CN116333409A - 一种具有高抗pid性能的poe复合膜及其制备方法 - Google Patents
一种具有高抗pid性能的poe复合膜及其制备方法 Download PDFInfo
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- CN116333409A CN116333409A CN202310370840.6A CN202310370840A CN116333409A CN 116333409 A CN116333409 A CN 116333409A CN 202310370840 A CN202310370840 A CN 202310370840A CN 116333409 A CN116333409 A CN 116333409A
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- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000012528 membrane Substances 0.000 title claims description 20
- 238000002360 preparation method Methods 0.000 title description 7
- 238000004132 cross linking Methods 0.000 claims abstract description 29
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 26
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 20
- 229910018557 Si O Inorganic materials 0.000 claims abstract description 19
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- AGKBXKFWMQLFGZ-UHFFFAOYSA-N (4-methylbenzoyl) 4-methylbenzenecarboperoxoate Chemical group C1=CC(C)=CC=C1C(=O)OOC(=O)C1=CC=C(C)C=C1 AGKBXKFWMQLFGZ-UHFFFAOYSA-N 0.000 claims description 10
- DTTYYQJHSSBLQJ-UHFFFAOYSA-N N=C=N.C(C)(C)C1=CC(=CC=C1)C(C)C.C(C)(C)C1=CC(=CC=C1)C(C)C Chemical compound N=C=N.C(C)(C)C1=CC(=CC=C1)C(C)C.C(C)(C)C1=CC(=CC=C1)C(C)C DTTYYQJHSSBLQJ-UHFFFAOYSA-N 0.000 claims description 10
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- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
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- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 8
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- 239000000155 melt Substances 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
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- 230000002195 synergetic effect Effects 0.000 abstract description 3
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- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 6
- 150000002978 peroxides Chemical class 0.000 description 6
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- 238000009740 moulding (composite fabrication) Methods 0.000 description 3
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- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 2
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- HSNHLHNSJCYPNU-UHFFFAOYSA-N o-propan-2-yl propan-2-ylsulfanylmethanethioate Chemical compound CC(C)OC(=S)SC(C)C HSNHLHNSJCYPNU-UHFFFAOYSA-N 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- MYOQALXKVOJACM-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy pentaneperoxoate Chemical compound CCCCC(=O)OOOC(C)(C)C MYOQALXKVOJACM-UHFFFAOYSA-N 0.000 description 1
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- 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 1
- BDNKZNFMNDZQMI-UHFFFAOYSA-N 1,3-diisopropylcarbodiimide Chemical compound CC(C)N=C=NC(C)C BDNKZNFMNDZQMI-UHFFFAOYSA-N 0.000 description 1
- FIYMNUNPPYABMU-UHFFFAOYSA-N 2-benzyl-5-chloro-1h-indole Chemical compound C=1C2=CC(Cl)=CC=C2NC=1CC1=CC=CC=C1 FIYMNUNPPYABMU-UHFFFAOYSA-N 0.000 description 1
- BIISIZOQPWZPPS-UHFFFAOYSA-N 2-tert-butylperoxypropan-2-ylbenzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1 BIISIZOQPWZPPS-UHFFFAOYSA-N 0.000 description 1
- SBVKVAIECGDBTC-UHFFFAOYSA-N 4-hydroxy-2-methylidenebutanamide Chemical compound NC(=O)C(=C)CCO SBVKVAIECGDBTC-UHFFFAOYSA-N 0.000 description 1
- GBISYXPXYCCKJU-UHFFFAOYSA-N C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.OCCNCC Chemical compound C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.OCCNCC GBISYXPXYCCKJU-UHFFFAOYSA-N 0.000 description 1
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 1
- 229940120146 EDTMP Drugs 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- WLLGXSLBOPFWQV-UHFFFAOYSA-N MGK 264 Chemical compound C1=CC2CC1C1C2C(=O)N(CC(CC)CCCC)C1=O WLLGXSLBOPFWQV-UHFFFAOYSA-N 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 1
- -1 N-dimethylacrylamide Chemical compound 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 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
- 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 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
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- BGRWYRAHAFMIBJ-UHFFFAOYSA-N diisopropylcarbodiimide Natural products CC(C)NC(=O)NC(C)C BGRWYRAHAFMIBJ-UHFFFAOYSA-N 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- BHBPJIPGXGQMTE-UHFFFAOYSA-N ethane-1,2-diol;2-methylprop-2-enoic acid Chemical compound OCCO.CC(=C)C(O)=O.CC(=C)C(O)=O BHBPJIPGXGQMTE-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal 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
- 238000013508 migration Methods 0.000 description 1
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- 238000007719 peel strength test Methods 0.000 description 1
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/22—Cellulose xanthate
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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Abstract
本申请提供了一种高抗PID性能的POE复合膜,按重量份计,其原料包括:POE树脂95‑100份,乙烯‑醋酸乙烯酯共聚物15‑30份、含有Si‑O键的C5‑C12饱和直链有机物15‑25份,PID调节剂0.3‑3份、交联剂0.1‑5.0份;通过各组分的协同作用,本申请的POE复合膜体系具有优异的透明度、交联程度、抗PID性能、力学强度和加工性能等,可用于双玻组件的封装中。
Description
技术领域
本发明涉及封装材料技术领域,尤其涉及一种具有高抗PID性能的POE复合膜及其制备方法。
背景技术
光伏封装胶膜是光伏组件的重要封装材料,其直接影响后者的电气性能;目前的光伏封装胶膜主要是EVA胶膜和POE胶膜;EVA胶膜透明度高、工艺成熟,但是其水汽透过率大,耐候性能差,应用EVA胶膜的双玻组件在后期会出现电气性能显著下降的问题;POE为乙烯-辛烯共聚物,具有饱和脂肪链结构并拥有较多短支链,分子链中不含有活泼极性基团,结晶度低,与EVA胶膜相比,在透光率指标上二者相当,而在水汽阻隔率、体积电阻率、耐紫外老化等性能指标上POE胶膜具有明显优势,因而是光伏组件封装胶膜的一种理想基体材料。
但是市场中的的POE胶膜仍然面临着一些致命缺点:如交联度偏低,在高温高湿条件下剥离力衰减大等,都会明显缩短POE胶膜的寿命,并降低双玻组件的性能。因此开发一种交联度高、在高温高湿条件下剥离力衰减小的POE胶膜在行业应用中具有非常重要的意义。
中国专利CN106281122B公开了一种POE封装胶膜用复合交联剂,利用高活性过氧化物、低活性过氧化物和交联协效剂的协同作用提高POE复合膜的交联程度,但是其技术方案中采用的过氧化物含量太多,仍然存在高温高湿下被分解的风险。中国专利CN106129152B公开了一种光伏组件封装用POE复合背面材料,其透明POE复合膜由95%的POE树脂和5%的改性添加剂组成,其只采用过氧化物交联剂提升POE复合膜的交联程度,交联程度仍然不够,也无法进一步解决水汽透过后引起的电势衰减现象。
发明内容
为了解决上述技术问题,本发明首先提供了一种具有高抗PID性能的POE复合膜。
进一步地,所述高抗PID性能的POE复合膜,按重量份计,其原料包括:POE树脂95-100份,乙烯-醋酸乙烯酯共聚物15-30份、含有Si-O键的C5-C12饱和直链有机物15-25份,PID调节剂0.3-3份、交联剂0.1-5.0份。
进一步地,所述POE树脂选自乙烯-α-丁烯共聚树脂、乙烯-α-己烯共聚树脂、乙烯-α-辛烯共聚树脂、乙烯-α-丙烯共聚树脂中的一种或几种的组合。
在一种优选的实施方式中,所述POE树脂为乙烯-α-辛烯共聚树脂,包括但不限于POE8210、POE8400、POE8401、POE8402、POE8407、POE8411中的至少一种。
优选地,所述POE树脂中辛烯的摩尔含量为25-50%,190℃、2.16kg下的熔融指数为15-25g/10min。POE树脂中辛烯的摩尔含量和其熔融指数明显影响POE复合膜的耐老化性能和体系的加工性能,分析原因为:POE树脂中的辛烯链段增加了POE的分子链柔性,但是当辛烯含量过多时,POE树脂中长支链部分的增加会在空间上抑制含有Si-O键的C5-C12饱和直链有机物的接枝程度,并且这种空间阻碍作用也会抑制POE复合膜原料体系在熔融过程中的交联,而部分辛烯链在后期UV过程中的断裂增加,降低POE树脂的光稳定性,也影响体系后期的光致交联程度;另一方面,当辛烯含量少于25%时,树脂链中的结晶乙烯量增加,在交联不充分时,POE复合膜的光透过率降低。
进一步地,所述乙烯-醋酸乙烯酯共聚物中VA质量含量为15-35%,熔融指数为10-45g/10min,包括但不限于Nipoflex633、Nipoflex710、Nipoflex750、Sumitate KA-10、Evflex150、Evflex450、Evatane 28-25、Evatane 33-25中的至少一种。
进一步地,所述乙烯-醋酸乙烯酯共聚物中VA质量含量为20-25%,熔融指数为10-35g/10min。
进一步地,所述含有Si-O键的C5-C12饱和直链有机物为含有Si-O键的C5-C12饱和直链烷烃和/或其有机盐。本申请发现使用含有Si-O键的C5-C12饱和直链有机物可提高POE复合膜的交联程度、剥离强度和疏水性;分析原因为:POE分子链和EVA分子链与含有Si-O键的C5-C12饱和直链有机物在熔融状态下产生接枝,而后烷氧基水解产生羟基并发生硅醇脱水形成Si-O-Si键而使体系中的POE和乙烯-醋酸乙烯酯共聚物产生交联,由于四个Si-O键形成的特殊立体结构,POE交联后会由原来的线形转变为三维立体网络状,乙烯-醋酸乙烯酯共聚物的交联则进一步增大,这种体系高程度的交联进一步提高了POE复合膜的耐湿热性和剥离强度。
进一步地,所述含有Si-O键的C5-C12饱和直链有机物选自3-三乙氧基甲硅烷基-1-丙胺、3-缩水甘油醚氧基丙基三甲氧基硅烷、3-巯丙基三甲氧基硅烷、N-氨乙基-3-氨丙基甲基二甲氧基硅烷、n-(β-氨乙基)-γ-氨丙基三乙氧基硅烷中的一种或几种的组合。
在一种优选的实施方式中,所述含有Si-O键的C5-C12饱和直链有机物为3-缩水甘油醚氧基丙基三甲氧基硅烷。
进一步地,所述含有Si-O键的C5-C12饱和直链有机物用量为POE树脂和乙烯-醋酸乙烯酯共聚物总量的10-20wt.%;含有Si-O键的C5-C12饱和直链有机物可平衡体系的刚柔性,有利于膜的加工过程,但是当其含量过多时,因其结构的空间阻碍性,无法继续对POE树脂进行接枝,对双玻组件的粘结强度改变非常小,体系中未被交联的含有Si-O键的C5-C12直链有机物将以游离态存在,其亲水基团可能会加剧水分子在体系中的穿透,因此控制其用量,抑制体系对水分子的吸引。
进一步地,所述PID调节剂选自纤维素黄原酸酯、二硫化二异丙基黄原酸酯、甲基丙烯酸羟乙酯、二(甲基丙烯酸)乙二醇酯、乙二胺四亚甲基膦酸、氨基三亚甲基膦酸、羟基乙叉二膦酸、二乙撑三胺五乙酸、N一羟乙基乙胺三乙酸、马来酸、季戊四醇、聚碳化二亚胺、单碳化二亚胺、双碳化二亚胺中的一种或几种的组合。
进一步地,所述PID调节剂选自纤维素黄原酸酯、二硫化二异丙基黄原酸酯、二环己基碳二亚胺、二异丙基碳化二亚胺、双(2,6-二异丙基苯)碳二亚胺中的一种或几种的组合。
在一种优选的实施方式中,所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺的组合,质量比为1:(1-5);本申请采用双(2,6-二异丙基苯)碳二亚胺抑制乙烯-醋酸乙烯酯共聚物的水解,并进一步使用纤维素黄原酸酯抑制乙烯-醋酸乙烯酯共聚物离解后与金属钠离子的结合,避免钠离子在内部的迁移造成的电势衰减现象,但是两者存在的极性基团和共轭结构可与乙烯-醋酸乙烯酯共聚物产生分子间作用力,并增加POE膜与双玻组件的粘结性能,但两者中的极性基团存在氧化降解风险,会降低POE膜的长期稳定性。
进一步地,所述纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺的质量比为1:(1-3)。
进一步地,所述交联剂选自季戊四醇三丙烯酸酯、二(4-甲基苯甲酰)过氧化物、丁基-4,4’-二(叔丁基过氧化)戊酸酯、丙氧基化新戊二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、三烯丙基异氰脲酸酯、2-甲基-2-亚硝基甲烷、N,N’-亚甲基双丙烯酰胺、羟甲基丙烯酰胺、羟乙基丙烯酰胺、N,N-二甲基丙烯酰胺、叔丁基过氧化异丙苯、叔丁基过氧化2-乙基已基碳酸酯、1,1-二叔丁基过氧化环己烷中的至少一种。
进一步地,所述交联剂为二(4-甲基苯甲酰)过氧化物和/或三羟甲基丙烷三甲基丙烯酸酯。
在一种优选的实施方式中,当所述交联剂为二(4-甲基苯甲酰)过氧化物和三羟甲基丙烷三甲基丙烯酸酯的组合,质量比为(2-5):(1-3)时,POE复合膜的高温高湿剥离力衰减更小;推测原因为:二(4-甲基苯甲酰)过氧化物在高温条件下分解成高活性的游离自由基,这些自由基会使POE树脂和乙烯-醋酸乙烯酯共聚物上的不活泼C形成新的C-C键而产生分子的交联,POE树脂中结晶的乙烯链节减少,可提高POE复合膜的光透过率,以上交联可在POE复合膜原料的熔融挤出过程中实现,进行初步的交联,但当其过氧化物的含量过多时,二(4-甲基苯甲酰)过氧化物自身的游离基与C游离基结合的可能性增大,体系中酯键含量的增多反而会导致在高温条件下POE复合膜内部分子链的断裂,另外熔融过程中过大的交联度也会增大加工过程的难度;因此,本申请在控制初步交联后,通过使用三羟甲基丙烷三甲基丙烯酸酯,使POE复合膜在制造后再进行UV光下的进一步交联,但本申请发现三羟甲基丙烷三甲基丙烯酸酯含量过多时,后期的UV交联程度太大,分子链的柔性降低,容易发生卷边、翘起等变形现象。
进一步地,所述POE复合膜的原料还可包括但不限于抗紫外助剂、抗氧化剂、光稳定剂、防老化剂、填料等中的一种或多种。
进一步地,所述抗紫外助剂包括但不限于醇酯类、亚磷酸酯类、三嗪类、苯酮类中的至少一种。
进一步地,所述抗氧化剂包括但不限于胺类、受阻酚类抗氧化剂、磷酸酯类、亚磷酸酯类中的至少一种。
其次,本发明还提供了所述POE复合膜的制备方法,包括以下步骤:
(1)将原料投入40-50℃的恒温搅拌装置中搅拌得到混合物;
(2)使用挤出机将混合物熔融挤出,挤出温度为80-150℃,挤出的熔体经过压花冷却成型、牵引、分切、收卷得到初膜;
(3)将初膜在光强500-2000Mw,波长200-500nm的汞灯或LED灯源下辐照0.2-3min,完成UV交联固化,即得POE复合膜。
优选地,所述步骤(2)中挤出温度为80-110℃。
优选地,所述步骤(3)中光强为800-1300Mw,辐照0.2-1min。
优选地,所述POE复合膜的厚度为0.2-0.5mm。
有益效果:
本申请将POE和EVA复合,进一步调控两者用量,在利用两者优点的同时,还采用含有Si-O键的C5-C12饱和直链有机物以增大体系的交联程度并抑制EVA酯键的离解,结合抗PID助剂在抑制水解和捕捉水解离子的两个层面抑制复合膜的电势衰减现象;另外,本申请还优化交联剂的种类和配比以进一步提高体系交联度,防止水汽的透过。通过各组分的协同作用,本申请的POE复合膜体系具有优异的透明度、交联程度、抗PID性能、力学强度和加工性能等,可用于双玻组件的封装中。
具体实施方式
实施例
实施例1
本实施例提供了一种具有高抗PID性能的POE复合膜,按重量份计,其原料包括:POE树脂(POE8411,陶氏)98份,乙烯-醋酸乙烯酯共聚物(Nipoflex633,日本东曹)25份、3-缩水甘油醚氧基丙基三甲氧基硅烷18.5份,PID调节剂1.8份、交联剂3.0份;
所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺,质量比为1:2;所述交联剂为二(4-甲基苯甲酰)过氧化物和三羟甲基丙烷三甲基丙烯酸酯的组合,质量比为3:2;
所述POE复合膜的制备方法为:
(1)将原料投入45℃的恒温搅拌装置中搅拌4h得到混合物;
(2)使用挤出机将混合物熔融挤出,挤出温度为100℃,挤出的熔体经过压花冷却成型、牵引、分切、收卷得到初膜。
(3)将初膜在光强1100Mw,波长380nm的汞灯下辐照0.5min,完成UV交联固化,即得POE复合膜;所述POE复合膜的厚度为0.35mm。
实施例2
本实施例提供了一种具有高抗PID性能的POE复合膜,按重量份计,其原料包括:POE树脂(POE8411,陶氏)95份,乙烯-醋酸乙烯酯共聚物(Nipoflex633,日本东曹)15份、3-缩水甘油醚氧基丙基三甲氧基硅烷22份,PID调节剂0.5份、交联剂5.0份;
所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺,质量比为1:1;所述交联剂为二(4-甲基苯甲酰)过氧化物和三羟甲基丙烷三甲基丙烯酸酯的组合,质量比为5:1;
所述POE复合膜的制备方法为:
(1)将原料投入40℃的恒温搅拌装置中搅拌4h得到混合物;
(2)使用挤出机将混合物熔融挤出,挤出温度为80℃,挤出的熔体经过压花冷却成型、牵引、分切、收卷得到初膜。
(3)将初膜在光强800Mw,波长500nm的汞灯下辐照20s,完成UV交联固化,即得POE复合膜;所述POE复合膜的厚度为0.5mm。
实施例3
本实施例提供了一种具有高抗PID性能的POE复合膜,按重量份计,其原料包括:POE树脂(POE8411,陶氏)100份,乙烯-醋酸乙烯酯共聚物(Nipoflex633,日本东曹)30份、3-缩水甘油醚氧基丙基三甲氧基硅烷15份,PID调节剂3份、交联剂1.5份;
所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺,质量比为1:3;所述交联剂为二(4-甲基苯甲酰)过氧化物和三羟甲基丙烷三甲基丙烯酸酯的组合,质量比为2:3;
所述POE复合膜的制备方法为:
(1)将原料投入50℃的恒温搅拌装置中搅拌5h得到混合物;
(2)使用挤出机将混合物熔融挤出,挤出温度为110℃,挤出的熔体经过压花冷却成型、牵引、分切、收卷得到初膜。
(3)将初膜在光强1300Mw,波长200nm的汞灯下辐照50s,完成UV交联固化,即得POE复合膜;所述POE复合膜的厚度为0.2mm。
实施例4
与实施例1基本一致,区别在于:所述含有Si-O键的C5-C12饱和直链有机物为n-(β-氨乙基)-γ-氨丙基三乙氧基硅烷(CAS:5089-72-5)。
实施例5
与实施例1基本一致,区别在于:所述3-缩水甘油醚氧基丙基三甲氧基硅烷为36份。
实施例6
与实施例1基本一致,区别在于:所述POE树脂为POE8450,陶氏,熔融指数为3.0g/10min。
实施例7
与实施例1基本一致,区别在于:所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺,质量比为1:5。
实施例8
与实施例1基本一致,区别在于:所述交联剂为二(4-甲基苯甲酰)过氧化物。
所述3-缩水甘油醚氧基丙基三甲氧基硅烷购自上海凯赛化工,所述n-(β-氨乙基)-γ-氨丙基三乙氧基硅烷购自科拉曼试剂有限公司,所述双(2,6-二异丙基苯)碳二亚胺购自寅源新材料股份有限公司。
性能测试方法:
1、抗PID性能:将实施例的POE复合膜按照:玻璃/抗PID的POE复合膜/电池片/抗PID的POE复合膜/背板组装并于145℃下抽真空5min,层压15min后进行测试,测试温度为85℃、湿度为85%,施加-1000V电压500小时后,测量其功率的衰减量。
2、剥离强度衰减测试:将POE与玻璃抽真空层压,按照国家标准GB/T2790《胶粘剂180°剥离强度试验方法挠性材料对刚性材料》标准进行剥离强度的测量,再测量DH2000后的剥离强度值,计算衰减量。
性能测试结果:
表1
Claims (10)
1.一种具有高抗PID性能的POE复合膜,其特征在于,按重量份计,其原料包括:POE树脂95-100份,乙烯-醋酸乙烯酯共聚物15-30份、含有Si-O键的C5-C12饱和直链有机物15-25份,PID调节剂0.3-3份、交联剂0.1-5.0份。
2.根据权利要求1所述的POE复合膜,其特征在于,所述POE树脂为乙烯-α-辛烯共聚树脂,190℃、2.16kg下的熔融指数为15-25g/10min。
3.根据权利要求1所述的POE复合膜,其特征在于,所述含有Si-O键的C5-C12饱和直链有机物选自3-三乙氧基甲硅烷基-1-丙胺、3-缩水甘油醚氧基丙基三甲氧基硅烷、3-巯丙基三甲氧基硅烷、N-氨乙基-3-氨丙基甲基二甲氧基硅烷、n-(β-氨乙基)-γ-氨丙基三乙氧基硅烷中的一种或几种的组合。
4.根据权利要求3所述的POE复合膜,其特征在于,所述含有Si-O键的C5-C12饱和直链有机物为3-缩水甘油醚氧基丙基三甲氧基硅烷。
5.根据权利要求4所述的POE复合膜,其特征在于,所述含有Si-O键的C5-C12饱和直链有机物用量为POE树脂和乙烯-醋酸乙烯酯共聚物总量的10-20wt.%。
6.根据权利要求1所述的POE复合膜,其特征在于,所述PID调节剂为纤维素黄原酸酯和双(2,6-二异丙基苯)碳二亚胺的组合。
7.根据权利要求1所述的POE复合膜,其特征在于,所述交联剂为二(4-甲基苯甲酰)过氧化物和/或三羟甲基丙烷三甲基丙烯酸酯。
8.根据权利要求1-7任一项所述的POE复合膜的制备方法,其特征
在于,包括以下步骤:
(1)将原料投入40-50℃的恒温搅拌装置中搅拌得到混合物;
(2)使用挤出机将混合物熔融挤出,挤出温度为80-150℃,挤出的熔体经过压花冷却成型、牵引、分切、收卷得到初膜;
(3)将初膜在光强500-2000Mw,波长200-500nm的汞灯或LED灯源下辐照0.2-3min,完成UV交联固化,即得POE复合膜。
9.根据权利要求8所述的POE复合膜的制备方法,其特征在于,所述步骤(2)中挤出温度为80-110℃。
10.根据权利要求9所述的POE复合膜的制备方法,其特征在于,所述步骤(3)中光强为800-1300Mw,辐照0.2-1min。
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