CN118388709A - Composite packaging adhesive film for battery assembly without main grid - Google Patents
Composite packaging adhesive film for battery assembly without main grid Download PDFInfo
- Publication number
- CN118388709A CN118388709A CN202410577008.8A CN202410577008A CN118388709A CN 118388709 A CN118388709 A CN 118388709A CN 202410577008 A CN202410577008 A CN 202410577008A CN 118388709 A CN118388709 A CN 118388709A
- Authority
- CN
- China
- Prior art keywords
- parts
- resin
- adhesive film
- intermediate product
- vinyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002313 adhesive film Substances 0.000 title claims abstract description 64
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 229920005989 resin Polymers 0.000 claims abstract description 45
- 239000011347 resin Substances 0.000 claims abstract description 45
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 41
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 37
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000004840 adhesive resin Substances 0.000 claims abstract description 24
- 229920006223 adhesive resin Polymers 0.000 claims abstract description 24
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 22
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000004611 light stabiliser Substances 0.000 claims abstract description 13
- 238000005266 casting Methods 0.000 claims abstract description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 52
- 239000013067 intermediate product Substances 0.000 claims description 50
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 47
- 239000000178 monomer Substances 0.000 claims description 47
- -1 amino vinyl Chemical group 0.000 claims description 43
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 43
- 239000000126 substance Substances 0.000 claims description 32
- 150000001336 alkenes Chemical class 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 20
- 239000003999 initiator Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 15
- HJIAMFHSAAEUKR-UHFFFAOYSA-N (2-hydroxyphenyl)-phenylmethanone Chemical compound OC1=CC=CC=C1C(=O)C1=CC=CC=C1 HJIAMFHSAAEUKR-UHFFFAOYSA-N 0.000 claims description 11
- 150000001412 amines Chemical class 0.000 claims description 11
- 229910044991 metal oxide Inorganic materials 0.000 claims description 11
- 150000004706 metal oxides Chemical class 0.000 claims description 11
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000006467 substitution reaction Methods 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- 238000005859 coupling reaction Methods 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 238000009966 trimming Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 230000032683 aging Effects 0.000 abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 102
- 239000010410 layer Substances 0.000 description 84
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 50
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 39
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 33
- 238000001914 filtration Methods 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 30
- 238000001035 drying Methods 0.000 description 23
- 238000003756 stirring Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 21
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 18
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 18
- 229910021641 deionized water Inorganic materials 0.000 description 18
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 18
- 238000005406 washing Methods 0.000 description 18
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 description 17
- 239000000706 filtrate Substances 0.000 description 17
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 16
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 16
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 14
- 239000000395 magnesium oxide Substances 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 12
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 12
- SNMOMUYLFLGQQS-UHFFFAOYSA-N 8-bromooct-1-ene Chemical compound BrCCCCCCC=C SNMOMUYLFLGQQS-UHFFFAOYSA-N 0.000 description 11
- 238000001291 vacuum drying Methods 0.000 description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 10
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 9
- 239000012141 concentrate Substances 0.000 description 9
- 239000012074 organic phase Substances 0.000 description 9
- 229910000027 potassium carbonate Inorganic materials 0.000 description 9
- MZFGYVZYLMNXGL-UHFFFAOYSA-N undec-10-enoyl chloride Chemical compound ClC(=O)CCCCCCCCC=C MZFGYVZYLMNXGL-UHFFFAOYSA-N 0.000 description 9
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 210000004027 cell Anatomy 0.000 description 8
- 238000003475 lamination Methods 0.000 description 8
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 8
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 8
- ZMXDDKWLCZADIW-WFVSFCRTSA-N 1-deuterio-n,n-dimethylformamide Chemical compound [2H]C(=O)N(C)C ZMXDDKWLCZADIW-WFVSFCRTSA-N 0.000 description 7
- NQSLZEHVGKWKAY-UHFFFAOYSA-N 6-methylheptyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C(C)=C NQSLZEHVGKWKAY-UHFFFAOYSA-N 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 125000004093 cyano group Chemical group *C#N 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 6
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 6
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 description 6
- 238000003466 welding Methods 0.000 description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 125000003700 epoxy group Chemical group 0.000 description 5
- 125000004185 ester group Chemical group 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- HTQNYBBTZSBWKL-UHFFFAOYSA-N 2,3,4-trihydroxbenzophenone Chemical compound OC1=C(O)C(O)=CC=C1C(=O)C1=CC=CC=C1 HTQNYBBTZSBWKL-UHFFFAOYSA-N 0.000 description 4
- 125000006414 CCl Chemical group ClC* 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- FKGFCVJJLGSFSB-UHFFFAOYSA-N non-8-en-1-ol Chemical compound OCCCCCCCC=C FKGFCVJJLGSFSB-UHFFFAOYSA-N 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 150000003384 small molecules Chemical class 0.000 description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 3
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- MOVRCMBPGBESLI-UHFFFAOYSA-N prop-2-enoyloxysilicon Chemical group [Si]OC(=O)C=C MOVRCMBPGBESLI-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical group [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 3
- 230000003313 weakening effect Effects 0.000 description 3
- MLQBTMWHIOYKKC-KTKRTIGZSA-N (z)-octadec-9-enoyl chloride Chemical compound CCCCCCCC\C=C/CCCCCCCC(Cl)=O MLQBTMWHIOYKKC-KTKRTIGZSA-N 0.000 description 2
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- QGFSQVPRCWJZQK-UHFFFAOYSA-N 9-Decen-1-ol Chemical compound OCCCCCCCCC=C QGFSQVPRCWJZQK-UHFFFAOYSA-N 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical group CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 description 2
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 125000002587 enol group Chemical group 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- UIZVMOZAXAMASY-UHFFFAOYSA-N hex-5-en-1-ol Chemical compound OCCCCC=C UIZVMOZAXAMASY-UHFFFAOYSA-N 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229920006280 packaging film Polymers 0.000 description 2
- 239000012785 packaging film Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- RIPYNJLMMFGZSX-UHFFFAOYSA-N (5-benzoylperoxy-2,5-dimethylhexan-2-yl) benzenecarboperoxoate Chemical compound C=1C=CC=CC=1C(=O)OOC(C)(C)CCC(C)(C)OOC(=O)C1=CC=CC=C1 RIPYNJLMMFGZSX-UHFFFAOYSA-N 0.000 description 1
- LEAQUNCACNBDEV-ZHACJKMWSA-N (e)-undec-1-en-1-ol Chemical compound CCCCCCCCC\C=C\O LEAQUNCACNBDEV-ZHACJKMWSA-N 0.000 description 1
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 1
- CZZZWEDUOMBCQE-UHFFFAOYSA-N 1-bromoundec-1-ene Chemical compound CCCCCCCCCC=CBr CZZZWEDUOMBCQE-UHFFFAOYSA-N 0.000 description 1
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- MUUOUUYKIVSIAR-UHFFFAOYSA-N 2-but-3-enyloxirane Chemical compound C=CCCC1CO1 MUUOUUYKIVSIAR-UHFFFAOYSA-N 0.000 description 1
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 description 1
- UKTHULMXFLCNAV-UHFFFAOYSA-N 2-hex-5-enyloxirane Chemical compound C=CCCCCC1CO1 UKTHULMXFLCNAV-UHFFFAOYSA-N 0.000 description 1
- VXDHQYLFEYUMFY-UHFFFAOYSA-N 2-methylprop-2-en-1-amine Chemical compound CC(=C)CN VXDHQYLFEYUMFY-UHFFFAOYSA-N 0.000 description 1
- FCZHJHKCOZGQJZ-UHFFFAOYSA-N 2-oct-7-enyloxirane Chemical compound C=CCCCCCCC1CO1 FCZHJHKCOZGQJZ-UHFFFAOYSA-N 0.000 description 1
- AIBRSVLEQRWAEG-UHFFFAOYSA-N 3,9-bis(2,4-ditert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP1OCC2(COP(OC=3C(=CC(=CC=3)C(C)(C)C)C(C)(C)C)OC2)CO1 AIBRSVLEQRWAEG-UHFFFAOYSA-N 0.000 description 1
- DMAYBPBPEUFIHJ-UHFFFAOYSA-N 4-bromobut-1-ene Chemical compound BrCCC=C DMAYBPBPEUFIHJ-UHFFFAOYSA-N 0.000 description 1
- UWDMKTDPDJCJOP-UHFFFAOYSA-N 4-hydroxy-2,2,6,6-tetramethylpiperidin-1-ium-4-carboxylate Chemical compound CC1(C)CC(O)(C(O)=O)CC(C)(C)N1 UWDMKTDPDJCJOP-UHFFFAOYSA-N 0.000 description 1
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 description 1
- LPNANKDXVBMDKE-UHFFFAOYSA-N 5-bromopent-1-ene Chemical compound BrCCCC=C LPNANKDXVBMDKE-UHFFFAOYSA-N 0.000 description 1
- RIMXEJYJXDBLIE-UHFFFAOYSA-N 6-bromohex-1-ene Chemical compound BrCCCCC=C RIMXEJYJXDBLIE-UHFFFAOYSA-N 0.000 description 1
- GNYDYUQVALBGGZ-UHFFFAOYSA-N 7-bromohept-1-ene Chemical compound BrCCCCCC=C GNYDYUQVALBGGZ-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- RECMXUUCYFGBEZ-UHFFFAOYSA-N cyclohexyl cyclohexyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC1CCCCC1 RECMXUUCYFGBEZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- PKNLWLCURZNADF-UHFFFAOYSA-N hex-5-enoyl chloride Chemical compound ClC(=O)CCCC=C PKNLWLCURZNADF-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- LQAVWYMTUMSFBE-UHFFFAOYSA-N pent-4-en-1-ol Chemical compound OCCCC=C LQAVWYMTUMSFBE-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 150000003141 primary amines Chemical group 0.000 description 1
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- GRJISGHXMUQUMC-UHFFFAOYSA-N silyl prop-2-enoate Chemical compound [SiH3]OC(=O)C=C GRJISGHXMUQUMC-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- RCFUFEMQNKVAGF-UHFFFAOYSA-N undec-2-enoyl chloride Chemical compound CCCCCCCCC=CC(Cl)=O RCFUFEMQNKVAGF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to the field of photovoltaic materials. The invention relates to a composite packaging adhesive film for a main-grid-free battery assembly, which is prepared by optimally designing an EVA layer and a POE layer through a formula, extruding by an extruder and casting to form a film. Wherein 100 parts of EVA resin of the EVA layer; 0.8-1.2 parts of cross-linking agent; 1.0-1.5 parts of auxiliary cross-linking agent; 4.0-6.0 parts of functional auxiliary agent; 0.1-0.2 part of antioxidant; 0.3-0.5 part of silane coupling agent as raw material; 100 parts of POE resin is used for the POE layer; 10-15 parts of PP resin; 8-12 parts of adhesive resin; 0.5-1.0 part of cross-linking agent; 1.0-1.5 parts of auxiliary cross-linking agent; 0.05-0.20 part of antioxidant; 0.05-0.15 part of light stabilizer is used as raw material. The composite adhesive film effectively solves the problems that in the prior art, the waterproof and ageing-resistant performance of the joint of the packaging adhesive film of the battery pack without the main grid is relatively poor, the adhesive force between the adhesive film and the battery piece is relatively weak, and the like.
Description
Technical Field
The invention relates to a composite packaging adhesive film for a battery component without a main grid. The invention belongs to the field of photovoltaic materials.
Background
Non-primary grid cells are increasingly receiving attention in the photovoltaic field due to their great potential in terms of solar energy conversion efficiency. Such cells are typically composed of multiple layers of semiconductor material to achieve higher light absorption efficiency and electron conduction performance. However, packaging technology is a critical challenge in the fabrication and application of non-primary gate cells. Conventional packaging methods often have difficulty meeting the special requirements of cells without a main grid, and packaging of these cells requires higher process accuracy to ensure that the optical and electrical properties of the material are not affected.
At present, the traditional photovoltaic packaging adhesive film on the market cannot be suitable for a battery assembly without a main grid, the welding strip is easy to displace in the lamination process, and the welding strip and the battery piece are easy to generate the phenomenon of virtual connection. The existing support layer of the integrated adhesive film without the main grid bearing and packaging is mainly EVA resin, and has lower peeling strength to the battery piece due to higher crosslinking degree, and meanwhile, the EVA can generate acetate ions under the damp and hot condition to generate certain corrosion effect to the welding belt; meanwhile, the shrinkage rate is high, so that the situation of the virtual joint of the welding strip is common; and the use of POE resin as the packaging adhesive film has the factor of insufficient adhesion of POE material to the battery and glass. In addition, the packaging adhesive film not only needs higher bonding strength, so that the problem of displacement and virtual connection of the welding strip in the lamination process is solved, but also has better water vapor barrier property and low corrosiveness. Therefore, a novel bearing packaging adhesive film for a photovoltaic module needs to be developed to meet the related requirements of a battery module without a main grid.
Disclosure of Invention
The invention aims to solve the problems that the joint of a packaging adhesive film of a battery component without a main grid is relatively poor in water resistance and ageing resistance, the adhesive force between the adhesive film and a battery piece is relatively weak, and the like in the prior art, and provides a composite packaging adhesive film for the battery component without the main grid and a preparation method thereof. The self-made functional auxiliary agent and the adhesive resin are used for preparing the composite material through coextrusion, so that the composite material has excellent viscosity, ageing resistance and corrosion resistance and has wide application potential. The technical scheme adopted for solving the technical problems is as follows:
A preparation method of a functional auxiliary agent comprises the following steps:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
S12, carrying out polymerization reaction on the vinyl monomer A and the intermediate product I under the action of an initiator A to obtain an intermediate product II;
S13, placing the nanoscale metal oxide and a silane coupling agent in an alcohol solvent for a coupling reaction to obtain an intermediate product III;
S14, performing coupling reaction on the intermediate product II and the intermediate product III to obtain a target product.
Further, the hydroxyl group-containing structural substance is a substance containing hydroxyl groups and having a light-stable structure; and
The usage ratio of the hydroxyl-containing structural material to the halogenated alkene is 1:1.
Further, the substance containing hydroxyl and having a light stable structure is added by the molar ratio of o-hydroxybenzophenones to hindered amines of 1.0-3.0:1.0.
Further, the vinyl monomer A is amino vinyl, hydroxy vinyl and ester vinyl according to the mol ratio of 4.0-6.0:2.0-4.0:2.0 adding; and
The amino alkene is that alkenyl amine and alkenyl amide are mixed according to a mol ratio of 1.0:2.0-4.0;
the hydroxy alkene is enol or/and hydroxy acrylic ester;
The ester group alkene is (methyl) acrylic ester or/and non-acrylic ester.
Further, the dosage ratio of the vinyl monomer A to the intermediate product I is 8.0-9.5mol:0.5-2.0mol.
Further, the metal oxide, the silane coupling agent and the alcohol solvent are used in an amount of 1g:3.3-5.5g:80mL.
Further, the dosage ratio of the intermediate II to the intermediate III is 10g:2.0-3.0g.
Another object of the present invention is to provide a functional auxiliary agent prepared by the preparation method.
A method of preparing a tackifying resin comprising the steps of:
S21, carrying out polymerization reaction on the vinyl monomer B under the action of an initiator B to obtain a target product.
Further, the vinyl monomer B is epoxy vinyl, ester vinyl, styrene, acrylonitrile and silane vinyl according to the mol ratio of 4.0-5.0:1.0-2.0:1.0-2.0:1.0-2.0:1.0 addition.
It is another object of the present invention to provide a tacky resin prepared by the method of preparation.
The invention also aims to provide a composite packaging adhesive film for a battery component without a main grid, which comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
0.8-1.2 parts of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
4.0-6.0 parts of functional auxiliary agent;
0.1-0.2 part of antioxidant;
0.3-0.5 part of silane coupling agent;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
10-15 parts of PP resin;
8-12 parts of adhesive resin;
0.5-1.0 part of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
0.05-0.20 part of antioxidant;
0.05-0.15 part of light stabilizer.
The invention also provides a preparation method of the composite packaging adhesive film for the battery component without the main grid, which comprises the following steps:
S31, mixing, i.e
Mixing and configuring the raw materials of each layer in a mixer according to a formula to obtain mixed raw materials for later use;
s32, co-extrusion, i.e
Respectively placing the mixed raw materials in the step S31 into an extruder, and carrying out melt blending, coextrusion, casting, traction, stretching and cooling; and
S33, film formation, i.e
And (3) performing thickness measurement, edge pressing, shaping, trimming and rolling to obtain the composite packaging adhesive film for the battery component without the main grid.
The invention has the beneficial effects that:
(1) The invention provides a composite packaging adhesive film for a main-grid-free battery assembly, wherein a self-made functional auxiliary agent is contained in an EVA layer formula system, and the EVA layer formula system is of an organic-inorganic hybrid core-shell structure; the core layer is nano-scale metal oxide, and the shell structure contains macromolecular chains of silane, amino, amido, hydroxyl, ester group, o-hydroxybenzophenone and hindered amine structures. Firstly, the metal oxide is an inorganic filler, so that the shrinkage rate of the adhesive film can be effectively reduced in the adhesive film lamination process, the displacement and virtual joint of a welding strip are reduced, and the adhesive has excellent adhesion to a base material; the second, nano-scale metal oxide has large specific surface area, can absorb free acid better, and has excellent corrosion resistance; on the one hand, polar groups such as amido, amino, hydroxyl, ester group and the like in the macromolecular chains can further improve the adhesive force of the adhesive film; on the other hand, the anti-corrosion agent has an inhibition effect on free acetic acid, and further improves the anti-corrosion performance; fourth, the macromolecule polar structure has excellent adsorptivity to small molecules in the EVA layer, so that the migration of the small molecules to the interface is reduced, and the adhesion between EVA and the interface is improved; and fifth, the hindered amine and the o-hydroxybenzophenone in the macromolecular chain are used as traditional light stabilizer and ultraviolet absorber components, so that the ultraviolet light stabilizer has excellent anti-oxidation and anti-aging effects, and the hindered amine and the o-hydroxybenzophenone have more excellent photo-oxidation and anti-aging effects under a proper proportion.
(2) The invention provides a composite packaging adhesive film for a main-grid-free battery assembly, which comprises a POE layer formula system and a self-made adhesive resin, wherein the POE layer formula system is a macromolecular chain with side groups containing epoxy groups, ester groups, phenyl groups, cyano groups and silane structures. Firstly, the chain entanglement of macromolecules, the main chain structure of a carbon chain and a phenyl structure ensure that the macromolecular polyurethane has certain compatibility in POE; the polar structure of the epoxy group, the ester group and the cyano group of the second side group has excellent adhesion to the EVA layer on one hand, and the delamination of the composite adhesive film is avoided; on the other hand, the polar micromolecular auxiliary agent can be adsorbed, so that delamination caused by the influence of migration to an interface on the bonding performance is avoided; the third, pendant silane structure focuses on adhesion to the substrate; fourth, the adhesive resin in the POE layer and the functional auxiliary agent shell layer in the EVA have similar structures, so that the bonding strength of the co-extrusion surface can be further improved.
(3) The invention provides a composite packaging adhesive film for a main-grid-free battery assembly, wherein a POE layer formula system contains PP resin, and on one hand, the PP resin also has excellent water blocking performance; on the other hand, the PP resin is easy to crystallize, has higher melting temperature and has positive effect on prolonging the service life of the packaging adhesive film under severe environment.
(4) The invention provides a composite packaging adhesive film for a main-grid-free battery assembly, which is formed by coextruding a POE layer and an EVA layer, wherein the low-shrinkage characteristic of the POE layer plays a supporting role on the EVA layer, so that the shrinkage rate of the EVA layer is reduced, and the adhesive force is improved.
(5) The invention provides a preparation method of a composite packaging adhesive film for a main-grid-free battery assembly, which reduces the use of small molecule auxiliary agents and improves the adhesive force between layers through formulation design; and is prepared by a coextrusion process. The composite packaging adhesive film also has excellent PID resistance and the like due to the blocking effect of the POE layer. The method has strong operability and practical significance for realizing industrialization of the product of the invention.
Detailed Description
The present invention will be described in detail with reference to examples. It is to be understood that the following examples are illustrative of embodiments of the present invention and are not intended to limit the scope of the invention.
The invention aims to develop a composite packaging adhesive film for a battery assembly without a main grid, so as to meet the application requirements of the existing battery assembly without the main grid. The realization thought is as follows: firstly, aiming at the defects of the existing single-layer adhesive film, the problems of water resistance, weather resistance, weld joint virtual joint displacement and the like caused by shrinkage rate are solved to a certain extent by using an EP two-layer composite adhesive film; then, aiming at the defects of the EVA layer and the POE layer, and from the aspect of reducing the use of small molecule auxiliary agents as much as possible, a solution scheme is designed. The method comprises the following steps: in one aspect, an EP composite adhesive film is prepared using a coextrusion technique; on the other hand, functional auxiliary agents used for the EVA layer and adhesive resin used for the POE layer are respectively prepared by self, and the lower adhesive force of the substrate is respectively modified aiming at the water resistance and weather resistance of the EVA layer, the high shrinkage rate and the POE layer. The theoretical basis of the realization is as follows: through molecular structure design, a series of reactions are firstly carried out, including substitution reaction of active hydrogen, free radical polymerization reaction of double bonds, silane coupling reaction of inorganic matters and preparation of functional auxiliary agent by coupling substitution reaction; the adhesive resin is obtained by free radical polymerization of double bonds; and then the functional auxiliary agent is used for the EVA layer and the adhesive resin is used for the POE layer to carry out coextrusion so as to obtain the composite adhesive film which has the effects of excellent water resistance, weather resistance, adhesive force, low shrinkage rate and the like. Embodiments of the invention are as follows:
The embodiment of the invention provides a preparation method of a functional auxiliary agent, which comprises the following steps:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
the hydroxyl-containing structural material is a material containing hydroxyl and having a light stable structure; and
The substance containing hydroxyl and having a light stable structure is added by the molar ratio of o-hydroxybenzophenone and hindered amine of 1.0-3.0:1.0.
S11 includes S111 and/or S112,
S111, adding a hydroxyl-containing structural substance A and an acid binding agent A into N, N-dimethylacetamide A, dissolving halogenated alkene A in N, N-dimethylformamide B, placing in a constant pressure dropping funnel, ice-bath, stirring, controlling the temperature of 0-5 ℃ to continuously react for 8-14h after the dropping is finished, and performing the reaction; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane A, adding saturated sodium bicarbonate solution A into the solution, washing for 3 times, washing with deionized water A for 3 times, separating, taking an organic phase, drying with anhydrous sodium sulfate A, filtering, distilling the filtrate under reduced pressure, and drying in vacuum at 80 ℃ for 4 hours to obtain an intermediate product IA.
The dosage ratio of the hydroxyl-containing structural substance A to the acid binding agent A, N to the N-dimethylformamide A to the halogenated alkene A, N to the N-dimethylformamide B to the dichloromethane A to the saturated sodium bicarbonate solution A to the deionized water A to the anhydrous sodium sulfate A is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
The hydroxyl-containing structural substance A is a substance containing hydroxyl and having a light stable structure;
The substances containing hydroxyl groups and having a light stable structure are o-hydroxybenzophenones and/or hindered amines;
The o-hydroxybenzophenones may be 2, 4-dihydroxybenzophenone, 2, 4-tetrahydroxybenzophenone, 2,3, 4-tetrahydroxybenzophenone, 2, 4-trihydroxybenzophenone, etc.; and, 2, 4-dihydroxybenzophenone is preferred.
The hindered amine can be 2, 6-tetramethyl-4-piperidinol 1,2, 6-pentamethyl-4-piperidinol or 4-hydroxy-2, 6-tetramethylpiperidyloxy and the like; and, 2, 6-tetramethyl-4-piperidinol is preferable.
The acid binding agent A can be pyridine, triethylamine and potassium carbonate; and, triethylamine is preferable.
The halogenated alkene A can be oleoyl chloride, palm oleoyl chloride, undecenoyl chloride, 5-hexenoyl chloride, 4-butenoyl chloride and the like; and, undecylenoyl chloride is preferred.
S112, adding a hydroxyl-containing structural substance B, an acid binding agent B and a polymerization inhibitor into N, N-dimethylformamide C, dissolving halogenated alkene B into N, N-dimethylformamide D, placing into a constant pressure dropping funnel, heating to 100-120 ℃ and stirring, controlling the temperature to continue to react for 1-2h after the dropping is finished, and after the reaction is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane B, adding saturated sodium bicarbonate solution B into the solution, washing for 3 times, washing with deionized water B for 3 times, separating, taking organic phase, drying with anhydrous sodium sulfate B, filtering, distilling the filtrate under reduced pressure, and vacuum drying at 80deg.C for 4h to obtain intermediate IB.
The dosage ratio of the hydroxyl-containing structural substance B, the acid binding agent B, N, the N-dimethylformamide C, the halogenated alkene B, N, the N-dimethylformamide D, the dichloromethane B, the saturated sodium bicarbonate solution B, the deionized water B and the anhydrous sodium sulfate B is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
the hydroxyl-containing structural substance B is a substance containing hydroxyl and having a light stable structure;
The substance containing hydroxyl and having a light stable structure is o-hydroxybenzophenone;
The o-hydroxybenzophenones may be 2, 4-dihydroxybenzophenone, 2, 4-tetrahydroxybenzophenone, 2,3, 4-tetrahydroxybenzophenone, 2, 4-trihydroxybenzophenone, etc.; and, 2, 4-dihydroxybenzophenone is preferred.
The acid binding agent B can be pyridine, triethylamine and potassium carbonate; and, potassium carbonate is preferable.
The halogenated alkene B can be 4-bromo-1-butene, 5-bromo-1-pentene, 6-bromo-1-hexene, 7-bromo-1-heptene, 8-bromo-1-octene, bromoundecene and the like; and, 8-bromo-1-octene is preferred.
The amount of the polymerization inhibitor is 0.5% of the mass of the halogenated alkene B.
The polymerization inhibitor can be hydroquinone, p-hydroxyanisole, tertiary butyl hydroquinone and the like; and, tertiary butyl hydroquinone is preferred.
S12, adding an alkene monomer A, an intermediate product I and an initiator AIBN into N, N-dimethylformamide E, heating to 75-85 ℃, and stirring for 6-10h; after the reaction is finished, the temperature is reduced to room temperature, the filtration is carried out, the filtrate is taken, the distillation is carried out under reduced pressure, and the vacuum drying is carried out for 6 hours at 60 ℃ to obtain an intermediate product II.
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 8.0-9.5mol:0.5 to 2.0mol:800mL.
The vinyl monomer A is amino vinyl, hydroxy vinyl and ester vinyl according to the mol ratio of 4.0-6.0:2.0-4.0:2.0 addition.
The amino alkene is that alkenyl amine and alkenyl amide are mixed according to a mol ratio of 1.0:2.0-4.0;
The alkenylamine, wherein the amino structure is required to be reacted with intermediate III in the next step, preferably a primary amine structure; the alkenylamine may be allylamine, 2-methylallylamine, or the like; and, allyl amine is preferred;
The alkenyl amide has higher polarity of the amide structure, and has higher bonding strength to the substrate, so that a higher proportion is required; the alkenylamide may be acrylamide, diacetone acrylamide, etc.; and diacetone acrylamide is preferable.
The hydroxy alkene is enol or/and hydroxy acrylic ester;
The enol may be 4-penten-1-ol, 5-hexen-1-ol, 8-nonen-1-ol, 9-decen-1-ol, undecenol, etc.; and, 8-nonen-1-ol is preferable;
the hydroxy acrylate may be hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, 4-hydroxybutyl acrylate, etc.; and, hydroxyethyl methacrylate is preferable.
The ester-based vinyl may be methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, isooctyl (meth) acrylate, or the like; and, ethyl methacrylate is preferable.
The amount of the initiator AIBN is 1.0-1.5% of the total mass of the vinyl monomer and the intermediate product I.
S13, adding the nanoscale metal oxide and the silane coupling agent into an alcohol solvent, carrying out ultrasonic oscillation for 0.5h, standing for 2h at room temperature, reacting for 6-10h at 40-60 ℃, filtering, taking insoluble matters, and drying for 12h at 40 ℃ to obtain an intermediate product III.
The dosage ratio of the nanoscale metal oxide to the silane coupling agent to the alcohol solvent is 1g:3.5-5.5g:80mL.
The nanoscale metal oxide can be magnesium oxide, aluminum oxide, zinc oxide or the like; and, magnesium oxide is preferable;
the magnesium oxide has a particle size of 500-1000nm, model DK-MgO-002, and is purchased from Beijing Kodaku island gold technology Co.
The alumina has an average particle diameter of 500nm and a model DK-Al2O3-500, and is purchased from Beijing De island gold technology Co.
The zinc oxide has an average particle diameter of 200nm, the model ZT-J300 and is purchased from Zhejiang Zhi Titania micro new material Co.
The silane coupling agent is an acryloxy silane coupling agent or an epoxy silane coupling agent;
The acryloyloxy silane coupling agent can be KH570, KH571, KH670, GX572 and the like; also, GX572 is preferable.
The epoxy silane coupling agent can be KH560 and the like; and, KH560 is preferable.
The alcohol solvent can be absolute methanol, absolute ethanol, absolute isopropanol and the like; and, absolute ethanol is preferable.
S14, adding the intermediate product II and the intermediate product III into N, N-dimethylformamide F, heating to 40-60 ℃, stirring for 3-6h, distilling under reduced pressure, and drying in a vacuum oven at 40 ℃ for 12h to obtain the target product.
The dosage ratio of the intermediate II to the intermediate III to the N, N-dimethylformamide F is 10g:2.0-3.0g:400mL.
A method of preparing a tackifying resin comprising the steps of:
S21, adding an alkene monomer B and an initiator AIBN into N, N-dimethylformamide G, heating to 75-85 ℃, and stirring for 6-10h; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and drying in vacuum at 60 ℃ for 6 hours to obtain a target product.
The vinyl monomer B is epoxy vinyl, ester vinyl, styrene, acrylonitrile and silane vinyl according to the mol ratio of 4.0-5.0:1.0-2.0:1.0-2.0:1.0-2.0:1.0 addition of
The epoxyalkene can be glycidyl methacrylate, allyl glycidyl ether, 1, 2-epoxy-5-hexene, 1, 2-epoxy-7-octene or 1, 2-epoxy-9-decene, etc.; and, allyl glycidyl ether is preferable.
The ester-based vinyl may be methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, isooctyl (meth) acrylate, or the like; and, isooctyl methacrylate is preferable.
The silane alkene is vinyl silane or acryloxy silane;
The vinyl silane can be KH151, KH171, KH172, etc.;
the acryloxysilane can be KH570, KH571, KH670, GX572, or the like; and, KH570 is preferable.
The amount of the initiator AIBN is 1.0-1.5% of the total mass of the vinyl monomer.
The embodiment of the invention provides a composite packaging adhesive film for a battery assembly without a main grid, which comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
0.8-1.2 parts of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
4.0-6.0 parts of functional auxiliary agent;
0.1-0.2 part of antioxidant;
0.3-0.5 part of silane coupling agent;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
10-15 parts of PP resin;
8-12 parts of adhesive resin;
0.5-1.0 part of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
0.05-0.20 part of antioxidant;
0.05-0.15 part of light stabilizer.
The EVA resin disclosed by the invention has the VA content of 28-33%. EVA resins having a VA content of 33% and a Melt Index (MI) of 31, purchased from DuPont, U.S. are preferred in the following examples of the present invention.
POE resin of the present invention, model XUS38660, was purchased from Dow chemical company, USA, and described in the following examples.
The PP resin in the following examples of the present invention is designated 1300 manufactured by Yanshan petrochemical company.
The cross-linking agent in the invention can be benzoyl peroxide, 2, 5-dimethyl-2, 5-bis (benzoyl peroxide) hexane, dicyclohexyl peroxycarbonate or dicumyl peroxide and the like; the crosslinker in the following examples of the invention is 2, 5-dimethyl-2, 5-bis (benzoylperoxy) hexane.
The auxiliary crosslinking agent is allyl and/or acryloxy.
The allyl auxiliary crosslinking agent can be triallyl cyanurate, triallyl isocyanurate and the like.
The acryloyloxy auxiliary crosslinking agent can be any composition of trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, propoxylated neopentyl glycol diacrylate and pentaerythritol triacrylate.
The auxiliary cross-linking agent in the following examples of the invention is triallyl isocyanurate, trimethylolpropane trimethacrylate and propoxylated trimethylolpropane triacrylate and pentaerythritol triacrylate which are added according to the mass ratio of 8:3:2:2.
The antioxidant is formed by compounding hindered phenols and phosphites. The hindered phenol antioxidant can be antioxidant 1010, antioxidant 1076, antioxidant 264, antioxidant 2246, etc.; and, antioxidant 1010 is preferable. The phosphite antioxidant can be antioxidant 168, antioxidant 242, antioxidant TPP, etc.; and, an antioxidant 168 is preferable. In the following examples of the present invention, antioxidant 1010 and antioxidant 168 were added in a mass ratio of 1:2.
The light stabilizer in the invention is hindered amine. The hindered amine can be UV-292, UV-770, GW540, or the like; also, UV-292 is preferred. The light stabilizer in the following examples of the present invention was UV-292.
The coupling agent in the following examples is a silane coupling agent, specifically a vinyl silane coupling agent, and may be KH151 or KH 171; and, KH171 is preferable.
In order to better understand the above-mentioned invention, the preparation method of the composite packaging adhesive film for the battery component without the main grid in the following embodiment of the invention comprises the following steps:
S31, mixing, i.e
Mixing and configuring the raw materials of each layer in a mixer according to a formula, and mixing and stirring for 2 hours at the temperature of 40 ℃ and the rotating speed of 80rpm to obtain mixed raw materials for later use;
s32, co-extrusion, i.e
Placing POE layer raw materials into a double-screw extruder, and carrying out melt blending at the temperature of 90 ℃, 95 ℃, 105 ℃ and 110 ℃ and the rotating speed of 50rpm in each region; placing EVA layer raw materials into a double-screw extruder, melting and blending at the temperature of 80 ℃, 90 ℃, 100 ℃, 105 ℃ and the rotation speed of 45rpm in each region, discharging through a coextrusion casting film die head, and drawing and stretching; and
S33, film formation, i.e
And (3) measuring thickness, pressing edges, shaping, trimming, and rolling to obtain the composite packaging adhesive film (the total thickness is 500 mu m, the POE layer is 200 mu m, and the EVA layer is 300 mu m) for the cell component without the main grid.
In order to further understand the present invention, the following detailed description is provided with reference to specific embodiments of a composite packaging adhesive film for a battery assembly without a main grid, and the scope of the present invention is not limited by the following embodiments.
Example 1
A preparation method of a functional auxiliary agent comprises the following steps:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
the hydroxyl-containing structural material is a material containing hydroxyl and having a light stable structure; and
The substance containing hydroxyl and having a light stable structure is added with 2, 4-dihydroxybenzophenone and 2, 6-tetramethyl-4-piperidinol according to a molar ratio of 2.0:1.0.
S11 includes S111 and S112,
S111, adding 2, 6-tetramethyl-4-piperidinol and triethylamine into N, N-dimethylacetamide A, dissolving undecylenoyl chloride into N, N-dimethylformamide B, placing into a constant pressure dropping funnel, ice-bath, stirring, controlling the temperature at 0 ℃ to continue to react for 10 hours after the dropping is finished, and controlling the temperature to be lower than the temperature of the mixture; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane A, adding saturated sodium bicarbonate solution A into the solution, washing for 3 times, washing with deionized water A for 3 times, separating, taking an organic phase, drying with anhydrous sodium sulfate A, filtering, distilling the filtrate under reduced pressure, and drying in vacuum at 80 ℃ for 4 hours to obtain an intermediate product IA.
The dosage ratio of the 2, 6-tetramethyl-4-piperidinol, triethylamine, N-dimethylformamide A, undecylenoyl chloride, N-dimethylformamide B, dichloromethane A, saturated sodium bicarbonate solution A, deionized water A and anhydrous sodium sulfate A is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g.
The infrared data are as follows: 3512cm -1: -OH is absent; 3287cm -1: -NH- (spike) present; 1735cm -1: -c=o present; 1622cm -1: -c=c-present; 703cm -1: C-Cl is absent.
S112, adding 2, 4-dihydroxybenzophenone, potassium carbonate and tertiary butyl hydroquinone into N, N-dimethylformamide C, dissolving 8-bromo-1-octene in N, N-dimethylformamide D, placing in a constant pressure dropping funnel, heating to 110 ℃ and stirring, controlling the temperature to continue to react for 1.5h after the dropping is finished, and after the reaction is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane B, adding saturated sodium bicarbonate solution B into the solution, washing for 3 times, washing with deionized water B for 3 times, separating, taking organic phase, drying with anhydrous sodium sulfate B, filtering, distilling the filtrate under reduced pressure, and vacuum drying at 80deg.C for 4h to obtain intermediate IB.
The dosage ratio of the 2, 4-dihydroxybenzophenone, the potassium carbonate, the N, N-dimethylformamide C, the 8-bromo-1-octene, the N, N-dimethylformamide D, the methylene dichloride B, the saturated sodium bicarbonate solution B, the deionized water B and the anhydrous sodium sulfate B is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
the dosage of the tertiary butyl hydroquinone is preferably 0.5 percent of the mass of the 8-bromo-1-octene.
The infrared data are as follows: 3501cm -1: -OH present and reduced; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1621cm -1: -c=c-present; 647cm -1: -C-Br is absent.
S12, adding an alkene monomer A, an intermediate product I and an initiator AIBN into N, N-dimethylformamide E, heating to 80 ℃, and stirring for 8 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain an intermediate product II #PDI＝1.66)。
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 8.5mol:1.5mol:800mL.
The vinyl monomer A is amino vinyl, 8-nonen-1-alcohol and ethyl methacrylate according to the mol ratio of 5.0:3.0:2.0 addition.
The amino alkene is allylamine and diacetone acrylamide according to the mol ratio of 1.0:3.0 mixing;
the amount of the initiator AIBN is 1.0 percent of the total mass of the vinyl monomer and the intermediate product I.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
S13, adding nano-grade magnesium oxide and a silane coupling agent GX572 into an absolute ethyl alcohol solvent, carrying out ultrasonic oscillation for 0.5h, standing for 2h at room temperature, reacting for 10h at 40 ℃, filtering, taking insoluble matters, and drying for 12h at 40 ℃ to obtain an intermediate product III.
The dosage ratio of the nano-grade magnesium oxide to the silane coupling agent GX572 to the absolute ethyl alcohol solvent is 1g:4.5g:80mL.
The infrared data are as follows: 3440cm -1: -OH weakening; 1735cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-present; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
S14, adding the intermediate product II and the intermediate product III into N, N-dimethylformamide F, heating to 40 ℃, stirring for 6 hours, distilling under reduced pressure, and drying in a vacuum oven at 40 ℃ for 12 hours to obtain the target product.
The dosage ratio of the intermediate II to the intermediate III to the N, N-dimethylformamide F is 10g:2.5g:400mL.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present and abated; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-absent; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
A method of preparing a tackifying resin comprising the steps of:
S21, adding an alkene monomer B and an initiator AIBN into N, N-dimethylformamide G, heating to 80 ℃, and stirring for 8 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain a target product @ PDI＝1.62)。
The vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 4.0:1.5:1.5:2.0:1.0 addition.
The amount of the initiator AIBN is 1.0 percent of the total mass of the vinyl monomer.
The infrared data are as follows: 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 2258cm -1: cyano groups are present; 1735cm -1: -c=o present; 1218cm -1、911cm-1、835cm-1: the epoxy group is present; 1109cm -1、801cm-1: -Si-O-presence; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
1.0 part of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
5.0 parts of functional auxiliary agent;
0.15 parts of antioxidant;
0.4 part of silane coupling agent KH 171;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
13 parts of PP resin;
10 parts of adhesive resin;
0.8 parts of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
0.14 parts of antioxidant;
0.10 parts of light stabilizer.
Example 2
Otherwise, the embodiment 1 is different in that:
A preparation method of a functional auxiliary agent comprises the following steps:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
the hydroxyl-containing structural material is a material containing hydroxyl and having a light stable structure; and
The substance containing hydroxyl and having a light stable structure is added with 2, 4-dihydroxybenzophenone and 2, 6-tetramethyl-4-piperidinol according to a molar ratio of 2.0:1.0.
S11 includes S111 and S112,
S111, adding 2, 6-tetramethyl-4-piperidinol and triethylamine into N, N-dimethylacetamide A, dissolving undecylenoyl chloride into N, N-dimethylformamide B, placing into a constant pressure dropping funnel, ice-bath, stirring, controlling the temperature at 5 ℃ to continue to react for 8 hours after the dropping is finished, and controlling the temperature to be lower than the temperature of the mixture; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane A, adding saturated sodium bicarbonate solution A into the solution, washing for 3 times, washing with deionized water A for 3 times, separating, taking an organic phase, drying with anhydrous sodium sulfate A, filtering, distilling the filtrate under reduced pressure, and drying in vacuum at 80 ℃ for 4 hours to obtain an intermediate product IA.
The dosage ratio of the 2, 6-tetramethyl-4-piperidinol, triethylamine, N-dimethylformamide A, undecylenoyl chloride, N-dimethylformamide B, dichloromethane A, saturated sodium bicarbonate solution A, deionized water A and anhydrous sodium sulfate A is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g.
The infrared data are as follows: 3512cm -1: -OH is absent; 3287cm -1: -NH- (spike) present; 1735cm -1: -c=o present; 1622cm -1: -c=c-present; 703cm -1: C-Cl is absent.
S112, adding 2, 4-dihydroxybenzophenone, potassium carbonate and tertiary butyl hydroquinone into N, N-dimethylformamide C, dissolving 8-bromo-1-octene in N, N-dimethylformamide D, placing in a constant pressure dropping funnel, heating to 120 ℃ and stirring, controlling the temperature to continue to react for 1h after the dropping is finished, and after the reaction is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane B, adding saturated sodium bicarbonate solution B into the solution, washing for 3 times, washing with deionized water B for 3 times, separating, taking organic phase, drying with anhydrous sodium sulfate B, filtering, distilling the filtrate under reduced pressure, and vacuum drying at 80deg.C for 4h to obtain intermediate IB.
The dosage ratio of the 2, 4-dihydroxybenzophenone, the potassium carbonate, the N, N-dimethylformamide C, the 8-bromo-1-octene, the N, N-dimethylformamide D, the methylene dichloride B, the saturated sodium bicarbonate solution B, the deionized water B and the anhydrous sodium sulfate B is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
the dosage of the tertiary butyl hydroquinone is preferably 0.5 percent of the mass of the 8-bromo-1-octene.
The infrared data are as follows: 3501cm -1: -OH present and reduced; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1621cm -1: -c=c-present; 647cm -1: -C-Br is absent.
S12, adding an alkene monomer A, an intermediate product I and an initiator AIBN into N, N-dimethylformamide E, heating to 75 ℃, and stirring for 10 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain an intermediate product II #PDI＝1.64)。
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 8.5mol:1.5mol:800mL.
The vinyl monomer A is amino vinyl, hydroxyethyl methacrylate and ethyl methacrylate according to the molar ratio of 5.0:3.0:2.0 addition.
The amino alkene is allylamine and diacetone acrylamide according to the mol ratio of 1.0:3.0 mixing;
the amount of the initiator AIBN is 1.5 percent of the total mass of the vinyl monomer and the intermediate product I.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
S13, adding nano-grade magnesium oxide and a silane coupling agent GX572 into an absolute ethyl alcohol solvent, carrying out ultrasonic oscillation for 0.5h, standing for 2h at room temperature, reacting for 6h at 60 ℃, filtering, taking insoluble matters, and drying for 12h at 40 ℃ to obtain an intermediate product III.
The dosage ratio of the nano-grade magnesium oxide to the silane coupling agent GX572 to the absolute ethyl alcohol solvent is 1g:4.5g:80mL.
The infrared data are as follows: 3440cm -1: -OH weakening; 1735cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-present; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
S14, adding the intermediate product II and the intermediate product III into N, N-dimethylformamide F, heating to 60 ℃, stirring for 3 hours, distilling under reduced pressure, and drying in a vacuum oven at 40 ℃ for 12 hours to obtain the target product.
The dosage ratio of the intermediate II to the intermediate III to the N, N-dimethylformamide F is 10g:2.0g:400mL.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present and abated; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-absent; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
A method of preparing a tackifying resin comprising the steps of:
S21, adding an alkene monomer B and an initiator AIBN into N, N-dimethylformamide G, heating to 75 ℃, and stirring for 10 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain a target product @ PDI＝1.62)。
The vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 5.0:2.0:1.0:1.0:1.0 addition.
The amount of the initiator AIBN is 1.5 percent of the total mass of the vinyl monomer.
The infrared data are as follows: 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 2258cm -1: cyano groups are present; 1735cm -1: -c=o present; 1218cm -1、911cm-1、835cm-1: the epoxy group is present; 1109cm -1、801cm-1: -Si-O-presence; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
Example 3
Otherwise, the embodiment 1 is different in that:
A preparation method of a functional auxiliary agent comprises the following steps:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
the hydroxyl-containing structural material is a material containing hydroxyl and having a light stable structure; and
The substance containing hydroxyl and having a light stable structure is added with 2, 4-dihydroxybenzophenone and 2, 6-tetramethyl-4-piperidinol according to a molar ratio of 2.0:1.0.
S11 includes S111 and S112,
S111, adding 2, 6-tetramethyl-4-piperidinol and triethylamine into N, N-dimethylacetamide A, dissolving undecylenoyl chloride into N, N-dimethylformamide B, placing into a constant pressure dropping funnel, ice-bath, stirring, controlling the temperature at 0 ℃ to continue to react for 14h after the dropping is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane A, adding saturated sodium bicarbonate solution A into the solution, washing for 3 times, washing with deionized water A for 3 times, separating, taking an organic phase, drying with anhydrous sodium sulfate A, filtering, distilling the filtrate under reduced pressure, and drying in vacuum at 80 ℃ for 4 hours to obtain an intermediate product IA.
The dosage ratio of the 2, 6-tetramethyl-4-piperidinol, triethylamine, N-dimethylformamide A, undecylenoyl chloride, N-dimethylformamide B, dichloromethane A, saturated sodium bicarbonate solution A, deionized water A and anhydrous sodium sulfate A is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g.
The infrared data are as follows: 3512cm -1: -OH is absent; 3287cm -1: -NH- (spike) present; 1735cm -1: -c=o present; 1622cm -1: -c=c-present; 703cm -1: C-Cl is absent.
S112, adding 2, 4-dihydroxybenzophenone, potassium carbonate and tertiary butyl hydroquinone into N, N-dimethylformamide C, dissolving 8-bromo-1-octene in N, N-dimethylformamide D, placing in a constant pressure dropping funnel, heating to 100 ℃ and stirring, controlling the temperature to continue to react for 2 hours after the dropping is finished, and after the reaction is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane B, adding saturated sodium bicarbonate solution B into the solution, washing for 3 times, washing with deionized water B for 3 times, separating, taking organic phase, drying with anhydrous sodium sulfate B, filtering, distilling the filtrate under reduced pressure, and vacuum drying at 80deg.C for 4h to obtain intermediate IB.
The dosage ratio of the 2, 4-dihydroxybenzophenone, the potassium carbonate, the N, N-dimethylformamide C, the 8-bromo-1-octene, the N, N-dimethylformamide D, the methylene dichloride B, the saturated sodium bicarbonate solution B, the deionized water B and the anhydrous sodium sulfate B is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
the dosage of the tertiary butyl hydroquinone is preferably 0.5 percent of the mass of the 8-bromo-1-octene.
The infrared data are as follows: 3501cm -1: -OH present and reduced; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1621cm -1: -c=c-present; 647cm -1: -C-Br is absent.
S12, adding an alkene monomer A, an intermediate product I and an initiator AIBN into N, N-dimethylformamide E, heating to 85 ℃, and stirring for 6 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain an intermediate product II #PDI＝1.67)。
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 8.5mol:1.5mol:800mL.
The vinyl monomer A is amino vinyl, hydroxy vinyl and ethyl methacrylate according to the molar ratio of 5.0:3.0:2.0 addition.
The amino alkene is allylamine and diacetone acrylamide according to the mol ratio of 1.0:3.0 mixing;
the hydroxy alkene is 8-nonen-1-alcohol and hydroxyethyl methacrylate according to the mol ratio of 1.0:1.0 mixing;
the amount of the initiator AIBN is 1.0 percent of the total mass of the vinyl monomer and the intermediate product I.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
S13, adding nano-grade magnesium oxide and a silane coupling agent GX572 into an absolute ethyl alcohol solvent, carrying out ultrasonic oscillation for 0.5h, standing for 2h at room temperature, reacting for 8h at 50 ℃, filtering, taking insoluble matters, and drying for 12h at 40 ℃ to obtain an intermediate product III.
The dosage ratio of the nano-grade magnesium oxide to the silane coupling agent GX572 to the absolute ethyl alcohol solvent is 1g:4.5g:80mL.
The infrared data are as follows: 3440cm -1: -OH weakening; 1735cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-present; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
S14, adding the intermediate product II and the intermediate product III into N, N-dimethylformamide F, heating to 50 ℃, stirring for 4 hours, distilling under reduced pressure, and drying in a vacuum oven at 40 ℃ for 12 hours to obtain the target product.
The dosage ratio of the intermediate II to the intermediate III to the N, N-dimethylformamide F is 10g:3.0g:400mL.
The infrared data are as follows: 3250-3550cm -1: -OH, -NH-present and abated; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1650-1750cm -1: -c=o present; 1605cm -1、811cm-1: -c=c-absent; 1109cm -1、801cm-1: -Si-O-presence; 621cm -1: mg-O-is present.
A method of preparing a tackifying resin comprising the steps of:
s21, adding an alkene monomer B and an initiator AIBN into N, N-dimethylformamide G, heating to 85 ℃, and stirring for 6 hours; after the reaction is finished, cooling to room temperature, filtering, taking filtrate, distilling under reduced pressure, and vacuum drying at 60 ℃ for 6 hours to obtain a target product @ PDI＝1.62)。
The vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 4.0:1.0:2.0:2.0:1.0 addition.
The amount of the initiator AIBN is 1.0 percent of the total mass of the vinyl monomer.
The infrared data are as follows: 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 2258cm -1: cyano groups are present; 1735cm -1: -c=o present; 1218cm -1、911cm-1、835cm-1: the epoxy group is present; 1109cm -1、801cm-1: -Si-O-presence; 1622cm -1、1605cm-1、810cm-1: -c=c-is absent.
Example 4
Otherwise, the embodiment 1 is different in that:
in the step S11,
The substance containing hydroxyl and having a light stable structure is added by the molar ratio of 2, 4-dihydroxybenzophenone to 2, 6-tetramethyl-4-piperidinol of 1.0:1.0.
Example 5
Otherwise, the embodiment 1 is different in that:
in the step S11,
The substance containing hydroxyl and having a light stable structure is added with 2, 4-dihydroxybenzophenone and 2, 6-tetramethyl-4-piperidinol according to a molar ratio of 3.0:1.0.
Example 6
Otherwise, the embodiment 1 is different in that:
A preparation method of a functional auxiliary agent comprises the step S11,
S11 is specifically S111,
S111, adding a hydroxyl-containing structural substance A and triethylamine into N, N-dimethylacetamide A, dissolving undecylenoyl chloride into N, N-dimethylformamide B, placing the mixture into a constant-pressure dropping funnel, carrying out ice bath, stirring, controlling the temperature at 0 ℃ after the dropping is finished, and continuously reacting for 10 hours after the reaction is finished; filtering, distilling under reduced pressure, dissolving the concentrate in dichloromethane A, adding saturated sodium bicarbonate solution A into the solution, washing for 3 times, washing with deionized water A for 3 times, separating, taking an organic phase, drying with anhydrous sodium sulfate A, filtering, distilling the filtrate under reduced pressure, and drying in vacuum at 80 ℃ for 4 hours to obtain an intermediate product IA.
The dosage ratio of the hydroxyl-containing structural substances A, triethylamine, N-dimethylformamide A, undecylenoyl chloride, N-dimethylformamide B, methylene dichloride A, saturated sodium bicarbonate solution A, deionized water A and anhydrous sodium sulfate A is as follows: 1mol:1.0mol:400mL:1mol:150mL:500mL:400mL:400mL:50g;
The hydroxyl-containing structural substance A is a substance containing hydroxyl and having a light stable structure; and
The substance containing hydroxyl and having a light stable structure is added with 2, 4-dihydroxybenzophenone and 2, 6-tetramethyl-4-piperidinol according to a molar ratio of 2.0:1.0.
The infrared data are as follows: 3501cm -1: -OH present and reduced; 3287cm -1: -NH- (spike) present; 3013cm -1: benzene ring-C-H is present; 1495cm -1、1597cm-1: the benzene ring exists; 1735cm -1: -c=o present; 1622cm -1: -c=c-present; 703cm -1: C-Cl is absent.
Example 7
Otherwise, the embodiment 1 is different in that:
in the step S12,
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 8.0mol:2.0mol:800mL.
Example 8
Otherwise, the embodiment 1 is different in that:
in the step S12,
The dosage ratio of the vinyl monomer A to the intermediate I, N to the N-dimethylformamide E is 9.5mol:0.5mol:800mL.
Example 9
Otherwise, the embodiment 1 is different in that:
in the step S12,
The vinyl monomer A is amino vinyl, 8-nonen-1-alcohol and ethyl methacrylate according to the mol ratio of 6.0:2.0:2.0 addition.
Example 10
Otherwise, the embodiment 1 is different in that:
in the step S12,
The vinyl monomer A is amino vinyl, 8-nonen-1-alcohol and ethyl methacrylate according to the mol ratio of 4.0:4.0:2.0 addition.
Example 11
Otherwise, the embodiment 1 is different in that:
in the step S12,
The amino alkene is allylamine and diacetone acrylamide according to the mol ratio of 1.0:2.0 mixing.
Example 12
Otherwise, the embodiment 1 is different in that:
in the step S12,
The amino alkene is allylamine and diacetone acrylamide according to the mol ratio of 1.0: 4.0.
Example 13
Otherwise, the embodiment 1 is different in that:
in the step S13,
The dosage ratio of the nano-grade magnesium oxide to the silane coupling agent GX572 to the absolute ethyl alcohol solvent is 1g:3.5g:80mL.
Example 14
Otherwise, the embodiment 1 is different in that:
in the step S13,
The dosage ratio of the nano-grade magnesium oxide to the silane coupling agent GX572 to the absolute ethyl alcohol solvent is 1g:5.5g:80mL.
Example 15
Otherwise, the embodiment 1 is different in that:
in the step S13,
The silane coupling agent GX572 was replaced with a silane coupling agent KH560.
Example 16
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
0.8 parts of cross-linking agent;
1.5 parts of auxiliary cross-linking agent;
4.0 parts of functional auxiliary agent;
0.2 parts of antioxidant;
0.3 part of silane coupling agent KH 171;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
15 parts of PP resin;
12 parts of adhesive resin;
0.5 parts of cross-linking agent;
1.5 parts of auxiliary cross-linking agent;
0.2 parts of antioxidant;
0.15 part of light stabilizer.
Example 17
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
1.2 parts of cross-linking agent;
1.0 parts of auxiliary cross-linking agent;
6.0 parts of functional auxiliary agent;
0.1 part of antioxidant;
0.5 part of silane coupling agent KH 171;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
10 parts of PP resin;
8 parts of adhesive resin;
1.0 part of cross-linking agent;
1.0 parts of auxiliary cross-linking agent;
0.05 parts of antioxidant;
0.05 part of light stabilizer.
Example 18
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
1.0 part of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
4.0 parts of functional auxiliary agent;
0.15 parts of antioxidant;
0.4 part of silane coupling agent KH 171;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
13 parts of PP resin;
12 parts of adhesive resin;
0.8 parts of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
0.14 parts of antioxidant;
0.10 parts of light stabilizer.
Example 19
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
1.0 part of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
6.0 parts of functional auxiliary agent;
0.15 parts of antioxidant;
0.4 part of silane coupling agent KH 171;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
13 parts of PP resin;
8 parts of adhesive resin;
0.8 parts of cross-linking agent;
1.2 parts of auxiliary cross-linking agent;
0.14 parts of antioxidant;
0.10 parts of light stabilizer.
The following examples are comparative to example 1 for a composite packaging film for a no-main-grid battery module:
comparative example 1
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
Functional auxiliary agents are not added into the EVA layer raw materials; and is also provided with
And no adhesive resin is added into the POE layer raw material.
Comparative example 2
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
Functional auxiliary agents are not added in the EVA layer raw materials.
Comparative example 3
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
And no adhesive resin is added into the POE layer raw material.
Comparative example 4
Otherwise, the embodiment 1 is different in that:
in the preparation method of the functional auxiliary agent, the intermediate product I is not prepared and added.
Comparative example 5
Otherwise, the embodiment 1 is different in that:
in the preparation method of the functional auxiliary agent, the substance which contains hydroxyl and has a light stable structure in the S11 is 2, 4-dihydroxybenzophenone.
Comparative example 6
Otherwise, the embodiment 1 is different in that:
In the preparation method of the functional auxiliary agent, the substance which contains hydroxyl and has a light stable structure in the S11 is 2, 6-tetramethyl-4-piperidinol.
Comparative example 7
Otherwise, the embodiment 1 is different in that:
a preparation method of a functional auxiliary agent comprises the steps that in S12, an alkene monomer A is amino alkene and styrene according to a molar ratio of 5.0:5.0 addition.
Comparative example 8
Otherwise, the embodiment 1 is different in that:
the functional auxiliary is the same as intermediate II in example 1.
Comparative example 9
Otherwise, the embodiment 1 is different in that:
A preparation method of a functional auxiliary agent replaces the magnesium oxide with silicon dioxide.
Comparative example 10
Otherwise, the embodiment 1 is different in that:
In the preparation method of the adhesive resin, the vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 0:1.5:1.5:2.0:1.0, i.e. no allyl glycidyl ether was added.
Comparative example 11
Otherwise, the embodiment 1 is different in that:
In the preparation method of the adhesive resin, the vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 4.0:1.5:1.5:0:1.0, i.e. no acrylonitrile was added.
Comparative example 12
Otherwise, the embodiment 1 is different in that:
In the preparation method of the adhesive resin, the vinyl monomer B is allyl glycidyl ether, isooctyl methacrylate, styrene, acrylonitrile and KH570 according to the mol ratio of 4.0:1.5:1.5:2.0:0, i.e. no KH570 was added.
Comparative example 13
Otherwise, the embodiment 1 is different in that:
A composite packaging adhesive film for a battery component without a main grid comprises an EVA layer and a POE layer,
PP resin is not added into the POE layer raw material.
Comparative example 14
Otherwise, the embodiment 1 is different in that:
a packaging adhesive film for a battery component without a main grid is an EVA adhesive film.
Comparative example 15
Otherwise, the embodiment 1 is different in that:
A packaging adhesive film for a battery assembly without a main grid is POE adhesive film.
The physical properties of the adhesive films prepared in examples 1 to 19 and comparative examples 1 to 15 of the present invention were measured, respectively, and the results are shown in Table 1.
Table 1 physical test performance of various examples
First, as can be seen from examples 1 to 19 of table 1, the composite packaging adhesive film for a no-main-grid battery module of the present invention has excellent adhesion, aging resistance, moisture barrier property, low shrinkage (EL display after lamination has no cold joint, displacement phenomenon) and the like.
Second, as can be seen from example 1 and comparative examples 1 to 3, the use of self-made functional aids and self-made adhesive resins for the composite packaging film of the present invention has an important effect on adhesion, aging resistance and low shrinkage. From example 1 and comparative examples 4 to 6, it can be observed that the self-made functional auxiliary agent is used in the composite packaging adhesive film, so that the composite packaging adhesive film has excellent ageing resistance, and the effect of the o-hydroxybenzophenone structure and the hindered amine structure is better under a proper proportion. From example 1 and comparative example 7, it can be observed that the hydroxyl and ester group structures in the self-made functional auxiliary agent help to promote the dispersion in EVA, inhibit EVA hydrolysis and reduce oxidation corrosion. As can be seen from example 1 and comparative examples 8 to 9, the inorganic substance is advantageous in reducing the shrinkage, while the metal oxide has a superior resistance to acid gas corrosion. It can be seen from examples 10-12 that the homemade adhesive resin epoxy, cyano has greater adhesion to EVA, while the silane coupling agent has greater adhesion to the battery tab. From examples 13-15, it can be observed that the PP resin has higher melting temperature, and the hot-pressing support property of the POE layer and even the composite adhesive film is better at the same temperature; the use of a separate EVA layer has the problems of poor water resistance and high shrinkage to form cold joint and displacement; the use of a separate POE layer has the problem of poor adhesion.
In summary, according to the composite packaging adhesive film for the main gate-free battery assembly, the EVA layer is compounded with the POE layer, the EVA layer provides adhesion, and the POE layer provides water resistance and weather resistance and low shrinkage rate; and the self-made functional auxiliary agent and the adhesive resin cooperate to effectively improve the comprehensive performance of the composite material.
The test method comprises the following steps:
(1) Peel force: sequentially stacking a battery piece, a composite packaging adhesive film (POE layer is attached to the battery piece, EVA layer is attached to the glass piece) and the glass piece, performing hot-pressing compounding at 145 ℃, and then providing a testing method for testing by referring to GB/T29848-2018; the assembly was conditioned on: test conditions: the above operations were repeated after DH2000h at +85℃, relative humidity 85℃.
(2) EL (electroluminescence) test after lamination: the test was performed with reference to the test method provided by IEC 61215, to test whether or not the EL had a cold joint or displacement after lamination (lamination of POE layer to battery sheet, lamination of EVA layer to glass sheet).
(3) Component laminate appearance: and sequentially stacking the composite packaging adhesive film, the cell array without the main grid and the composite packaging adhesive film to obtain a photovoltaic module, vacuumizing at 145 ℃ for 5min, laminating for 10min, and observing the appearance of the laminated cell module to see whether the cell is hidden to crack and whether delamination white spots exist.
(4) Water vapor transmission rate: the water vapor transmittance is measured by an infrared sensor method according to the standard GB/T21529-2008 by adopting a model C390H water vapor transmittance tester, and the test condition is 38 ℃ and 90% relative humidity.
(5) Ultraviolet aging resistance: and carrying out ultraviolet irradiation aging test on the obtained composite packaging adhesive film according to the requirements specified by International electrotechnical Commission standard IEC 61345. Test conditions: the surface temperature of the test piece is 60+/-5 ℃, the ultraviolet wavelength range is 280-400nm, the irradiation intensity is 15 kW.h/m 2, and the ultraviolet irradiation test time is 2000hr.
The visible light transmittance before and after the test was measured, and the retention rate of the visible light transmittance was calculated as follows:
retention of visible light transmittance = average light transmittance after test/average light transmittance before test x 100%.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (13)
1. The preparation method of the functional auxiliary agent is characterized by comprising the following steps of:
S11, carrying out substitution reaction on a hydroxyl-containing structural substance and halogenated alkene to obtain an intermediate product I;
S12, carrying out polymerization reaction on the vinyl monomer A and the intermediate product I under the action of an initiator A to obtain an intermediate product II;
S13, placing the nanoscale metal oxide and a silane coupling agent in an alcohol solvent for a coupling reaction to obtain an intermediate product III;
S14, performing coupling reaction on the intermediate product II and the intermediate product III to obtain a target product.
2. The method according to claim 1, wherein,
The hydroxyl-containing structural material is a material containing hydroxyl and having a light stable structure; and
The usage ratio of the hydroxyl-containing structural material to the halogenated alkene is 1:1.
3. The method according to claim 2, wherein,
The substance containing hydroxyl and having a light stable structure is added by the molar ratio of o-hydroxybenzophenone and hindered amine of 1.0-3.0:1.0.
4. The method according to claim 1, wherein,
The vinyl monomer A is amino vinyl, hydroxy vinyl and ester vinyl, and the vinyl monomer A is added according to the molar ratio of 4.0-6.0:2.0-4.0:2.0-4.0; and
The amino alkene is that alkenyl amine and alkenyl amide are mixed according to a mol ratio of 1.0:2.0-4.0.
5. The method according to claim 1, wherein,
The dosage ratio of the vinyl monomer A to the intermediate product I is 8.0-9.5mol:0.5-2.0mol.
6. The method according to claim 1, wherein,
The dosage of the metal oxide, the silane coupling agent and the alcohol solvent is 1g:3.3-5.5g:80mL.
7. The method according to claim 1, wherein,
The dosage ratio of the intermediate product II to the intermediate product III is 10g:2.0-3.0g.
8. A functional auxiliary agent prepared by the preparation method of any one of claims 1 to 7.
9. A method for preparing an adhesive resin, comprising the steps of:
S21, carrying out polymerization reaction on the vinyl monomer B under the action of an initiator B to obtain a target product.
10. The method according to claim 9, wherein,
The vinyl monomer B is epoxy vinyl, ester vinyl, styrene, acrylonitrile and silane vinyl according to the mol ratio of 4.0-5.0:1.0-2.0:1.0-2.0:1.0-2.0:1.0 addition.
11. A tacky resin produced by the production method of claim 9 or 10.
12. A composite packaging adhesive film for a battery component without a main grid is characterized by comprising an EVA layer and a POE layer,
The EVA layer comprises the following raw materials in parts by weight:
100 parts of EVA resin;
0.8-1.2 parts of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
4.0-6.0 parts of functional auxiliary agent;
0.1-0.2 part of antioxidant;
0.3-0.5 part of silane coupling agent;
the POE layer comprises the following raw materials in parts by weight:
100 parts of POE resin;
10-15 parts of PP resin;
8-12 parts of adhesive resin;
0.5-1.0 part of cross-linking agent;
1.0-1.5 parts of auxiliary cross-linking agent;
0.05-0.20 part of antioxidant;
0.05-0.15 part of light stabilizer.
13. The preparation method of the composite packaging adhesive film for the main-grid-free battery assembly is characterized by comprising the following steps of:
S31, mixing, i.e
Mixing and configuring the raw materials of each layer in a mixer according to a formula to obtain mixed raw materials for later use;
s32, co-extrusion, i.e
Respectively placing the mixed raw materials in the step S31 into an extruder, and carrying out melt blending, coextrusion, casting, traction, stretching and cooling; and
S33, film formation, i.e
And (3) performing thickness measurement, edge pressing, shaping, trimming and rolling to obtain the composite packaging adhesive film for the battery component without the main grid.
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