CN103724785A - 一种低填充无卤膨胀型阻燃光伏封装材料及其制备方法 - Google Patents
一种低填充无卤膨胀型阻燃光伏封装材料及其制备方法 Download PDFInfo
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- CN103724785A CN103724785A CN201310667408.XA CN201310667408A CN103724785A CN 103724785 A CN103724785 A CN 103724785A CN 201310667408 A CN201310667408 A CN 201310667408A CN 103724785 A CN103724785 A CN 103724785A
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- Prior art keywords
- hydroxyl
- butyl
- tert
- benzotriazole
- phenyl
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- 238000011049 filling Methods 0.000 title claims abstract description 26
- 239000003063 flame retardant Substances 0.000 title claims abstract description 26
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- 239000000463 material Substances 0.000 claims abstract description 42
- -1 phosphorous acid ester Chemical class 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 150000001412 amines Chemical class 0.000 claims abstract description 14
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- 238000000034 method Methods 0.000 claims abstract description 8
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- 239000000203 mixture Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- 239000012964 benzotriazole Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 18
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
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- IUTYMBRQELGIRS-UHFFFAOYSA-N boric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OB(O)O.NC1=NC(N)=NC(N)=N1 IUTYMBRQELGIRS-UHFFFAOYSA-N 0.000 claims description 15
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 7
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- RKMGAJGJIURJSJ-UHFFFAOYSA-N 2,2,6,6-Tetramethylpiperidine Substances CC1(C)CCCC(C)(C)N1 RKMGAJGJIURJSJ-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 6
- FIDRAVVQGKNYQK-UHFFFAOYSA-N 1,2,3,4-tetrahydrotriazine Chemical compound C1NNNC=C1 FIDRAVVQGKNYQK-UHFFFAOYSA-N 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 150000001912 cyanamides Chemical class 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
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- 239000010452 phosphate Substances 0.000 claims description 5
- UWSMKYBKUPAEJQ-UHFFFAOYSA-N 5-Chloro-2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2H-benzotriazole Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O UWSMKYBKUPAEJQ-UHFFFAOYSA-N 0.000 claims description 4
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- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
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- UKJARPDLRWBRAX-UHFFFAOYSA-N n,n'-bis(2,2,6,6-tetramethylpiperidin-4-yl)hexane-1,6-diamine Chemical compound C1C(C)(C)NC(C)(C)CC1NCCCCCCNC1CC(C)(C)NC(C)(C)C1 UKJARPDLRWBRAX-UHFFFAOYSA-N 0.000 claims description 3
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- OMWSZDODENFLSV-UHFFFAOYSA-N (5-chloro-2-hydroxyphenyl)-phenylmethanone Chemical compound OC1=CC=C(Cl)C=C1C(=O)C1=CC=CC=C1 OMWSZDODENFLSV-UHFFFAOYSA-N 0.000 claims description 2
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- XTARNDCHFFABBE-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4,5-dichlorophenol Chemical compound OC1=CC(Cl)=C(Cl)C=C1N1N=C2C=CC=CC2=N1 XTARNDCHFFABBE-UHFFFAOYSA-N 0.000 claims description 2
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- ITLDHFORLZTRJI-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-5-octoxyphenol Chemical compound OC1=CC(OCCCCCCCC)=CC=C1N1N=C2C=CC=CC2=N1 ITLDHFORLZTRJI-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本发明提供了一种低填充无卤膨胀型阻燃光伏封装材料,主要由质量组成如下的原料制成:光伏封装基体材料100份,微胶囊化膨胀型阻燃剂10~23份,经偶联剂处理的无机纳米阻燃剂2~15份,过氧化物类交联剂0.1~10份,酚类或亚磷酸脂类抗氧剂0.05~5份,受阻胺类光稳定剂0.01~5份,紫外光吸收剂0.01~2份,增粘剂0.01~3份;本发明采用直接固相缩聚工艺和微胶囊技术,制备微胶囊化聚磷酸三聚氰胺硼酸盐阻燃剂,再利用无机纳米阻燃剂的协效作用,有效降低了阻燃剂的填充量,从而低成本的实现了改善封装材料的阻燃性能的同时保证其力学性能和绝缘性能不显著下降;通过其他助剂的加入,保证阻燃光伏封装材料的绝缘性能、耐湿热、紫外老化性能等性能满足光伏封装领域的要求。
Description
(一)技术领域
本发明涉及一种低填充无卤膨胀型阻燃光伏封装材料及其制备方法。
(二)背景技术
光伏作为一种清洁的、无噪声污染的可再生能源,同时具有不排放温室效应气体的优点。随着能源需求的日益增长和环境污染的日益严重,更好的利用太阳能被认为是一种最佳的解决方案之一。在实际应用中,大多数太阳能电池封装成“三明治”结构,典型的如:玻璃/EVA/ARC-Si/EVA/TPT结构。而上述结构中EVA的氧指数仅为19,属于易燃材料,且燃烧时易产生带有毒性气体的黑烟。
目前常用于EVA阻燃的阻燃体系为磷系、氮系、硅系、无机或复合型阻燃剂。其中,以镁铝化合物为代表的无机阻燃剂存在因添加量大而导致材料加工困难、力学性能下降等问题。环保膨胀型阻燃剂则往往需要将“碳源”、“酸源”、“气源”等多个阻燃剂物理共混后进行复配阻燃,才能获得较好的阻燃效果,容易产生分散不均、易迁移和相容性等问题。
鉴于上述状况,目前需要一种可以利用现有EVA设备连续生产同时具有高效阻燃效果的阻燃光伏封装材料。
(三)发明内容
本发明目的即是提供一种低填充无卤膨胀型阻燃光伏封装材料及其制备方法。
本发明采用的技术方案是:
一种低填充无卤膨胀型阻燃光伏封装材料,主要由质量组成如下的原料制成:
所述光伏封装基体材料为下列之一或其中两种以上的混合物:乙烯-醋酸乙烯酯共聚物(EVA)、茂金属催化聚乙烯、乙烯辛烯共聚物、乙烯戊烯共聚物;
所述微胶囊化膨胀型阻燃剂为微胶囊化聚磷酸三聚氰胺硼酸盐(MPB-S);由聚磷酸三聚氰胺硼酸盐(MPB)经超细化处理,再用密胺树脂包覆制得,聚磷酸三聚氰胺硼酸盐(MPB)可以磷酸类化合物、三聚氰胺类化合物和硼酸为原料,采用直接固相缩聚工艺合成。
所述经偶联剂处理的无机纳米阻燃剂为经偶联剂处理的纳米氢氧化铝、纳米氢氧化镁、纳米二氧化硅、纳米氧化锌和纳米二氧化钛中的一种或多种,优选为经偶联剂处理的纳米氢氧化镁和/或纳米氧化锌,粒径为10nm~100nm;所述偶联剂为本领域常规偶联剂,优选为硅烷偶联剂。
上述原料为制备所述低填充无卤膨胀型阻燃光伏封装材料所用的主要原料,不包括制备过程中所用的溶剂。所述过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂为本领域常规助剂。
具体的,所述过氧化物类交联剂可为下列之一或其中两种以上的混合物:1,1-二(叔丁基过氧化)-3,3,5-三甲基环己烷、2,5-二甲基己烷-2,5-二叔丁基过氧化物、2,5-二甲基-2,5-双(苯甲酰过氧)-己烷、过氧化二异丙苯、双(2-叔丁基过氧化异丙基)苯、过氧化叔丁基异丙苯、二叔丁基过氧化物、过苯甲酸叔戊酯、2,2-双(叔戊基过氧)-丁烷、二叔戊基过氧化物、叔丁基过氧化苯甲酸酯、二苯甲酰基过氧化物、二(4-氯苯甲酰基)过氧化物、二(2,4-二氯苯甲酸基)过氧化物、二(4-甲基苯甲酰基)过氧化物、正丁基-4,4-二(叔丁基过氧化)戊酸酯、乙基-3,3-二(叔丁基过氧化)-丁酸酯、叔丁基过氧化-异丙基碳酸酯、叔丁基过氧化-2-乙基己基碳酸酯、邻,邻-叔丁基-邻-异丙基-单-过氧化碳酸酯、叔丁基过氧化碳酸-2-乙基己酯、邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯;优选为邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯。
所述酚类或亚磷酸脂类抗氧剂为下列之一或其中两种以上的混合物:1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮、2,2’-亚甲基-双-(4-乙基-6-叔丁基苯酚)、2,2’-亚甲基-双-(4-甲基-6-叔丁基苯酚)、β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八酯、三(2,4-二叔丁基苯基)亚磷酸酯、二(2,4-二枯基苯基)季戊四醇二亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯、三(壬基苯基)亚磷酸酯。优选为下列之一或其中两种以上的混合物:1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮、三(2,4,-二叔丁基苯基)亚磷酸酯、三(2,4,-二枯基苯基)季戊四醇二亚磷酸酯。
所述受阻胺类光稳定剂为下列之一或其中两种以上的混合物:3,5-二叔丁基-4-羟基-苯甲酸十六烷基酯、三(1,2,2,6,6-五甲基-4-哌啶基)亚磷酸酯、癸二酸双-2,2,6,6-四甲基哌啶醇酯、双-1-癸烷氧基-2,2,6,6-四甲基哌啶-4-醇癸二酸酯、丁二酸和4-羟基-2,2,6,6-四甲基-1-哌啶醇的聚合物、N,N’-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺和2,4-二氯-6-(1,1,3,3-四甲基丁基)氨基-1,3,5-三嗪的聚合物、N,N’-双(2,2,6,6-五甲基-4-哌啶基)-1,6-己二胺和吗啉-2,4,6-三氯-1,3,5-三嗪的聚合物。优选为下列之一或其中两种以上的混合物:癸二酸双-2,2,6,6-四甲基哌啶醇酯、双(1,2,2,6,6-五甲基-4-哌啶基)贵二酸酯、甲基-1,2,2,6,6-五甲基-4-哌啶基贵二酸酯。
所述紫外光吸收剂为下列之一或其中两种以上的混合物:2,2’-(1,4-亚苯基)双(4H-3,1-苯并噁嗪-4-酮)、2,2’-双(3,1-苯并噁嗪-4-酮)、2,2’-四亚甲基双(3,1-苯并噁嗪-4-酮)、2,2’-十亚甲基双(3,1-苯并噁嗪-4-酮)、2,2’-对亚苯基双(3,1-苯并噁嗪-4-酮)、2,2’-间亚甲基双(3,1-苯并噁嗪-4-酮)、1,3,5-三(3,1-苯并噁嗪-4-酮-2-基)苯、2,4,6-三(3,1-苯并噁嗪-4-酮-2-基)萘、2,8-二甲基-4H,6H-苯并(1,2-d;5,4-d’)双(1,3)-噁嗪-4,6-二酮、6’,6-磺酰基双(2-甲基-4H,3,1-苯并噁嗪-4-酮)、6,7’-亚甲基双(2-甲基-4H,3,1-苯并噁嗪-4-酮)、2-羟基-4-甲氧基二苯甲酮、2,4-二羟基二苯甲酮、2-羟基-4-n-辛氧基二苯甲酮、2-羟基-4-甲氧基-2’-羧基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、2-羟基-5-氯二苯甲酮、双-(2-甲氧基-4-羟基-5-苯甲酰基苯基)甲烷、2-(2’-羟基苯基)苯并***、2-(2’-羟基-5-甲基苯基)苯并***、2-(2’-羟基-5-甲基苯基)-5-羧酸丁基酯苯并***、2-(2’-羟基-5’-甲基苯基)-5,6-二氯苯并***、2-(2’-羟基-5-甲基苯基)-5-乙基磺酸苯并***、2-(2’-羟基-5’-叔丁基苯基)-5-氯苯并***、2-(2’-羟基-5’-叔丁基苯基)苯并***、2-(2’-羟基-5’-氨苯基)苯并***、2-(2’-羟基3’,-5’-二甲基苯基)苯并***、2-(2’-甲基-4’-羟基苯基)苯并***、2-(2’-羟基-5-羧基苯基)苯并***乙基酯、2-(2’-羟基-3’甲基-5’-叔丁基苯基)苯并***、2-(2’-十八烷基氧基-3’,5’-二甲基苯基)-5-甲基苯并***、2-(2’-羟基-3’,5’-二叔丁基苯基)-5-氯苯并***、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯苯并***、2-(2’-羟基-5’-甲氧基苯基)苯并***、2-(2’-羟基-3’,5’-二叔丁基苯基)-5-氯苯并***、2-(2’-羟基-5’-环己基苯基)苯并***、2-(2’-羟基-4’,5’-二甲基苯基)-5-羧酸苯并***丁基酯、2-(2’-羟基-3’,5’-二氯苯基)苯并***、2-(2’-羟基-4’,5’-二氯苯基)苯并***、2-(2’-羟基-3’,5’-二甲基苯基)-5-乙基磺酰苯并***、2-(2’-羟基-4’-辛氧基苯基)苯并***、2-(2’-羟基-5’-甲氧基苯基)-5-甲基苯并***、2-(2’-羟基-5’-甲基苯基)-5-羧酸酯苯并***、2-(2’-羟基-5’-叔辛基苯基)-5-苯并***或2-(2’-乙酰氧基-5’-甲基苯基)苯并***。优选为下列之一或其中两种以上的混合物:2,2-四亚甲基双(3,1-苯并噁嗪-4-酮)、2-(2’-羟基-5-甲基苯基)苯并***、2,2’-二羟基-4,4’-二甲氧基二苯甲酮。
所述增粘剂为下列之一或其中两种以上的混合物:γ-氨丙基三乙氧基硅烷、γ-甲基丙烯酸酰氧基丙基三甲氧基硅烷、γ-缩水甘油醚氧丙基三甲基硅烷、3-氨丙基三甲基硅烷;优选为γ-氨丙基三乙氧基硅烷。
本发明还涉及所述封装材料的制备方法,所述方法包括:
(1)将磷酸类化合物、三聚氰胺类化合物和硼酸按1.05~1.5:1:1~1.5摩尔比球磨混合10~20min,得到MPB混合原料;所述磷酸类化合物为聚磷酸铵、磷酸、双酚二磷酸盐中的一种或多种,优选为聚磷酸铵;所述三聚氰胺类化合物选自三聚氰胺、三聚氰胺尿酸盐或其组合,优选为三聚氰胺;
(2)将步骤(1)中获得的MPB混合原料在300~350℃下反应1~3h,制得MPB9(聚磷酸三聚氰胺硼酸盐);
(3)将步骤(2)中获得的MPB球磨15~30min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB18wt%~25wt%的MPB溶液;再加入与MPB质量比为1:15~25的十六烷基三甲基溴化铵,搅拌0.5~1h;加入密胺树脂(三聚氰胺甲醛树脂),使其在MPB溶液中的浓度范围为1wt~5wt%,用磷酸调节MPB溶液pH至4~5,将溶液水浴加热至70~90℃,反应1.5~3h,冷却,抽滤,用去离子水洗涤3~5次,然后在70~90℃下干燥18~22h,制得MPB-S(微胶囊化聚磷酸三聚氰胺硼酸盐);
(4)向0.5wt%~1.5wt%的硅烷偶联剂无水乙醇溶液(即溶质为硅烷偶联剂,溶剂为无水乙醇,硅烷偶联剂质量浓度为0.5%~1.5%)中加入无机纳米阻燃剂,超声混合1~3h,振荡频率100~140次/min,50~90℃的温度下烘干10~34h,得到改性无机纳米阻燃剂,备用。其中硅烷偶联剂的质量用量为无机纳米阻燃剂质量的0.5%~3%;所述偶联剂可为下列之一:KH550、KH570。
(5)将配方量的过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂共同在50~70℃的水浴中搅拌10~30min,得混合助剂,备用;
(6)先将配方量的光伏封装基体材料加入到混料机中,然后将1/3~2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1~2min;再将剩余的混合助剂加入到混料机中,继续搅拌1~2min后,再将配方量的步骤(3)得到的MPB-S和步骤(4)制得的改性无机纳米阻燃剂加入到混料机中,搅拌3~5min,得混合物;
(7)将步骤(6)得到的混合物倒入挤出机,在80~100℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到所述低填充无卤膨胀型阻燃光伏封装材料。
本发明的有益效果主要体现在:本发明采用直接固相缩聚工艺和微胶囊技术,制备微胶囊化聚磷酸三聚氰胺硼酸盐阻燃剂,再利用无机纳米阻燃剂的协效作用,有效降低了阻燃剂的填充量,从而低成本的实现了改善封装材料的阻燃性能的同时保证其力学性能和绝缘性能不显著下降;通过其他助剂的加入,保证阻燃光伏封装材料的绝缘性能、耐湿热、紫外老化性能等性能满足光伏封装领域的要求。
(四)具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此:
实施例1:
一种低填充无卤膨胀型阻燃光伏封装材料,以重量份计,其主要原料组成如下:100份VA含量为33%的乙烯-醋酸乙烯酯共聚物(美国杜邦公司),10份MPB-S,15份粒径为10nm的氧化锌,0.1份受阻胺类光稳定剂癸二酸双-2,2,6,6-四甲基哌啶醇酯(上海焱佳塑化有限公司),0.2份抗氧剂1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮/三(2,4,-二叔丁基苯基)亚磷酸酯复配物(质量比1:2,天大天海科技发展有限公司),0.2份交联剂邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯(广州力本(巨龙)橡胶原料贸易有限公司),0.1份紫外吸收剂2,2-四亚甲基双(3,1-苯并噁嗪-4-酮)(南京众何晟科技有限公司),3份增粘剂γ-氨丙基三乙氧基硅烷(南京立派化工有限公司)。
上述低填充无卤膨胀型阻燃光伏封装材料按照如下方法制备:
(1)将磷酸铵、三聚氰胺和硼酸按1.05:1:1.5摩尔比球磨混合15min,得到MPB混合原料。
(2)将步骤(1)中获得的MPB混合原料在300℃,1个大气压下,反应3h,制得MPB。
(3)将步骤(2)中获得的MPB球磨20min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB20wt%的MPB溶液;再加入与MPB质量比为1:25的十六烷基三甲基溴化铵,搅拌0.5h;加入密胺树脂(三聚氰胺甲醛树脂),使其在MPB溶液中的浓度范围为1wt%,用10wt%的磷酸调节MPB溶液PH至4.5左右,将溶液水浴加热至80℃,反应2h,冷却,抽滤,用去离子水洗涤3~5次,然后在80℃下干燥20h,制得MPB-S。
(4)向0.5wt%的硅烷偶联剂KH550无水乙醇溶液中加入粒径为10nm的氧化锌,其中硅烷偶联剂KH550的用量为氧化锌质量的1%,超声混合2h,振荡频率140次/min,80℃的温度下烘干30h,得到改性纳米氧化锌,备用。
(5)将配方量的过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂共同在60℃的水浴中搅拌20min,得混合助剂,备用。
(6)先将配方量的光伏封装基体材料加入到混料机中,然后将1/3~2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1~2min;再将剩余的混合助剂加入到混料机中,继续搅拌1~2min。
(7)将配方量的步骤(3)得到的MPB-S和步骤(4)制得的改性纳米氧化锌加入到混料机中,搅拌3~5min,得混合物。
(8)将步骤(7)得到的混合物倒入挤出机,在90℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到本发明的低填充无卤膨胀型阻燃光伏封装材料S-1。
实施例2:
一种低填充无卤膨胀型阻燃光伏封装材料,以重量份计,其组成如下:100份VA含量为16%的乙烯醋酸乙烯酯共聚物(美国杜邦公司)中,23份MPB-S,2份粒径为20nm的氢氧化镁,0.1份受阻胺类光稳定剂癸二酸双-2,2,6,6-四甲基哌啶醇酯(上海焱佳塑化有限公司),0.2份抗氧剂1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮/三(2,4,-二枯基苯基)季戊四醇二亚磷酸酯复配物(质量比1:4,天大天海科技发展有限公司),1.5份交联剂邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯(广州力本(巨龙)橡胶原料贸易有限公司),0.1份紫外吸收剂紫外吸收剂2,2-四亚甲基双(3,1-苯并噁嗪-4-酮)(南京众何晟科技有限公司),0.4份增粘剂γ-氨丙基三乙氧基硅烷(南京立派化工有限公司)。
上述低填充无卤膨胀型阻燃光伏封装材料按照如下方法制备:
(1)将磷酸铵、三聚氰胺和硼酸按1.5:1:1摩尔比球磨混合18min,得到MPB混合原料。
(2)将步骤(1)中获得的MPB混合原料在330℃,1个大气压下,反应2.5h,制得MPB。
(3)将步骤(2)中获得的MPB球磨18min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB20wt%的MPB溶液;再加入与MPB质量比为1:20的十六烷基三甲基溴化铵,搅拌0.5h;加入密胺树脂(三聚氰胺甲醛树脂),使其在MPB溶液中的浓度范围为1wt%,用10wt%的磷酸调节MPB溶液PH至4.5左右,将溶液水浴加热至80℃,反应2h,冷却,抽滤,用去离子水洗涤3~5次,然后在80℃下干燥20h,制得MPB-S。
(4)向0.5wt%的硅烷偶联剂KH550无水乙醇溶液中加入粒径为20nm的氢氧化镁,其中硅烷偶联剂KH550的用量为氧化锌质量的0.5%,超声混合1h,振荡频率100次/min,50℃的温度下烘干15h,得到改性纳米氢氧化镁,备用。
(5)将配方量的过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂、增塑剂共同在60℃的水浴中搅拌20min,得混合助剂,备用。
(6)先将配方量的光伏封装基体材料加入到混料机中,然后将1/3-2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1-2min;再将剩余的混合助剂加入到混料机中,继续搅拌1-2min。
(7)将配方量的步骤(3)得到的MPB-S和步骤(4)制得的改性纳米氢氧化镁加入到混料机中,搅拌3-5min,得混合物。
(8)将步骤(7)得到的混合物倒入挤出机,在90℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到本发明的低填充无卤膨胀型阻燃光伏封装材料S-2。
实施例3:
一种低填充无卤膨胀型阻燃光伏封装材料,以重量份计,其组成如下:100份VA含量为40%的乙烯-醋酸乙烯酯共聚物(美国杜邦公司),20份MPB-S,5份粒径为30nm的氢氧化铝,0.1份受阻胺类光稳定剂双(1,2,2,6,6-五甲基-4-哌啶基)贵二酸酯/甲基-1,2,2,6,6-五甲基-4-哌啶基贵二酸酯复配物(质量比1:1,北京天罡有限责任公司),0.2份抗氧剂1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮/三(2,4,-二枯基苯基)季戊四醇二亚磷酸酯复配物(质量比1:4,天大天海科技发展有限公司),1.5份交联剂邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯(广州力本(巨龙)橡胶原料贸易有限公司),0.5份紫外吸收剂2-(2’-羟基-5-甲基苯基)苯并***(南京众何晟科技有限公司),0.4份增粘剂γ-氨丙基三乙氧基硅烷(南京立派化工有限公司)。
上述低填充无卤膨胀型阻燃光伏封装材料按照如下方法制备:
(1)将磷酸铵、三聚氰胺和硼酸按1.05:1:1.2摩尔比球磨混合15min,得到MPB混合原料。
(2)将步骤(1)中获得的MPB混合原料在330℃,1个大气压下,反应2.5h,制得MPB。
(3)将步骤(2)中获得的MPB球磨20min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB20wt%的MPB溶液;再加入与MPB质量比为1:20的十六烷基三甲基溴化铵,搅拌0.5h;加入密胺树脂(三聚氰胺甲醛树脂),使其在MPB溶液中的浓度范围为1wt%,用10wt%的磷酸调节MPB溶液PH至4.5左右,将溶液水浴加热至80℃,反应2h,冷却,抽滤,用去离子水洗涤3-5次,然后在80℃下干燥20h,制得MPB-S。
(4)向0.5wt%的硅烷偶联剂KH570无水乙醇溶液中加入粒径为30nm的氢氧化铝,其中硅烷偶联剂KH570的用量为氧化锌质量的0.5%,超声混合2h,振荡频率110次/min,80℃的温度下烘干24h,得到改性纳米氢氧化铝,备用。
(5)将配方量的过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂共同在60℃的水浴中搅拌20min,得混合助剂,备用。
(6)先将配方量的光伏封装基体材料加入到混料机中,然后将1/3-2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1-2min;再将剩余的混合助剂加入到混料机中,继续搅拌1-2min。
(7)将配方量的步骤(3)得到的MPB-S和步骤(4)制得的改性纳米氢氧化铝加入到混料机中,搅拌3-5min,得混合物。
(8)将步骤(7)得到的混合物倒入挤出机,在90℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到本发明的低填充无卤膨胀型阻燃光伏封装材料S-3。
实施例4:
一种低填充无卤膨胀型阻燃光伏封装材料,以重量份计,其组成如下:100份茂金属催化聚乙烯(PEKN,三菱化学公司)树脂原料,18份MPB-S,7份粒径为50m的二氧化硅,0.1份受阻胺类光稳定剂癸二酸双-2,2,6,6-四甲基哌啶醇酯(上海焱佳塑化有限公司),0.2份抗氧剂1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮/三(2,4,-二叔丁基苯基)亚磷酸酯复配物(质量比1:2,天大天海科技发展有限公司),0.2份交联剂邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯(广州力本(巨龙)橡胶原料贸易有限公司),0.1份紫外吸收剂2,2’-二羟基-4,4’-二甲氧基二苯甲酮(南京众何晟科技有限公司),3份增粘剂γ-氨丙基三乙氧基硅烷(南京立派化工有限公司)。
上述低填充无卤膨胀型阻燃光伏封装材料按照如下方法制备:
(1)将磷酸铵、三聚氰胺和硼酸按1.1:1:1.2摩尔比球磨混合15min,得到MPB混合原料。
(2)将步骤(1)中获得的MPB混合原料在330℃,1个大气压下,反应2.5h,制得MPB。
(3)将步骤(2)中获得的MPB球磨20min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB20wt%的MPB溶液;再加入与MPB质量比为1:20的十六烷基三甲基溴化铵,搅拌0.5h;加入密胺树脂(三聚氰胺甲醛树脂),使其在MPB溶液中的浓度范围为1wt%,用10wt%的磷酸调节MPB溶液PH至4.5左右,将溶液水浴加热至80℃,反应2h,冷却,抽滤,用去离子水洗涤3-5次,然后在80℃下干燥20h,制得MPB-S。
(4)向0.5wt%的硅烷偶联剂KH570无水乙醇溶液中加入粒径为50m的二氧化硅,其中硅烷偶联剂KH570的用量为氧化锌质量的0.5%,超声混合2h,振荡频率120次/min,80℃的温度下烘干24h,得到改性纳米二氧化硅,备用。
(5)将配方量的过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂共同在60℃的水浴中搅拌20min,得混合助剂,备用。
(6)先将配方量的光伏封装基体材料加入到混料机中,然后将1/3~2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1~2min;再将剩余的混合助剂加入到混料机中,继续搅拌1~2min。
(7)将配方量的步骤(3)得到的MPB-S和步骤(4)制得的改性纳米二氧化硅加入到混料机中,搅拌3~5min,得混合物。
(8)将步骤(7)得到的混合物倒入挤出机,在90℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到本发明的低填充无卤膨胀型阻燃光伏封装材料S-4。
对比例:
在90份VA含量为33%的乙烯-醋酸乙烯酯共聚物中,加入10份茂金属催化的乙烯-戊烯共聚物,3份光稳定剂N,N’-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺和2,4-二氯-6-(1,1,3,3-四甲氧基)氨基-1,3,5-三嗪的聚合物,2份抗氧剂1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮/三(2,4-二叔丁基苯基)亚磷酸酯复配物,5份交联剂邻,邻-叔丁基-邻-(2-乙基己基)-单-过氧化碳酸酯,并混合均匀。
将混合物在挤出机中进行共混挤出,温度控制在90℃,挤出物经过流延、冷却、分切、卷取工序,制得封装胶膜,记为C-1。
性能测试:
低填充无卤膨胀型阻燃光伏封装材料的各项性能指标通过以下的方法来进行测定:
1、阻燃性能
阻燃性能按照UL94Test标准进行测试。
2、氧指数
氧指数按照标准ISO4589-1984进行测试。
3、与TPT的粘接强度
按照标准GB/T2790-1995进行测试。
4、耐紫外光辐照性能
按照国际电工委员会标准IEC61345规定要求进行紫外辐照老化测试。
试验条件:试样表面温度60±5℃;波长为280-400nm范围,辐照强度为15KW·h/m2。黄变指数(ΔYI)是由按GB2409-80进行分析。
5、耐湿热老化性能
按GB/T2423.3试验方法进行湿热老化试验。
试验条件:+85℃,相对湿度85%,2000h。
黄变指数(ΔYI)按GB2409-80进行分析。
6、体积电阻率
按照标准GB/T1410进行测定。
通过上述实施例得到的低填充无卤膨胀型阻燃光伏封装材料,经上述测试方法进行评价,其评价结果下表所示:
本发明并不局限于所述的实施例,本领域的技术人员在不脱离本发明的精神即公开范围内,仍可做一些修正或改变,故本发明的权利保护范围以权利要求书限定的范围为准。
Claims (7)
2.如权利要求1所述的封装材料,其特征在于所述过氧化物类交联剂为下列之一或其中两种以上的混合物:1,1-二(叔丁基过氧化)-3,3,5-三甲基环己烷、2,5-二甲基己烷-2,5-二叔丁基过氧化物、2,5-二甲基-2,5-双(苯甲酰过氧)-己烷、过氧化二异丙苯、双(2-叔丁基过氧化异丙基)苯、过氧化叔丁基异丙苯、二叔丁基过氧化物、过苯甲酸叔戊酯、2,2-双(叔戊基过氧)-丁烷、二叔戊基过氧化物、叔丁基过氧化苯甲酸酯、二苯甲酰基过氧化物、二(4-氯苯甲酰基)过氧化物、二(2,4-二氯苯甲酸基)过氧化物、二(4-甲基苯甲酰基)过氧化物、正丁基-4,4-二(叔丁基过氧化)戊酸酯、乙基-3,3-二(叔丁基过氧化)-丁酸酯、叔丁基过氧化-异丙基碳酸酯、叔丁基过氧化-2-乙基己基碳酸酯、邻,邻-叔丁基-邻-异丙基-单-过氧化碳酸酯、叔丁基过氧化碳酸-2-乙基己酯、邻,邻-叔戊基-邻-(2-乙基己基)-单-过氧化碳酸酯。
3.如权利要求1所述的封装材料,其特征在于所述酚类或亚磷酸脂类抗氧剂为下列之一或其中两种以上的混合物:1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苯甲基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮、2,2’-亚甲基-双-(4-乙基-6-叔丁基苯酚)、2,2’-亚甲基-双-(4-甲基-6-叔丁基苯酚)、β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八酯、三(2,4-二叔丁基苯基)亚磷酸酯、二(2,4-二枯基苯基)季戊四醇二亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯、三(壬基苯基)亚磷酸酯。
4.如权利要求1所述的封装材料,其特征在于所述受阻胺类光稳定剂为下列之一或其中两种以上的混合物:3,5-二叔丁基-4-羟基-苯甲酸十六烷基酯、三(1,2,2,6,6-五甲基-4-哌啶基)亚磷酸酯、癸二酸双-2,2,6,6-四甲基哌啶醇酯、双-1-癸烷氧基-2,2,6,6-四甲基哌啶-4-醇癸二酸酯、丁二酸和4-羟基-2,2,6,6-四甲基-1-哌啶醇的聚合物、N,N’-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺和2,4-二氯-6-(1,1,3,3-四甲基丁基)氨基-1,3,5-三嗪的聚合物、N,N’-双(2,2,6,6-五甲基-4-哌啶基)-1,6-己二胺和吗啉-2,4,6-三氯-1,3,5-三嗪的聚合物。
5.如权利要求1所述的封装材料,其特征在于所述紫外光吸收剂为下列之一或其中两种以上的混合物:2,2’-(1,4-亚苯基)双(4H-3,1-苯并噁嗪-4-酮)、2,2’-双(3,1-苯并噁嗪-4-酮)、2,2’-四亚甲基双(3,1-苯并噁嗪-4-酮)、2,2’-十亚甲基双(3,1-苯并噁嗪-4-酮)、2,2’-对亚苯基双(3,1-苯并噁嗪-4-酮)、2,2’-间亚甲基双(3,1-苯并噁嗪-4-酮)、1,3,5-三(3,1-苯并噁嗪-4-酮-2-基)苯、2,4,6-三(3,1-苯并噁嗪-4-酮-2-基)萘、2,8-二甲基-4H,6H-苯并(1,2-d;5,4-d’)双(1,3)-噁嗪-4,6-二酮、6’,6-磺酰基双(2-甲基-4H,3,1-苯并噁嗪-4-酮)、6,7’-亚甲基双(2-甲基-4H,3,1-苯并噁嗪-4-酮)、2-羟基-4-甲氧基二苯甲酮、2,4-二羟基二苯甲酮、2-羟基-4-n-辛氧基二苯甲酮、2-羟基-4-甲氧基-2’-羧基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、2-羟基-5-氯二苯甲酮、双-(2-甲氧基-4-羟基-5-苯甲酰基苯基)甲烷、2-(2’-羟基苯基)苯并***、2-(2’-羟基-5-甲基苯基)苯并***、2-(2’-羟基-5-甲基苯基)-5-羧酸丁基酯苯并***、2-(2’-羟基-5’-甲基苯基)-5,6-二氯苯并***、2-(2’-羟基-5-甲基苯基)-5-乙基磺酸苯并***、2-(2’-羟基-5’-叔丁基苯基)-5-氯苯并***、2-(2’-羟基-5’-叔丁基苯基)苯并***、2-(2’-羟基-5’-氨苯基)苯并***、2-(2’-羟基3’,-5’-二甲基苯基)苯并***、2-(2’-甲基-4’-羟基苯基)苯并***、2-(2’-羟基-5-羧基苯基)苯并***乙基酯、2-(2’-羟基-3’甲基-5’-叔丁基苯基)苯并***、2-(2’-十八烷基氧基-3’,5’-二甲基苯基)-5-甲基苯并***、2-(2’-羟基-3’,5’-二叔丁基苯基)-5-氯苯并***、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯苯并***、2-(2’-羟基-5’-甲氧基苯基)苯并***、2-(2’-羟基-3’,5’-二叔丁基苯基)-5-氯苯并***、2-(2’-羟基-5’-环己基苯基)苯并***、2-(2’-羟基-4’,5’-二甲基苯基)-5-羧酸苯并***丁基酯、2-(2’-羟基-3’,5’-二氯苯基)苯并***、2-(2’-羟基-4’,5’-二氯苯基)苯并***、2-(2’-羟基-3’,5’-二甲基苯基)-5-乙基磺酰苯并***、2-(2’-羟基-4’-辛氧基苯基)苯并***、2-(2’-羟基-5’-甲氧基苯基)-5-甲基苯并***、2-(2’-羟基-5’-甲基苯基)-5-羧酸酯苯并***、2-(2’-羟基-5’-叔辛基苯基)-5-苯并***或2-(2’-乙酰氧基-5’-甲基苯基)苯并***。
6.如权利要求1所述的封装材料,其特征在于所述增粘剂为下列之一或其中两种以上的混合物:γ-氨丙基三乙氧基硅烷、γ-甲基丙烯酸酰氧基丙基三甲氧基硅烷、γ-缩水甘油醚氧丙基三甲基硅烷、3-氨丙基三甲基硅烷。
7.如权利要求1所述封装材料的制备方法,所述方法包括:
(1)将磷酸类化合物、三聚氰胺类化合物和硼酸按1.05~1.5:1:1~1.5摩尔比球磨混合10~20min,得到MPB混合原料;所述磷酸类化合物为聚磷酸铵、磷酸、双酚二磷酸盐中的一种或多种,所述三聚氰胺类化合物选自三聚氰胺、三聚氰胺尿酸盐或其组合;
(2)将步骤(1)中获得的MPB混合原料在300~350℃下反应1~3h,制得MPB;
(3)将步骤(2)中获得的MPB球磨15~30min,将球磨后的MPB加入到水和酒精体积比为1:1的溶液中,配制成含MPB18wt%~25wt%的MPB溶液;再加入与MPB质量比为1:15~25的十六烷基三甲基溴化铵,搅拌0.5~1h;加入密胺树脂,使其在MPB溶液中的浓度范围为1wt~5wt%,用磷酸调节MPB溶液pH至4~5,将溶液水浴加热至70~90℃,反应1.5~3h,冷却,抽滤,用去离子水洗涤3~5次,然后在70~90℃下干燥18~22h,制得MPB-S;
(4)向0.5wt%~1.5wt%的偶联剂无水乙醇溶液中加入无机纳米阻燃剂,超声混合1~3h,振荡频率100~140次/min,50~90℃的温度下烘干10~34h,得到改性无机纳米阻燃剂,备用;
(5)将过氧化物类交联剂、酚类或亚磷酸脂类抗氧剂、受阻胺类光稳定剂、紫外光吸收剂、增粘剂共同在50~70℃的水浴中搅拌10~30min,得混合助剂,备用;
(6)先将光伏封装基体材料加入到混料机中,然后将1/3~2/3步骤(5)获得的混合助剂加入到混料机中,搅拌1~2min;再将剩余的混合助剂加入到混料机中,继续搅拌1~2min后,再将步骤(3)得到的MPB-S和步骤(4)制得的改性无机纳米阻燃剂加入到混料机中,搅拌3~5min,得混合物;
(7)将步骤(6)得到的混合物倒入挤出机,在80~100℃的温度下进行挤出、流延成膜、冷却、分切及收卷,得到所述低填充无卤膨胀型阻燃光伏封装材料。
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CN108998974A (zh) * | 2018-09-11 | 2018-12-14 | 宁波叮叮家居科技有限公司 | 一种防紫外线窗帘面料的制备方法 |
CN112409391A (zh) * | 2020-11-20 | 2021-02-26 | 云南江磷集团股份有限公司 | 硼酸密胺盐热缩聚物抗熔滴剂及其在pa6中的应用 |
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