the thickness ratio of the heat-sealing layer is 2:6:2, and the temperature of the cooling roller is 25 ℃; annealing the cooled film, wherein the annealing temperature is 40 ℃; then corona treatment and edge cutting treatment are carried out, and finally the polypropylene film C is obtained by rolling.
Example 4
1. Preparing mesoporous silica loaded with cerium chloride with the mass fraction of 0.05%:
weighing a proper amount of mesoporous silicon oxide product and adding the mesoporous silicon oxide product into a pre-prepared cerium chloride solution with the concentration of 0.05 mol/L; and (3) performing ultrasonic treatment for 30min to fully disperse the mesoporous silicon oxide in the cerium chloride solution. Vacuumizing the mixed solution, and finally obtaining the cerium chloride mesoporous silica with the load mass fraction of 0.05 percent through the working procedures of filtering, drying, roasting and the like; wherein the mesoporous silica has a particle size of 1 μm and a specific surface area of 237m2(ii)/g, pore size 14 nm; the loading amount of the cerium chloride is calculated according to the mass difference before and after loading of the mesoporous silica.
2. Preparing a special polypropylene film for a lithium battery flexible package aluminum plastic film:
the adhesive layer comprises the following components: 100 parts of binary copolymer polypropylene, 15 parts of maleic anhydride modified polypropylene, 1 part of slipping agent and 1 part of anti-blocking agent; the support layer comprises the following components: 100 parts of binary copolymerized polypropylene; the heat-sealing layer comprises the following components: 80 parts of binary copolymer polypropylene, 20 parts of ternary copolymer polypropylene, 15 parts of polyolefin elastomer, 1.5 parts of slipping agent, 1.5 parts of anti-blocking agent and 0.05 part of mesoporous silica loaded with 0.05% of cerium chloride in mass percentage prepared in the step 1;
weighing the components in sequence, mixing the components uniformly by using a high-speed mixer respectively, adding the components into three extruders for melting and plasticizing, wherein each component contained in the heat-sealing layer is subjected to three-section heating in the first extruder: the temperature range of the first section is 150-170 ℃, the temperature range of the second section is 170-190 ℃, the temperature range of the third section is 190-220 ℃, and a molten mass of the heat sealing layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the support layer in a second extruder: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three-section heating is finished; and (3) carrying out three-stage heating on the components contained in the bonding layer in a third extruder: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated;
filtering the obtained melts of the heat sealing layer, the supporting layer and the bonding layer by a filter, feeding the filtered melts into a three-layer co-extrusion die head, and casting the extruded melts onto a cooling roller with a smooth surface to rapidly cool and form a film; wherein, the total thickness of the polypropylene film is set to be 40 μm, and the adhesive layer: a support layer: the thickness ratio of the heat-sealing layer is 1:7:2, and the temperature of the cooling roller is 25 ℃; annealing the cooled film, wherein the annealing temperature is 45 ℃; then corona treatment and edge cutting treatment are carried out, and finally the polypropylene film D is obtained by rolling.
Blank control example 1
Blank comparative example 1 differs from example 1 in that: the support layer and the heat seal layer do not contain mesoporous silicon oxide loaded with 1% of cerium nitrate by mass, and the rest of the formula and the preparation process are the same, so that the polypropylene film E is finally prepared.
Blank control example 2
Blank control example 2 differs from example 1 in that: the support layer and the heat seal layer contain 0.01 part of cerium nitrate, the cerium nitrate is directly added into the formula components without mesoporous silica loading, and the rest of the formula and the preparation process are the same, so that the polypropylene film F is finally prepared.
Blank control example 3
Blank control example 4
Blank control example 4 differs from example 3 in that: the support layer and the heat seal layer contain 0.04 parts of cerium nitrate, the cerium nitrate is directly added into the components of the formula without mesoporous alumina load, and the rest of the formula and the preparation process are the same, so that the polypropylene film H is finally prepared.
The prepared polypropylene films A-H are prepared into aluminum plastic films A-H by adopting a dry forming process, the structure is nylon/adhesive/aluminum foil/adhesive/polypropylene film, and then the performance of the aluminum plastic films is tested, and the test results are shown in the following table 1. When the thickness of the polypropylene film is 80 μm, the total thickness of the aluminum plastic film is 152 μm, and when the thickness of the polypropylene film is 40 μm, the total thickness of the aluminum plastic film is 113 μm. Comparative examples 1 and 2 are commercially available aluminum plastic films of the same type, with the thicknesses of 152 μm and 113 μm respectively, and are marked as aluminum plastic film I and aluminum plastic film J respectively.
And (3) testing puncture strength: the puncture strength was determined according to the specification "6.6.13 puncture strength" in GB/T10004-2008. The puncture needle head starts to puncture from one side of the heat sealing layer.
Electrolyte resistance performance test: cutting the aluminum-plastic film into samples with the diameter of 15mm multiplied by 100mm, soaking the samples in electrolyte with the temperature of 85 ℃ for 7 days, wherein the electrolyte comprises EC/DEC/DMC (1: 1:1+1 mol/L) LiFeF6+1000ppm H2And O, taking out the sample, washing the residual electrolyte, and testing the peel strength between the polypropylene film and the aluminum foil of the sample at the testing speed of 100 mm/min.
TABLE 1 electrolyte resistance test and puncture strength test results for each aluminum-plastic film
As can be seen from table 1 above:
(1) the aluminum-plastic film E prepared from the polypropylene film E prepared in the blank comparative example 1 has little difference in electrolyte resistance and puncture strength from the aluminum-plastic film I in the comparative example 1, and the aluminum-plastic film G prepared from the polypropylene film G prepared in the blank comparative example 3 has little difference in electrolyte resistance and puncture strength from the aluminum-plastic film J in the comparative example 2;
(2) compared with the aluminum plastic films E and J, the aluminum plastic films A to D prepared from the polypropylene films A to D prepared in the embodiments 1 to 4 have better electrolyte resistance and puncture strength;
the mesoporous material loaded with the rare earth salt is added into at least one of the heat sealing layer, the supporting layer and the bonding layer of the polypropylene film by 0.05-2 parts, so that the capturing capability of the polypropylene film layer on fluorine ions can be obviously improved, hydrofluoric acid is prevented from penetrating through the polypropylene film layer, the adhesive and the aluminum foil are prevented from being corroded by the hydrofluoric acid, and the puncture resistance of the polypropylene film is improved.
(3) The aluminum-plastic film F prepared from the polypropylene film F prepared in the blank comparative example 2 is superior to the aluminum-plastic film E in electrolyte resistance but lower than the aluminum-plastic film a. The rare earth salt is loaded on the mesoporous silica, and the mesoporous silica can increase the contact area of the rare earth salt and hydrofluoric acid, so that the capability of the polypropylene film layer for capturing fluorine ions is improved. The aluminum-plastic film H prepared from the polypropylene film H prepared in the blank comparative example 4 is superior to the aluminum-plastic film G in electrolyte resistance, but lower than the aluminum-plastic film C, and the results show the same rule.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The polypropylene film is characterized by comprising a heat sealing layer, a supporting layer and an adhesive layer from the inner side to the outer side in sequence; the heat-sealing layer comprises 100 parts by mass of first polypropylene and 5-20 parts by mass of polyolefin elastomer; the support layer comprises 100 parts of a second polypropylene; the adhesive layer comprises 100 parts of third polypropylene and 5-20 parts of maleic anhydride modified polypropylene; wherein the heat sealing layer further comprises 0.01-5 parts of mesoporous material loaded with rare earth salt;
the particle size range of the mesoporous material is 0.1-5 mu m, the pore size distribution range is 2-50 nm, and the specific surface area range is 150-500 m2/g。
2. The polypropylene film of claim 1, wherein the first polypropylene, the second polypropylene and the third polypropylene are each selected from the group consisting of any one or a combination of two of a binary copolymer polypropylene and a ternary copolymer polypropylene.
3. The polypropylene film according to claim 1, wherein the thickness ratio of the heat-sealing layer, the supporting layer and the bonding layer is (1-2) to (4-8): (1-2).
4. The polypropylene film according to claim 1, wherein the mesoporous material is one or a combination of mesoporous silica and mesoporous alumina; and/or
The rare earth salt is any one or a combination of more of lanthanum chloride, lanthanum nitrate, cerium chloride and cerium nitrate.
5. The polypropylene film according to claim 4, wherein the rare earth salt is present in an amount of 0.01 to 5% by mass based on the total mass of the rare earth salt-supporting mesoporous material.
6. The polypropylene film according to any one of claims 1 to 5, wherein the rare earth salt-loaded mesoporous material is prepared by a process comprising:
dipping the mesoporous material in 0.05-0.5 mol/L rare earth salt solution, and carrying out ultrasonic treatment for 0.3-1 h;
and after ultrasonic treatment, sequentially vacuumizing, filtering and drying to obtain the mesoporous material loaded with the rare earth salt.
7. A method for preparing a polypropylene film according to any one of claims 1 to 6, comprising:
respectively and uniformly mixing the components contained in the heat-sealing layer, the supporting layer and the bonding layer, and then respectively carrying out melting plasticization in three extruders to respectively obtain melts of the heat-sealing layer, the supporting layer and the bonding layer;
carrying out three-layer co-extrusion on the melt of the heat sealing layer, the supporting layer and the bonding layer in a three-layer co-extrusion die head, and then cooling on a cooling roller to form a film;
and annealing the cooled film to obtain the polypropylene film.
8. The method according to claim 7,
the step of respectively uniformly mixing the components contained in the heat-sealing layer, the supporting layer and the bonding layer and then respectively carrying out melting plasticization in three extruders to respectively obtain melts of the heat-sealing layer, the supporting layer and the bonding layer comprises the following steps of:
uniformly mixing the components contained in the heat-sealing layer, and then heating the mixture in a first extruder in three stages, wherein the temperature of the first stage is 150-170 ℃, the temperature of the second stage is 170-190 ℃, the temperature of the third stage is 190-220 ℃, and a molten mass of the heat-sealing layer is obtained after the heating in the three stages is finished; and
uniformly mixing the components contained in the supporting layer, and then heating in a second extruder in three stages: the temperature range of the first section is 180-210 ℃, the temperature range of the second section is 210-230 ℃, the temperature range of the third section is 230-250 ℃, and a molten mass of the supporting layer is obtained after the three sections are heated; and
uniformly mixing the components contained in the bonding layer, and then heating in a third extruder in three stages: the temperature range of the first section is 170-190 ℃, the temperature range of the second section is 190-220 ℃, the temperature range of the third section is 220-240 ℃, and a molten mass of the bonding layer is obtained after the three sections are heated; and/or
The temperature setting range of the cooling roller is 20-35 ℃; and/or
The temperature setting range of the annealing treatment is 40-60 ℃.
9. An aluminum-plastic film comprising the polypropylene film according to any one of claims 1 to 6.
10. A lithium battery comprising the aluminum plastic film as recited in claim 9.
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