CN117445511A - 一种铝塑复合膜及其制备方法 - Google Patents
一种铝塑复合膜及其制备方法 Download PDFInfo
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- CN117445511A CN117445511A CN202311378657.7A CN202311378657A CN117445511A CN 117445511 A CN117445511 A CN 117445511A CN 202311378657 A CN202311378657 A CN 202311378657A CN 117445511 A CN117445511 A CN 117445511A
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- layer
- aluminum
- coupling agent
- plastic composite
- composite film
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- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 239000004033 plastic Substances 0.000 title claims abstract description 76
- 229920003023 plastic Polymers 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 239000011241 protective layer Substances 0.000 claims abstract description 87
- 239000010410 layer Substances 0.000 claims abstract description 77
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 72
- 239000000843 powder Substances 0.000 claims abstract description 62
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 60
- 239000011737 fluorine Substances 0.000 claims abstract description 60
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 55
- 239000000945 filler Substances 0.000 claims abstract description 49
- 230000004888 barrier function Effects 0.000 claims abstract description 44
- 239000012790 adhesive layer Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000012793 heat-sealing layer Substances 0.000 claims abstract description 27
- -1 polypropylene Polymers 0.000 claims abstract description 24
- 239000004743 Polypropylene Substances 0.000 claims abstract description 16
- 229920001155 polypropylene Polymers 0.000 claims abstract description 16
- 229920005604 random copolymer Polymers 0.000 claims abstract description 14
- 239000002667 nucleating agent Substances 0.000 claims abstract description 8
- 125000001153 fluoro group Chemical group F* 0.000 claims abstract description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 55
- 239000007822 coupling agent Substances 0.000 claims description 35
- 239000004593 Epoxy Substances 0.000 claims description 24
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 15
- 229920001911 maleic anhydride grafted polypropylene Polymers 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 abstract description 40
- 238000005260 corrosion Methods 0.000 abstract description 23
- 230000007797 corrosion Effects 0.000 abstract description 23
- 238000013329 compounding Methods 0.000 abstract description 4
- 230000000149 penetrating effect Effects 0.000 abstract 2
- 229910052782 aluminium Inorganic materials 0.000 description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 7
- 239000002985 plastic film Substances 0.000 description 7
- 229920006255 plastic film Polymers 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000007405 data analysis Methods 0.000 description 4
- NLSFWPFWEPGCJJ-UHFFFAOYSA-N 2-methylprop-2-enoyloxysilicon Chemical compound CC(=C)C(=O)O[Si] NLSFWPFWEPGCJJ-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical group CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical group CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- FWLUTJHBRZTAMP-UHFFFAOYSA-N B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+] Chemical compound B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+].[Li+] FWLUTJHBRZTAMP-UHFFFAOYSA-N 0.000 description 1
- 229920003313 Bynel® Polymers 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical group C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001500 lithium hexafluoroborate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- AYOOGWWGECJQPI-NSHDSACASA-N n-[(1s)-1-(5-fluoropyrimidin-2-yl)ethyl]-3-(3-propan-2-yloxy-1h-pyrazol-5-yl)imidazo[4,5-b]pyridin-5-amine Chemical compound N1C(OC(C)C)=CC(N2C3=NC(N[C@@H](C)C=4N=CC(F)=CN=4)=CC=C3N=C2)=N1 AYOOGWWGECJQPI-NSHDSACASA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
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- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
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- 238000002161 passivation Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
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- 238000002444 silanisation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/10—Primary casings; Jackets or wrappings
- H01M50/116—Primary casings; Jackets or wrappings characterised by the material
- H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
- H01M50/126—Primary casings; Jackets or wrappings characterised by the material having a layered structure comprising three or more layers
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- Mechanical Engineering (AREA)
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
本申请涉及复合膜技术领域,具体公开了一种铝塑复合膜及其制备方法。一种铝塑复合膜,由外到内,包括外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层;保护层,包括三元无规共聚聚丙烯100份、相容剂5‑8份、改性填料10‑25份、成核剂1‑5份;改性填料为经过硅烷偶联剂处理的含氟微粉和硅粉;其制备方法为:将三元无规共聚聚丙烯、相容剂、改性填料、成核剂混合后,熔融共挤出,得到保护层;由外到内,将外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层复合后,得到铝塑复合膜。本申请的保护层具有良好的耐腐蚀性,阻隔热封层渗透的电解液继续渗透入第二胶黏剂层中,有利于提高铝塑复合膜的耐电解液性能。
Description
技术领域
本申请涉及复合膜技术领域,更具体地说,它涉及一种铝塑复合膜及其制备方法。
背景技术
铝塑复合膜,简称铝塑膜,是一种用于封装锂离子电池的复合软包装外壳材料,常用于软包电池中。通过铝塑膜对组装后的单片电芯进行密封,能够起到保护内部电极、隔绝外界环境的重要作用。
目前,铝塑膜由外到内依次由外阻层(尼龙)、阻透层(铝材)以及热封层(聚丙烯)通过胶黏剂复合而成,具有良好的耐穿刺性能、高阻隔性能、耐电解液性能、耐高温绝缘性能以及高冷冲压成型性能。
然而,由于锂离子电池的电解液是由渗透性极强的有机溶剂,以及极易水解的六氟磷酸锂、六氟硼酸锂等组成。因此,虽然热封层具有良好的耐电解液腐蚀性,但是长期与电解液接触后,还是容易被电解液溶胀、腐蚀。所以依然存在部分电解液渗透入胶黏剂中并腐蚀胶黏剂,使得热封层和阻透层分层,从而破坏了铝塑膜结构,降低了铝塑复合膜的耐电解液性能。
发明内容
为了提高铝塑膜的耐电解液性能,本申请提供一种铝塑复合膜及其制备方法。
第一方面,本申请提供一种铝塑复合膜,采用如下的技术方案:
一种铝塑复合膜,由外到内,包括外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层;
所述保护层,包括如下重量份数的组分:
三元无规共聚聚丙烯100份;
相容剂5-8份;
改性填料10-25份;
成核剂1-5份;
所述改性填料为经过硅烷偶联剂处理的含氟微粉和硅粉。
通过采用上述技术方案,含氟微粉和硅粉具有良好的耐腐蚀性。将含氟微粉和硅粉混合后,由于硅粉具有良好的吸附性,可吸附部分表面光滑的含氟微粉。一方面,含氟微粉的表面能较低,部分吸附在硅粉表面的含氟微粉降低了硅粉的表面能,促进了硅粉在三元无规共聚聚丙烯等组分中的分散,有利于提高所得保护层的耐腐蚀性能。另一方面,硅粉作为载体吸附部分含氟微粉,增加了含氟微粉在三元无规共聚聚丙烯中的粘结强度,有利于含氟微粉在保护层中发挥出良好的耐腐蚀性能。
同时,通过采用硅烷偶联剂对含氟微粉和硅粉进行表面处理,进一步促进了含氟微粉和硅粉在三元无规共聚聚丙烯等组分中分散和附着,有利于提高所得保护层的耐腐蚀性能。而且含氟微粉和硅粉表面包覆有一层硅烷偶联剂还增加了保护层和第二胶黏剂层的相容性,有利于提高保护层和第二胶黏剂层的粘结强度。
因此,将保护层设置在第二胶黏剂层和热封层之间,由于保护层具有良好的耐腐蚀性能,有效减少渗透的电解液腐蚀第二胶黏剂层、阻透层第一胶黏剂层、外阻层,有利于提高铝塑膜的耐电解液性能。
优选的,所述改性填料的制备方法为:将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4-5,然后加入预先混合的含氟微粉和硅粉,搅拌混合,过滤,干燥,得到改性填料。
通过采用上述技术方案,先将含氟微粉和硅粉混合,使得硅粉表面先吸附部分含氟微粉,有利于提高硅粉在混合液中的分散性。然后,将硅烷偶联剂溶于水和有机溶剂中,在pH值为4-5的环境下可水解出硅醇,硅醇可与硅粉、先吸附部分含氟微粉的硅粉表面键合,并在含氟微粉和硅粉表面形成一层硅烷偶联剂包覆层,有利于提高含氟微粉和硅粉在三元无规共聚聚丙烯等组分中的分散性和相容性,提高保护层的耐腐蚀性能,从而提高最终所得铝塑膜的耐电解液性能。
优选的,所述硅烷偶联剂为苯基硅烷偶联剂和环氧基偶联剂中的一种或两种。
通过采用上述技术方案,苯基硅烷偶联剂和环氧基偶联剂的化学结构中含有苯基和环氧基,使得苯基硅烷偶联剂和环氧基偶联剂具有良好的抗化学腐蚀能力。因此,采用苯基硅烷偶联剂和环氧基偶联剂对含氟微粉和硅粉进行改性,有利于提高保护层的耐腐蚀性能,提高最终所得铝塑复合膜的耐电解液性能。
优选的,所述硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂混合组成,硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂的重量比为1:(0.8-1.2)。
通过采用上述技术方案,将苯基硅烷偶联剂和环氧基偶联剂混合复配对含氟微粉和硅粉进行硅烷化处理,在含氟微粉和硅粉表面包覆一层含有苯基和环氧基的有机硅层后添加至保护层中,有利于提高保护层的耐腐蚀性能。
优选的,所述含氟微粉为聚四氟乙烯微粉、聚偏氟乙烯微粉和聚全氟乙丙烯微粉中的一种或多种。
通过采用上述技术方案,聚四氟乙烯微粉、聚偏氟乙烯微粉和聚全氟乙丙烯微粉具有良好的耐腐蚀性能,将上述含氟微粉添加在保护层中,有利于提高最终所得铝塑复合膜的耐电解液性能。
优选的,所述改性填料中,硅烷偶联剂、含氟微粉和硅粉的重量比为1:(0.2-0.4):(0.4-0.7)。
通过采用上述技术方案,优化硅烷偶联剂、含氟微粉和硅粉的重量,有利于在硅粉表面吸附含氟微粉,以及硅烷偶联剂在含氟微粉和硅粉表面形成有机膜层,提高含氟微粉和硅粉在保护层中的分散性、相容性和粘结强度,从而提高最终所得铝塑复合膜持久的耐电解液性能。
优选的,所述硅粉还经过预处理,预处理步骤为:将硅粉加入pH值为9-11的碱性水溶液中,搅拌混合后,过滤,水洗,干燥,得到预处理的硅粉。
通过采用上述技术方案,在强碱性环境下,硅粉表面形成微刻蚀,使得硅粉表面粗化,增大了硅粉的表面积,有利于提高硅粉吸附含氟微粉的含量,增加了含氟微粉在三元无规共聚聚丙烯中的粘结强度,有利于含氟微粉在保护层中发挥出良好的耐腐蚀性能,提高铝塑复合膜的耐电解液性能。
优选的,所述相容剂为马兰酸酐接枝聚丙烯,所述马兰酸酐接枝聚丙烯的密度为0.92g/cm3,190℃,2.16Kg条件下的熔融指数为60-80g/10min。
通过采用上述技术方案,马兰酸酐接枝聚丙烯具有较高的反应活性,与含氟微粉、硅粉表米包覆的硅烷偶联剂的相容性较好,有利于提高含氟微粉、硅粉在三元无规共聚聚丙烯中的相容性和粘结强度,提高保护层的耐电解液性能。同时,马兰酸酐接枝聚和丙烯热封层、第二胶黏剂层具有良好的相容性,使得保护层和阻透层、热封层中相容界面的分子链相互缠绕结合,提高保护层和阻透层、热封层的粘结强度。
第二方面,本申请提供一种铝塑复合膜的制备方法,采用如下的技术方案:
一种铝塑复合膜的制备方法,包括以下步骤:
S1:将三元无规共聚聚丙烯、相容剂、改性填料、成核剂混合后,熔融共挤出,得到保护层;
S2:由外到内,将外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、S1所得保护层和热封层复合后,得到铝塑复合膜。
通过采用上述技术方案,将阻透层通过胶黏剂直接和外阻层、保护层、热封层进行复合,减少了对热封层进行第二次高温加热,使得所得铝塑复合膜具有良好的冲深成型性能。同时,本申请保护层和铝塑复合膜的制备方法简单,适合大规模生产。
综上所述,本申请具有以下有益效果:
1、由于本申请采用经过硅烷偶联剂处理的含氟微粉和硅粉制备所得的保护层,具有良好的耐腐蚀性能,可阻挡渗透的电解液继续渗入第二胶黏剂层中,有利于提高铝塑复合膜的耐电解液性能;
2、本申请在改性填料的制备方法中,通过预先将含氟微粉和硅粉共混,再进行硅烷偶联剂改性,有利于硅烷偶联剂均匀的对硅粉进行包覆,有利于提高改性填料在保护层中的分散性、相容性和粘结强度,从而使得保护层具有长久的耐电解液性能;
3、本申请铝塑复合膜的制备方法,通过采用简单的干法工艺将外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、S1所得保护层和热封层复合,所得的铝塑复合膜具有良好的冲深成型性能和耐电解液性能。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
制备例
制备例1
一种改性填料,各组分及其重量(kg)如下表所示。
上述改性填料,包括以下制备步骤:
A1:将含氟微粉加入硅粉中,在40kHz条件下超声搅拌2h后,得到预先混合的含氟微粉和硅粉;
本申请制备例中,含氟微粉为聚全氟乙丙烯微粉,白度为98%,平均粒径为4.2μm,150℃,2h条件下的热失重为0.05%,熔点为264℃;
硅粉,分子式为Ca3(Si3O9),粒度为325目,硅含量>92%,牌号SF85,含水率1.2,活性指数109。
A2:将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4,搅拌混合3h后,加入预先混合的含氟微粉和硅粉,在30kHz条件下超声搅拌混合2h,过滤,干燥,得到改性填料;
本申请制备例中,硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂混合组成,苯基硅烷偶联剂和环氧基偶联剂的重量比为1:1,其中,苯基硅烷偶联剂为苯基三乙氧基硅烷,环氧基偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷。
有机溶剂为乙醇。
制备例2-5
一种改性填料,与制备例1的不同之处在于,各组分及其重量(kg)如下表所示。
制备例6
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂混合组成,苯基硅烷偶联剂和环氧基偶联剂的重量比为1:0.8。
制备例7
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂混合组成,苯基硅烷偶联剂和环氧基偶联剂的重量比为1:1.2。
制备例8
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂由甲基丙烯酰氧基硅烷偶联剂和环氧基偶联剂混合组成,甲基丙烯酰氧基硅烷偶联剂和环氧基偶联剂的重量比为1:1,其中,甲基丙烯酰氧基硅烷偶联剂为γ-甲基丙烯酰氧基丙基三甲氧基硅烷。
制备例9
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂为环氧基偶联剂,其中,环氧基偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷。
制备例10
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂为苯基硅烷偶联剂,其中,苯基硅烷偶联剂为苯基三乙氧基硅烷。
制备例11
一种改性填料,与制备例1的不同之处在于,硅烷偶联剂为苯基硅烷偶联剂,其中,苯基硅烷偶联剂为二乙氧基二苯基硅烷。
制备例12
一种改性填料,与制备例1的不同之处在于,硅粉还经过预处理,预处理步骤为:将硅粉加入pH值为9的碱性水溶液中,在40kHz条件下超声搅拌1.5h后,过滤,水洗至pH值为7后,干燥,得到预处理的硅粉。
制备例13
一种改性填料,与制备例1的不同之处在于,包括以下制备步骤:
将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4,搅拌混合3h后,加入含氟微粉和硅粉,在30kHz条件下超声搅拌混合2h,过滤,干燥,得到改性填料。
性能检测
对本申请实施例和对比例所得的铝塑复合膜进行剥离力检测,检测方法如下:
将铝塑复合膜裁切为15mm宽,150mm长,先检测阻透层和保护层的初始剥离力;再将裁切的铝塑复合膜浸泡在1mol/L六氟磷酸锂电解液中,并加入1%水,然后放在85℃烘箱烘烤24h,检测阻透层和保护层的末期剥离力,其中,检测时的剥离速度为50mm/min。
实施例
实施例1
一种铝塑复合膜,由外到内,由外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层组成。
本申请实施例中,外阻层的材料为市售的尼龙膜,由苏州恒拓包装材料有限公司定制,厚度为20μm;
阻透层为市售经过钝化处理的铝箔,型号为3004,厚度为30μm;
热封层,为市售的聚丙烯绝缘薄膜,由温州鑫泰新材料股份有限公司定制,热封层的厚度为20μm;
第一胶黏剂层和第二胶黏剂层为聚氨酯热熔胶,型号为pur4663,厚度为2μm。
保护层,各组分及其重量(kg)如下表所示。
上述铝塑复合膜的制备方法,包括以下步骤:
S1:将三元无规共聚聚丙烯、相容剂、改性填料、成核剂混合后,熔融共挤出,得到保护层;本申请实施例中,三元无规共聚聚丙烯的牌号为800EPS;相容剂为马兰酸酐接枝聚丙烯,型号为B1,马兰酸酐接枝聚丙烯的密度为0.92g/cm3,190℃,2.16Kg条件下的熔融指数为60-80g/10min;改性填料为制备例1制备的改性填料;成核剂型号为ATL-5803。
S2:由外到内,将外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、S1所得保护层和热封层通过干法工艺复合后,得到铝塑复合膜。
实施例2-3
一种铝塑复合膜,与实施例1的不同之处在于,保护层中,各组分及其重量(kg)如下表所示。
对本申请实施例2-3所得的铝塑复合膜,进行剥离力检测,检测结果如下表所示。
通过对上表进行数据分析可知,本申请实施例1-3所得的铝塑复合膜中,阻透层和保护层的初始剥离力高达13.0-15.8N/15mm,在电解液中浸渍24h后,阻透层和保护层的末期剥离力高达11.8-15.0N/15mm。由此表明,本申请实施例1-3所得的铝塑复合膜,在电解液中浸渍24h后,阻透层和保护层依然具有较高的剥离力,因此铝塑复合膜具有良好的耐电解液性。
实施例4-15
一种铝塑复合膜,与实施例1的不同之处在于,保护层中的改性填料为下表制备例制备而成。
实施例 | 制备例 |
实施例4 | 制备例2 |
实施例5 | 制备例3 |
实施例6 | 制备例4 |
实施例7 | 制备例5 |
实施例8 | 制备例6 |
实施例9 | 制备例7 |
实施例10 | 制备例8 |
实施例11 | 制备例9 |
实施例12 | 制备例10 |
实施例13 | 制备例11 |
实施例14 | 制备例12 |
实施例15 | 制备例13 |
对本申请实施例4-15所得的铝塑复合膜,进行剥离力检测,并计算剥离力相对降低变化量,计算公式为:剥离力相对降低变化量=(初始剥离-末期剥离力)/初始剥离*100%,检测结果如下表所示。
通过对上表进行数据分析可知,相较于实施例1、4、5中阻透层和保护层的剥离力相对降低变化量,实施例6、7中阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,在本申请铝塑复合膜的制备总原料中,在制备保护层中的改性填料时,当硅烷偶联剂、含氟微粉和硅粉的重量比为1:(0.2-0.4):(0.4-0.7),可提高铝塑复合膜的耐电解液性,提高阻透层和保护层的结构强度。
相较于实施例1、8、9中阻透层和保护层的剥离力相对降低变化量,实施例10、11、12、13中阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,在本申请铝塑复合膜的制备总原料中,在制备保护层中的改性填料时,当硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂按重量比1:(0.8-1.2)混合组成,可提高铝塑复合膜的耐电解液性能。分析其原因可能是,苯基硅烷偶联剂和环氧基偶联剂中含有的苯基和环氧基具有良好的耐腐蚀性能,因此将苯基硅烷偶联剂和环氧基偶联剂复配使用,提高了保护层的耐腐蚀性能,从而提高了铝塑复合膜的耐电解液性能。
相较于实施例1中阻透层和保护层的剥离力相对降低变化量,实施例14中阻透层和保护层的剥离力相对降低变化量明显降低。由此表明,在本申请铝塑复合膜的制备总原料中,在制备保护层中的改性填料时,硅粉还经过碱性水溶液进行预处理,可提高铝塑复合膜的耐电解液性能。分析其原因可能是,碱性水溶液可以腐蚀硅粉,增加硅粉的表面积,有利于增加硅粉表面吸附含氟微粉的含量,提高硅粉在保护层组分中的分散性、相容性以及含氟微粉在保护层组分中的粘结强度,从而提高了保护层的耐腐蚀性能,使得铝塑复合膜在电解液中浸泡24h后,阻透层和保护层依然具有较高的剥离力。
相较于实施例1中阻透层和保护层的剥离力相对降低变化量,实施例15中阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,在本申请铝塑复合膜的制备总原料中,在制备保护层中的改性填料时,先将含氟微粉和硅粉进行预先混合,可提高铝塑复合膜的耐电解液性能。分析其原因可能是,预先将含氟微粉和硅粉进行混合,促使硅粉吸附含氟微粉,可降低硅粉的表面能,促使硅粉在保护层组分中充分分散、相容,并且有利于含氟微粉在保护层组分中的附着,从而提高了保护层的耐腐蚀性能,使得铝塑复合膜在电解液中浸泡24h后,阻透层和保护层依然具有较高的剥离力。
实施例16
一种铝塑复合膜,与实施例1的不同之处在于,相容剂为马兰酸酐接枝聚丙烯,牌号为Bynel 50E739,马兰酸酐接枝聚丙烯的密度为0.890g/cm3,190℃,2.16Kg条件下的熔融指数为6g/10min。
实施例17
一种铝塑复合膜,与实施例1的不同之处在于,相容剂为马兰酸酐接枝聚丙烯,型号为B1A,马兰酸酐接枝聚丙烯的密度为0.92g/cm3,190℃,2.16Kg条件下的熔融指数为80-110g/10min。
对本申请实施例16-17所得的铝塑复合膜,进行剥离力检测,并计算剥离力相对降低变化量,计算公式为:剥离力相对降低变化量=(初始剥离-末期剥离力)/初始剥离*100%,检测结果如下表所示。
通过对上表进行数据分析可知,相较于实施例1中阻透层和保护层的剥离力相对降低变化量,实施例16、17中阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,在本申请铝塑复合膜的制备总原料中,马兰酸酐接枝聚丙烯的密度为0.92g/cm3,190℃,2.16Kg条件下的熔融指数为60-80g/10min,可提高铝塑复合膜的耐腐蚀性能。分析其原因可能是,具有上述物理性能的马兰酸酐接枝聚丙烯与改性填料具有良好的相容性,使得改性填料可充分分散在保护层中,并具有良好的粘结强度,从而提高了保护层的耐腐蚀性能,使得铝塑复合膜在电解液中浸泡24h后,阻透层和保护层依然具有较高的剥离力。
同时,相较于实施例16、17,实施例1中阻透层和保护层的初始剥离力更高,分析其原因可能是上述物理性能的马兰酸酐接枝聚丙烯不仅具有良好的加工性能,也具有良好的强度,使得保护层和第二胶黏剂层、热封层在复合时,使得保护层和第二胶黏剂层、保护层和热封层中相容界面的分子链相互缠绕结合,从而提高了阻透层和保护层、保护层和热封层的粘结强度
对比例
对比例1
一种铝塑复合膜,与实施例1的不同之处在于,由外到内,由外阻层、第一胶黏剂层、阻透层、第二胶黏剂层和热封层组成。
对比例2
一种铝塑复合膜,与实施例1的不同之处在于,保护层中,改性填料为含氟微粉和硅粉的混合物。
上述改性填料,包括以下制备步骤:
将含氟微粉加入硅粉中,在40kHz条件下超声搅拌2h后,得到预先混合的含氟微粉和硅粉。
对比例3
一种铝塑复合膜,与实施例1的不同之处在于,保护层中,改性填料为经过硅烷偶联剂处理的含氟微粉。
上述改性填料,包括以下制备步骤:
将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4,搅拌混合3h后,加入预先混合的含氟微粉,在30kHz条件下超声搅拌混合2h,过滤,干燥,得到改性填料。
对比例4
一种铝塑复合膜,与实施例1的不同之处在于,保护层中,改性填料为经过硅烷偶联剂处理的硅粉。
上述改性填料,包括以下制备步骤:
将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4,搅拌混合3h后,加入预先混合的硅粉,在30kHz条件下超声搅拌混合2h,过滤,干燥,得到改性填料。
对本申请对比例1-4所得的铝塑复合膜,进行剥离力检测,并计算剥离力相对降低变化量,计算公式为:剥离力相对降低变化量=(初始剥离-末期剥离力)/初始剥离*100%,检测结果如下表所示。
通过对上表进行数据分析可知,相较于实施例1中阻透层和保护层的剥离力相对降低变化量,对比例1中阻透层和保护层的初始剥离力明显降低,阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,铝塑复合膜,由外到内,由外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层复合而成,可提高铝塑复合膜的耐电解液性能。分析其原因可能是,保护层中经过硅烷偶联剂处理的含氟微粉和硅粉具有良好的耐腐蚀性能,可阻挡渗透入保护层中的电解液继续渗透入第二胶黏剂层中,从而提高了铝塑复合膜的耐腐蚀性。同时,保护层中的马兰酸酐接枝聚丙烯与第二胶黏剂层和热封层具有良好的相容性,使得第二胶黏剂层和热封层的相容界面的分子链相互缠绕结合,提高保阻透层和保护层的粘结强度相较于实施例1中阻透层和保护层的剥离力相对降低变化量,对比例2、3、4中阻透层和保护层的初始剥离力明显降低,阻透层和保护层的剥离力相对降低变化量明显增加。由此表明,在铝塑复合膜的制备总原料中,改性填料为经过硅烷偶联剂处理的含氟微粉和硅粉,可提高铝塑复合膜的耐电解液性能,使得铝塑复合膜在电解液中浸泡24h后,阻透层和保护层依然具有较高的剥离力。分析其原因可能是,经过硅烷偶联剂处理的含氟微粉和硅粉在保护层中具有良好的相容性和粘结强度,使得保护层具有持久的耐腐蚀性能,从而保护层能阻挡渗透的电解液持续渗透入第二胶黏剂层中,从而提高了铝塑复合膜的耐电解液性能。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (9)
1.一种铝塑复合膜,其特征在于,由外到内,包括外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、保护层和热封层;
所述保护层,包括如下重量份数的组分:
三元无规共聚聚丙烯 100份;
相容剂 5-8份;
改性填料 10-25份;
成核剂 1-5份;
所述改性填料为经过硅烷偶联剂处理的含氟微粉和硅粉。
2.根据权利要求1所述的铝塑复合膜,其特征在于,所述改性填料的制备方法为:将硅烷偶联剂、水和有机溶剂混合后,得到混合液;调节混合液调节pH值为4-5,然后加入预先混合的含氟微粉和硅粉,搅拌混合,过滤,干燥,得到改性填料。
3.根据权利要求2所述的铝塑复合膜,其特征在于,所述硅烷偶联剂为苯基硅烷偶联剂和环氧基偶联剂中的一种或两种。
4.根据权利要求3所述的铝塑复合膜,其特征在于,所述硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂混合组成,硅烷偶联剂由苯基硅烷偶联剂和环氧基偶联剂的重量比为1:(0.8-1.2)。
5.根据权利要求1所述的铝塑复合膜,其特征在于,所述含氟微粉为聚四氟乙烯微粉、聚偏氟乙烯微粉和聚全氟乙丙烯微粉中的一种或多种。
6.根据权利要求2所述的铝塑复合膜,其特征在于,所述改性填料中,硅烷偶联剂、含氟微粉和硅粉的重量比为1:(0.2-0.4):(0.4-0.7)。
7.根据权利要求2所述的铝塑复合膜,其特征在于,所述硅粉还经过预处理,预处理步骤为:将硅粉加入pH值为9-11的碱性水溶液中,搅拌混合后,过滤,水洗,干燥,得到预处理的硅粉。
8.根据权利要求1所述的铝塑复合膜,其特征在于,所述相容剂为马兰酸酐接枝聚丙烯,所述马兰酸酐接枝聚丙烯的密度为0.92g/cm³,190℃,2.16Kg条件下的熔融指数为60-80g/10min。
9.权利要求1-8任一所述铝塑复合膜的制备方法,其特征在于,包括以下步骤:
S1:将三元无规共聚聚丙烯、相容剂、改性填料、成核剂混合后,熔融共挤出,得到保护层;
S2:由外到内,将外阻层、第一胶黏剂层、阻透层、第二胶黏剂层、S1所得保护层和热封层复合后,得到铝塑复合膜。
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