CN107353859A - 一种复合型光伏背板用绝缘胶粘剂材料及应用 - Google Patents
一种复合型光伏背板用绝缘胶粘剂材料及应用 Download PDFInfo
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- CN107353859A CN107353859A CN201710561997.1A CN201710561997A CN107353859A CN 107353859 A CN107353859 A CN 107353859A CN 201710561997 A CN201710561997 A CN 201710561997A CN 107353859 A CN107353859 A CN 107353859A
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- acid
- butyl
- component
- adhesive material
- photovoltaic back
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Abstract
本发明公开了一种复合型光伏背板用绝缘胶粘剂材料及应用。该绝缘胶粘剂材料由A、B两组分构成。A组分包含有主体树脂、辅助树脂及助剂,其中主体树脂为羟基聚酯树脂,其羟值为5~30mgKOH/g,酸值为0.2~5mgKOH/g,数均分子量为5000~50000,玻璃化转变温度为‑40℃~30℃。在惰性气体保护下,由小分子多元酸与多元醇经酯化缩聚反应制成。B组分为交联组分。使用时,A组分和B组分按需求以不同比例混合。本发明绝缘胶粘剂材料不仅具有长期稳定的粘结性能,同时在耐热性、绝缘性、耐候性方面也具有优异的表现,可用于制备高耐候性复合型光伏背板。本发明原料易得,工艺可控,操作简便。
Description
技术领域
本发明涉及复合用胶粘剂材料领域,尤其涉及一种复合型光伏背板用绝缘胶粘剂材料及应用。
背景技术
光伏是一种利用太阳电池半导体材料的光伏效应,将太阳光辐射能直接转换为电能的一种新型发电系统,有独立运行和并网运行两种方式。由于太阳能电池寿命长,与火力发电、核能发电相比,太阳能电池不会引起环境污染,国际上对于太阳能光伏电池的需求日益庞大。截至2016年底,全球光伏装机总量达到300GW。其中,2016全球光伏新增装机70GW,比2015年增长大约30%,成为全球光伏装机增长的一个里程碑。近年来,我国光伏产业发展迅速,在2016年新增装机量中,我国贡献了34.54GW,同比2015年增长了128%,同时累计装机量达到77.42GW,新增和累计装机容量均成为全球第一。
然而,要使太阳能发电真正达到实用水平,还有两个重要的制约因素急需解决,一是要提高太阳能光电转换效率并降低其成本,二是要实现太阳能发电同的电网联网。对于提高转换效率和降低成本,例如,黑硅、PERC、半片、叠瓦技术,以及高反射、导热胶膜及背板封装材料等等,业内技术人员不论从硅片技术、电流收集技术,还是辅材增益技术上,都在不断进行提质增效方面的创新研究。
光伏背板,作为位于光伏组件的背面,起着隔绝电池片以及封装胶膜材料与外界环境的作用,是光伏组件的背部遁甲。光伏背板直接与外部环境大面积接触,需具备优异的耐湿热老化、耐紫外辐照、耐高低温冲击、水汽阻隔性和电气绝缘性等,才能满足光伏组件长达25年的使用寿命要求。同时光伏背板的耐候性上来看,光伏背板耐候性越好,对光伏组件的长期稳定性保障越高,光伏组件使用寿命越长,光伏组件电站端平均度电成本越低。因而,家强光伏背板材料的耐候性,对降低太阳能发电的成本具有重要意义。
光伏背板包含无机类和高分子类,其中高分子类由于其在可靠性和工艺性方面的优势,占据90%以上的比例。高分子类光伏背板根据生产工艺不同又分为复合型、涂覆型和共挤型。复合型光伏背板多以PVF、PVDF等氟膜或PA、PO膜,通过胶粘剂与PET基材粘结而成,其中以TPT、KPK、KPF等最为常见,已成为目前光伏背板产品的主要产品类型。然而,氟膜、PO膜均为非极性材料,表面能低,不仅浸润性差,与胶粘剂的粘结性也很差,故对胶粘剂的品质要求较高。光伏组件长期在户外应用,在服役过程中受温度和湿度双重个因素的综合影响,易发生胶粘剂水解失效,导致背板材料发层层间分层现象,从而降低了背板产品的耐候性以及使用寿命。故而,对于复合型光伏背板,除了要关注各层材料的质量,粘结各层材料的胶粘剂也至关重要,需要得到更高重视。
有关复合型光伏背板的报道很多,多数关注背板结构中的各层材料匹配性和功能性,诸如CN104494266A、CN104512082A、CN205069653U、CN104842616A、CN101350370A、CN102208465A、CN104494263A等专利,其内容涉及粘剂材料均很少,对于胶粘剂的可靠性研究更少。
因此,开发出一类高质量的复合型背板用绝缘胶粘剂材料,使其具有优异的粘结性能,同时在耐湿热性能、绝缘性能和耐老化等性能方面也具有优异的长期稳定性,是高质量的复合型光伏背板结构中需要解决的重要课题。
发明内容
本发明的目的是为了弥补现有技术的不足,提供一种复合型光伏背板用绝缘胶粘剂材料及应用,这种胶粘材料内部具有致密交联结构,在粘结性、耐湿热性、绝缘性、耐候性方面均具有优异的性能,同时在耐紫外性能、耐冷热性能和内聚性能等方面也表现优异,可以满足复合型光伏背板的长期可靠性要求。
本发明的目的是通过以下技术方案实现的:一种复合型光伏背板用绝缘胶粘剂材料,由A组分和B组分以重量比为3~20:1的比例混合组成;其中,A组分包含60%~99wt%的主体树脂、1~40wt%的辅助树脂及0~10wt%的助剂,B组分为交联组分;
所述主体树脂为含羟基聚酯树脂,其羟值为5~30mgKOH/g,酸值为0.2~5mgKOH/g,数均分子量为5000~50000,玻璃化转变温度为-40℃~30℃,在惰性气体保护下由多元酸与多元醇经酯化缩聚反应制备而成;
所述辅助树脂由聚己内酯二元醇、聚碳酸酯二元醇、聚丙交酯二元醇、聚己内酯二元醇、聚醚二元醇、聚氧化乙烯二元醇、聚丁二烯二元醇、氢化聚丁二烯二元醇、聚四氢呋喃二元醇、己二酸系聚酯二元醇、癸二酸系聚酯二元醇、双酚A型环氧树脂、氢化双酚A型环氧树脂、双酚F型环氧树脂、脂肪族缩水甘油醚型环氧树脂、缩水甘油酯型环氧树脂中的一种或多种按照任意配比组成;
所述助剂由40~99wt%水解稳定剂、0~20wt%无机填料、0~20wt%紫外助剂、1~20wt%抗热氧老化剂、0~20wt%催化剂A组成;
所述B组分由六亚甲基二异氰酸酯三聚体、六亚甲基二异氰酸酯预聚物、异佛尔酮二异氰酸酯三聚体、异佛尔酮二异氰酸酯预聚物、氢化苯二亚甲基异氰酸酯三聚体、氢化苯二亚甲基异氰酸酯预聚物、甲醚化多羟甲基三聚氰胺树脂、丁醚化多羟甲基三聚氰胺树脂、混醚化多羟甲基三聚氰胺树脂、聚酰胺、聚亚甲基二胺、二乙烯三胺、五甲基二乙烯三胺、三乙烯四胺、二乙撑三胺、三乙撑四胺、(2、3-二甲基)二亚丁基三胺的一种或多种按照任意配比组成。
进一步地,所述在惰性气体保护下由多元酸与多元醇经酯化缩聚反应制备而成具体为:
(1)在配有温度计、回流冷凝管、减压蒸馏器、搅拌器、油水分离器的反应釜中,首先经若干次抽真空通惰性气体过程,将反应釜内部更换成惰性气体氛围;然后边通惰性气体,边将反应釜升温至100~150℃后,打开冷凝水和搅拌器;
(2)边搅拌边将称量好的多元醇加入到反应釜中,保温30~60分钟后,再依次将多元酸、催化剂B缓慢加入到反应釜中,其中,多元醇的羟基与多元酸的羧基的摩尔比为1.01~1.5:1,催化剂B用量为多元醇和多元酸总质量的0.01%~0.50%;
(3)以5~15℃/小时的升温速度,升温至180~200℃;再以2~8℃/小时的升温速度,缓慢升温至230~260℃,保温反应20~26小时,直至无水分从油水分离器滴下;
(4)于惰性气体保护下,称取多元醇和多元酸总质量的0.005~0.50%催化剂B加入反应釜中,开启真空泵,抽真空10~15小时,直至无水分抽出;
(5)搅拌,自然冷却至140~160℃后,出料,制备得到含羟基聚酯树脂。
进一步地,所述水解稳定剂由碳化二亚胺类水解稳定剂、噁唑啉类水解稳定剂、环氧类水解稳定剂中的一种或多种按任意配比混合组成;所述无机填料由粒径为0.1um~1.0um的湿法云母粉、滑石粉、煅烧高岭土、氧化锌、蒙脱土、氮化硼、钛白粉中的一种或多种按任意配比混合组成;所述紫外助剂由2-羟基-4-甲氧基二苯甲酮、2-羟基-4-正辛氧基二苯甲酮、2,4-二羟基二苯甲酮、2,2,4-三羟基二苯甲酮、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯代苯并三氮唑、2-(2’-羟基-3’,5’-二叔丁基-5’-甲基苯基)-5-氯代苯并三氮唑、3-[3-(2-H-苯并三唑-2-基)-4-羟基-5-叔丁基苯基]-丙酸-聚乙二醇酯、2-(2’-羟基-5'-叔辛基)-苯并三唑、2,2’-亚甲基-(6-(2H-苯并三唑)-4-叔辛基)苯酚、2-(2H-苯并三唑-2-基)-6-十二烷基-4-甲基苯酚、2-(2’-羟基-5’-叔辛基苯基)苯并三唑、2-(4,6-双(2,4-二甲基苯基)-1,3,5-三嗪-2-基)-5-辛氧基酚、2-[4-[2-羟基-3-十三烷氧基丙基]氧基]-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-[4-[2-羟基-3-十二烷氧基丙基]氧基]-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、双(1,2,2,6,6-五甲基-4-哌啶基)-癸二酸酯/单(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯复配物、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、聚{[6-[(1,1,3,3-四甲基丁基)氨基]]-1,3,5-三嗪-2,4-[(2,2,6,6,-四甲基-哌啶基)亚氨、双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、2,2,6,6-四甲基-4-哌啶硬脂酸酯、聚丁二酸(4-羟基-2,2,6,6-四甲基-1-哌啶乙醇)酯、N-(2-乙氧基苯基)-N’-(4-乙基苯基)乙二酰胺、N-(4-苯甲酸乙酯)-N’,N’-(甲基,苯基)甲脒中的一种或多种按任意配比混合组成;所述抗热氧老化剂由四(3,5-二叔丁基-4-羟基)苯丙酸季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、2’-亚甲基双-(4-甲基-6-叔丁基苯酚)、1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯、2,6-二叔丁基-4-甲基苯酚、4,4’-二异丙苯基二苯胺、β-十二烷基硫代丙酸季戊四醇酯、三乙二醇醚-二(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯、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、亚磷酸三(2,4-二叔丁基苯基)酯、双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯、3,9-双十八烷氧基-2,4,8,10-四氧-3,9-二磷螺环[5,5]十一烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、4,4’-对开异丙基二苯基C12-15-醇亚磷酸酯中的一种或多种按任意配比混合组成;所述催化剂A由二甲氨基乙基醚、辛酸亚锡、二月桂酸二辛基锡、氧化单丁基锡、单丁基三异辛酸锡、二月桂酸二丁基锡、醋酸、对甲苯磺酸、邻苯二甲酸、月桂酸、异辛酸中的一种或多种按任意配比混合组成。
进一步地,所述多元醇由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇、1,9-壬二醇、1,10-癸二醇、新戊二醇、异戊二醇、季戊二醇、季戊四醇、2-甲基-2,4-戊二醇、2-乙基-2-羟甲基-1,3-丙二醇、2-甲基-2-羟甲基-1,3-丙二醇、二乙二醇、一缩二乙二醇、三乙二醇、二缩三乙二醇中的一种或多种按任意配比混合组成。
进一步地,所述多元酸由间苯二甲酸、邻苯二甲酸、对苯二甲酸、草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二酸、月桂二酸、甲基丁二酸、3-异丁基戊二酸、3-乙基-3-甲基戊二酸中的一种或多种按任意配比混合组成。
6.根据权利要求2所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述催化剂B由对甲苯磺酸、辛酸亚锡、氯化亚锡、二月桂酸二辛基锡、氧化单丁基锡、单丁基三异辛酸锡、二月桂酸二丁基锡、丁基锡酸、钛酸四正丁酯、钛酸四异丙酯、四异丁基钛酸酯、乙二醇锑、三氧化二锑、醋酸锌、醋酸锑中的一种或多种按任意配比混合组成。
进一步地,所述绝缘胶粘剂材料用于聚对苯二甲酸乙二醇酯薄膜、聚偏氟乙烯薄膜、聚氟乙烯薄膜、聚烯烃薄膜、聚乙烯醋酸乙烯酯膜、聚酰胺薄膜之间相互粘结,制备复合型光伏背板。
进一步地,该应用具体为:使用时,将A组分溶解于酯类或酮类溶剂中配制成固含量为48-52wt%的溶液,B组分溶解于酯类或酮类溶剂配制成固含量为68-72wt%的溶液,A组分和B组分以重量比为3~20:1的比例混合,均匀涂覆在被粘接材料表面,施胶量为3-15g/m2,固化温度40-60℃,固化时间2-4天。
本发明所用原料均可市购获得。
本发明的有益效果主要体现在:通过胶水配方体系优化,制备出一种具有强粘结性、高绝缘性及优异耐候性的复合型光伏背板用胶粘剂材料。该胶粘剂体系为交联结构,内聚能较高,不易发生内部断裂,有效保证了光伏背板在使用过程中多层材料一体化结构。胶粘剂绝缘性较高,具有高的体积电阻率、耐漏电起痕指数及绝缘距离,可满足1500V或更高电压光伏背板的需求。另外,该绝缘胶粘剂还在热稳定性、耐湿热老化、耐紫外老化、耐冷热冲击等方面具有优异的综合性能,能够在严苛的户外环境中保持稳定的粘结强度和耐候性,为复合型光伏及相应光伏组件的长期可靠性提供保障。
具体实施方式
下面结合实施例对本发明作进一步描述,但本发明的保护范围不仅局限于实施例。
在本发明实施例中,胶粘剂所粘结的材料为厚度为250μm PET和厚度为25μm的PVDF。
需要说明的是,绝缘胶粘剂及复合型光伏背板的各项性能指标是通过以下的方法来进行测定的:
1.粘结强度
测试方法参照标准GB/T 2790《绝缘胶粘剂180°剥离强度试验方法挠性材料对刚性材料》。
试样尺寸:300mm*10mm。
拉伸速度:100mm/min。
2.表面电阻率
测试方法参照标准GB/T 1410《材料体积电阻率和表面电阻率试验方法》。
试样尺寸:100mm*100mm。
测试条件:测试电压1500V。
3.相对漏电起痕指数
测试方法参照标准GB/T 4207《固体绝缘材料耐电痕化指数和相比电痕化指数的测定方法》。
试验条件:23℃,相对湿度50%。
4.绝缘距离
测试方法参照标准IEC 62788-2《Measurement Procedures for Materials usedin Photovoltaic
Modules–Part 2:Polymeric materials–Frontsheets and backsheets》。
试验条件:23℃,相对湿度50%。
5.恒定耐湿热老化性能
测试方法参照标准GB/T 2423.3《高低温湿热试验方法》。
试验条件:+85℃,相对湿度85%。
试验前、后对试样黄变指数(ΔYI)按国标GB 2409《塑料黄色指数试验方法》测定。
6.紫外老化性能
测试方法参照标准GB/T 19394《光伏(PV)组件紫外试验》。
试验条件:表面温度为60℃,340nm&1.2W/m2。
7.冷热冲击性能
测试方法参照标准GB/T 2423.3《高低温湿热试验方法》。
试验条件:-40℃-+85℃,相对湿度85%。
8.热老化性能
样品放置于150℃烘箱内老化48h。
实施例1:
(1)制备绝缘胶粘剂:
在惰性气体氛围反应釜中,于150℃边搅拌边缓慢边加入称量好的多元醇,包含520.75g的新戊二醇(井冈化工有限公司)、104.15g的1,5-戊二醇(井冈化工有限公司)、73.12g的1,8-辛二醇(丽盛化工有限公司),保温30分钟后,再依次将多元酸包含664.52g的间苯二甲酸(佰仟化工有限公司)、332.26g的邻苯二甲酸(佰仟化工有限公司)、99.03g的月桂二酸(金宇化工有限公司)和0.18g的催化剂钛酸四正丁酯(宏明化学试剂有限公司)缓慢加入到反应釜中;以5℃/小时的升温速度,升温至180℃;再以2℃/小时的升温速度,缓慢升温至230℃,保温反应26小时;称0.18g的催化剂钛酸四正丁酯(宏明化学试剂有限公司)加入反应釜中,开启真空泵,真空度保持-0.1MPa抽真空10小时后,停止加热和抽真空,边搅拌自然冷却至140℃后,出料,得到含羟基聚酯树脂。测得酸值为0.2mgKOH/g,羟值为5mg KOH/g,数均分子量为12700,玻璃化转变温度为-34℃。
A组分包含60wt%的羟基聚酯树脂、20wt%的聚四亚甲基醚二醇(日本三菱)、20wt%的双酚A型环氧树脂(艾迪森化工有限公司);B组分包含80wt%的聚酰胺(美国杜邦公司)和20wt%的三乙撑四胺(晶沪化工有限公司);将A组分配制成50±2%的乙酸乙酯溶液,B组分配制成70±2%的乙酸乙酯溶液,备用。
(2)制备复合型光伏背板样品:
将配制成溶液的A、B组分按3:1比例进行预先混合并搅拌均匀,在PET表面通过自动化连续成型或间歇式工艺均匀涂覆上克重为6g/m2干胶含量的胶粘剂5μm,待溶剂挥发干燥后,贴合上PVDF膜,放入烘房内,在40℃,静置固化96h后,样品制备完成。
实施例2:
(1)制备绝缘胶粘剂:
在惰性气体氛围反应釜中,于100℃边搅拌边缓慢边加入称量好的多元醇,包含520.75g的季戊二醇(井冈化工有限公司)、67.09g的2-乙基-2-羟甲基-1,3-丙二醇(名成化工有限公司)、120.15g的2-甲基-2-羟甲基-1,3-丙二醇(名成化工有限公司)、152.18g的1,3-丙二醇(广丰化工有限公司),保温60分钟后,再依次将多元酸包含664.52g的对苯二甲酸(佰仟化工有限公司)、155.51g的癸二酸(金宇化工有限公司)、132.12g的甲基丁二酸和9.06g的催化剂氧化单丁基锡(澣思化工有限公司)缓慢加入到反应釜中;以15℃/小时的升温速度,升温至200℃;再以8℃/小时的升温速度,缓慢升温至260℃,保温反应20小时;称0.09g的催化剂氧化单丁基锡(澣思化工有限公司)加入反应釜中,开启真空泵,真空度保持-0.1MPa抽真空15小时后,停止加热和抽真空,边搅拌自然冷却至160℃后,出料,得到含羟基聚酯树脂。测得酸值为3.0mgKOH/g,羟值为30mg KOH/g,数均分子量为43000,玻璃化转变温度为30℃。
A组分包含80wt%的羟基聚酯树脂、5wt%的聚己二酸丁二醇酯二元醇(誉宇新材料科技有限公司)、5wt%的聚碳酸酯二元醇(华凯树脂有限公司)、10wt%的苯基缩水甘油醚水解稳定剂(弘裕化工有限公司);B组分包含60wt%的异佛尔酮二异氰酸酯三聚体(德国拜耳公司)和40wt%的氢化苯二亚甲基异氰酸酯预聚物(德国拜耳公司);将A组分配制成50±2%的乙酸丁酯溶液,B组分配制成70±2%的乙酸乙酯溶液,备用。
(2)制备复合型光伏背板样品:
将配制成溶液的A、B组分按20:1比例进行预先混合并搅拌均匀,在PET表面通过自动化连续成型或间歇式工艺均匀涂覆上克重为3g/m2干胶含量的胶粘剂3μm,待溶剂挥发干燥后,贴合上PVDF膜,放入烘房内,在60℃,静置固化40h后,样品制备完成。
实施例3:
(1)制备绝缘胶粘剂:
在惰性气体氛围反应釜中,于140℃边搅拌边缓慢边加入称量好的多元醇,包含520.75g的新戊二醇(井冈化工有限公司)、354.51g的1,6-己二醇(广丰化工有限公司)、40.25g的2-乙基-2-羟甲基-1,3-丙二醇(名成化工有限公司),保温40分钟后,再依次将多元酸包含664.52g的邻苯二甲酸(佰仟化工有限公司)、332.26g的对苯二甲酸(佰仟化工有限公司)、141.58g的癸二酸(海力化工股份有限公司)、164.60g的戊二酸(海力化工股份有限公司)和6.09g的催化剂三氧化二锑(上海新典化学材料有限公司)缓慢加入到反应釜中;以10℃/小时的升温速度,升温至170℃;再以5℃/小时的升温速度,缓慢升温至240℃,保温反应23小时;称5.89g的催化剂三氧化二锑(上海新典化学材料有限公司)缓加入反应釜中,开启真空泵,真空度保持-0.1MPa抽真空12小时后,停止加热和抽真空,边搅拌自然冷却至140℃后,出料,得到含羟基聚酯树脂。测得酸值为1.3mgKOH/g,羟值为24mg KOH/g,数均分子量为21400,玻璃化转变温度为-30℃。
A组分包含99wt%的羟基聚酯树脂、1wt%的氢化聚丁二烯二元醇(德国巴斯夫公司);B组分为含氢化苯二亚甲基异氰酸酯三聚体(德国拜耳公司);将A组分配制成50±2%的丁酮溶液,B组分配制成70±2%的乙酸丁酯溶液,备用。
(2)制备复合型光伏背板样品:
将配制成溶液的A、B组分按8:1比例进行预先混合并搅拌均匀,在PET表面通过自动化连续成型或间歇式工艺均匀涂覆上克重为15g/m2干胶含量的胶粘剂13μm,待溶剂挥发干燥后,贴合上PVDF膜,放入烘房内,在50℃,静置固化48h后,样品制备完成。
实施例4:
(1)制备绝缘胶粘剂:
在惰性气体氛围反应釜中,于120℃边搅拌边缓慢边加入称量好的多元醇,包含680.75g的季戊四醇(井冈化工有限公司)、73.16g的1,8-辛二醇(丽盛化工有限公司)、38.05g的1,3-丙二醇(广丰化工有限公司)、101.13g的1,10-癸二醇(丽盛化工有限公司),保温50分钟后,再依次将多元酸包含378.21g的草酸、230.30g的月桂二酸(金宇化工有限公司)、193.65g的戊二酸(海力化工股份有限公司)和5.09g催化剂二月桂酸二辛基锡(九邦化工有限公司)缓慢加入到反应釜中;以5℃/小时的升温速度,升温至190℃;再以5℃/小时的升温速度,缓慢升温至250℃,保温反应24小时;称3.10g催化剂二月桂酸二辛基锡(九邦化工有限公司)加入反应釜中,开启真空泵,真空度保持-0.1MPa抽真空14小时后,停止加热和抽真空,边搅拌自然冷却至150℃后,出料,得到含羟基聚酯树脂。测得酸值为5mgKOH/g,羟值为28mg KOH/g,数均分子量为5000,玻璃化转变温度为-40℃。
A组分包含70wt%的羟基聚酯树脂、8wt%的聚己内酯二元醇(日本大赛璐公司)、12wt%的脂肪族缩水甘油醚型环氧树脂(惠峰合成材料有限公司)、4wt%的水解稳定剂I型(德国莱茵化学)、2wt%的钛白粉CR-60-2(日本石原公司)、2wt%的2-[4-[2-羟基-3-十二烷氧基丙基]氧基]-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪(台湾双键化学公司)、1wt%的亚磷酸三(2,4-二叔丁基苯基)酯(台湾永光化学公司)、1wt%的对甲苯磺酸(飞歌化学有限公司);B组分包含70wt%的丁醚化多羟甲基三聚氰胺树脂(金水源化工有限公司)和30wt%的二乙烯三胺(晶沪化工有限公司);将A组分配制成50±2%的乙酸乙酯溶液,B组分配制成70±2%的乙酸丁酯溶液,备用。
(2)制备复合型光伏背板样品:
将配制成溶液的A、B组分按9:1比例进行预先混合并搅拌均匀,在PET表面通过自动化连续成型或间歇式工艺均匀涂覆上克重为8g/m2干胶含量的胶粘剂7μm,待溶剂挥发干燥后,贴合上PVDF膜,放入烘房内,在50℃,静置固化60h后,样品制备完成。
实施例5:
(1)制备绝缘胶粘剂:
在惰性气体氛围反应釜中,于140℃边搅拌边缓慢边加入称量好的多元醇,包含371.6g的乙二醇(广丰化工有限公司)、36.05g的2-乙基-2-羟甲基-1,3-丙二醇(名成化工有限公司)、202.25g的1,10-癸二醇、150.18g的二缩三乙二醇(名成化工有限公司),保温30分钟后,再依次将多元酸包含664.52g的邻苯二甲酸(佰仟化工有限公司)、178.81g的3-异丁基戊二酸(茜泾化工有限公司)、438.42g的己二酸(海力化工股份有限公司)和4.50g的催化剂四异丁基钛酸酯(宏明化学试剂有限公司)缓慢加入到反应釜中;以10℃/小时的升温速度,升温至170℃;再以5℃/小时的升温速度,缓慢升温至240℃,保温反应26小时;称4.50g的催化剂四异丁基钛酸酯(宏明化学试剂有限公司)加入反应釜中,开启真空泵,真空度保持-0.1MPa抽真空12小时后,停止加热和抽真空,边搅拌自然冷却至120℃后,出料,得到含羟基聚酯树脂。测得酸值为0.5mgKOH/g,羟值为18mg KOH/g,数均分子量为50000,玻璃化转变温度为5℃。
A组分包含80wt%的羟基聚酯树脂、6wt%的聚亚丁基醚二醇(晓星化工有限公司)、4wt%的聚四氢呋喃二元醇(日本三菱公司)、9.9wt%的聚(2-乙基-2-噁唑啉)(昊睿化学有限公司)、0.1wt%的双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯(德国巴斯夫公司);B组分包含60wt%的六亚甲基二异氰酸酯三聚体(日本聚氨酯公司)和40wt%的氢化苯二亚甲基异氰酸酯三聚体(德国拜耳公司);将A组分配制成50±2%的丁酮溶液,B组分配制成70±2%的丙酮溶液,备用。
(2)制备复合型光伏背板样品:
将配制成溶液的A、B组分按15:1比例进行预先混合并搅拌均匀,在PET表面通过自动化连续成型或间歇式工艺均匀涂覆上克重为10g/m2干胶含量的胶粘剂10μm,待溶剂挥发干燥后,贴合上PVDF膜,放入烘房内,在55℃,静置固化72h后,样品制备完成。
比较例1:
市场上购得光伏背板KPK,结构为PVDF/胶粘剂/PET/胶粘剂/PVDF,胶粘剂厚度10μm,总厚度320μm。
对实施例1、2、3、4、5制得的胶粘剂及制备的复合型光伏背板以及比较例1的光伏背板进行性能检测,结果如表1所示。
表1:性能参数表格
由表中数据可知,本发明绝缘胶粘剂,具有较高的初始粘结性,在湿热、紫外、冷热冲击、热严酷老化后粘结性的衰减较低,具有优异的保持率。另外,还具有很好的绝缘性和黄变性能,能不仅完全满足复合型普通光伏背板的使用要求,还能满足1500V或更高电压光伏背板的需求。本发明原料易得,工艺可控,操作简便,产品质量批次性稳定,不仅为复合型光伏背板的各层材料长期一体化提供保障,而且为光伏背板更长寿命的户外应用提供了重要技术支持。
Claims (10)
1.一种复合型光伏背板用绝缘胶粘剂材料,由A组分和B组分以重量比为3~20:1的比例混合组成;其中,A组分包含60%~99wt%的主体树脂、1~40wt%的辅助树脂和0~10wt%的助剂等,B组分为交联组分。
所述主体树脂为含羟基聚酯树脂,其羟值为5~30mgKOH/g,酸值为0.2~5mgKOH/g,数均分子量为5000~50000,玻璃化转变温度为-40℃~30℃,在惰性气体保护下由多元酸与多元醇经酯化缩聚反应制备而成。
所述辅助树脂由聚己内酯二元醇、聚碳酸酯二元醇、聚丙交酯二元醇、聚己内酯二元醇、聚醚二元醇、聚氧化乙烯二元醇、聚丁二烯二元醇、氢化聚丁二烯二元醇、聚四氢呋喃二元醇、己二酸系聚酯二元醇、癸二酸系聚酯二元醇、双酚A型环氧树脂、氢化双酚A型环氧树脂、双酚F型环氧树脂、脂肪族缩水甘油醚型环氧树脂、缩水甘油酯型环氧树脂中的一种或多种按照任意配比组成。
所述助剂由40~99wt%水解稳定剂、0~20wt%无机填料、0~20wt%紫外助剂、1~20wt%抗热氧老化剂、0~20wt%催化剂A组成。
所述B组分由六亚甲基二异氰酸酯三聚体、六亚甲基二异氰酸酯预聚物、异佛尔酮二异氰酸酯三聚体、异佛尔酮二异氰酸酯预聚物、氢化苯二亚甲基异氰酸酯三聚体、氢化苯二亚甲基异氰酸酯预聚物、甲醚化多羟甲基三聚氰胺树脂、丁醚化多羟甲基三聚氰胺树脂、混醚化多羟甲基三聚氰胺树脂、聚酰胺、聚亚甲基二胺、二乙烯三胺、五甲基二乙烯三胺、三乙烯四胺、二乙撑三胺、三乙撑四胺、(2、3-二甲基)二亚丁基三胺的一种或多种按照任意配比组成。
2.根据权利要求1所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述在惰性气体保护下由多元酸与多元醇经酯化缩聚反应制备而成具体为:
(1)在配有温度计、回流冷凝管、减压蒸馏器、搅拌器、油水分离器的反应釜中,首先经若干次抽真空通惰性气体过程,将反应釜内部更换成惰性气体氛围;然后边通惰性气体,边将反应釜升温至100~150℃后,打开冷凝水和搅拌器。
(2)边搅拌边将称量好的多元醇加入到反应釜中,保温30~60分钟后,再依次将多元酸、催化剂B缓慢加入到反应釜中,其中,多元醇的羟基与多元酸的羧基的摩尔比为1.01~1.5:1,催化剂B用量为多元醇和多元酸总质量的0.01%~0.50%。
(3)以5~15℃/小时的升温速度,升温至180~200℃;再以2~8℃/小时的升温速度,缓慢升温至230~260℃,保温反应20~26小时,直至无水分从油水分离器滴下。
(4)于惰性气体保护下,称取多元醇和多元酸总质量的0.005~0.50%催化剂B加入反应釜中,开启真空泵,抽真空10~15小时,直至无水分抽出。
(5)搅拌,自然冷却至140~160℃后,出料,制备得到含羟基聚酯树脂。
3.根据权利要求1所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述水解稳定剂由碳化二亚胺类水解稳定剂、噁唑啉类水解稳定剂、环氧类水解稳定剂中的一种或多种按任意配比混合组成;所述无机填料由粒径为0.1um~1.0um的湿法云母粉、滑石粉、煅烧高岭土、氧化锌、蒙脱土、氮化硼、钛白粉中的一种或多种按任意配比混合组成;所述紫外助剂由2-羟基-4-甲氧基二苯甲酮、2-羟基-4-正辛氧基二苯甲酮、2,4-二羟基二苯甲酮、2,2,4-三羟基二苯甲酮、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯代苯并三氮唑、2-(2’-羟基-3’,5’-二叔丁基-5’-甲基苯基)-5-氯代苯并三氮唑、3-[3-(2-H-苯并三唑-2-基)-4-羟基-5-叔丁基苯基]-丙酸-聚乙二醇酯、2-(2’-羟基-5'-叔辛基)-苯并三唑、2,2’-亚甲基-(6-(2H-苯并三唑)-4-叔辛基)苯酚、2-(2H-苯并三唑-2-基)-6-十二烷基-4-甲基苯酚、2-(2’-羟基-5’-叔辛基苯基)苯并三唑、2-(4,6-双(2,4-二甲基苯基)-1,3,5-三嗪-2-基)-5-辛氧基酚、2-[4-[2-羟基-3-十三烷氧基丙基]氧基]-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-[4-[2-羟基-3-十二烷氧基丙基]氧基]-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、双(1,2,2,6,6-五甲基-4-哌啶基)-癸二酸酯/单(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯复配物、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、聚{[6-[(1,1,3,3-四甲基丁基)氨基]]-1,3,5-三嗪-2,4-[(2,2,6,6,-四甲基-哌啶基)亚氨、双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、2,2,6,6-四甲基-4-哌啶硬脂酸酯、聚丁二酸(4-羟基-2,2,6,6-四甲基-1-哌啶乙醇)酯、N-(2-乙氧基苯基)-N’-(4-乙基苯基)乙二酰胺、N-(4-苯甲酸乙酯)-N’,N’-(甲基,苯基)甲脒中的一种或多种按任意配比混合组成。
4.根据权利要求1所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述抗热氧老化剂由四(3,5-二叔丁基-4-羟基)苯丙酸季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、2’-亚甲基双-(4-甲基-6-叔丁基苯酚)、1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯、2,6-二叔丁基-4-甲基苯酚、4,4’-二异丙苯基二苯胺、β-十二烷基硫代丙酸季戊四醇酯、三乙二醇醚-二(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯、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、亚磷酸三(2,4-二叔丁基苯基)酯、双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯、3,9-双十八烷氧基-2,4,8,10-四氧-3,9-二磷螺环[5,5]十一烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、4,4’-对开异丙基二苯基C12-15-醇亚磷酸酯中的一种或多种按任意配比混合组成。
5.根据权利要求1所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述催化剂A由二甲氨基乙基醚、辛酸亚锡、二月桂酸二辛基锡、氧化单丁基锡、单丁基三异辛酸锡、二月桂酸二丁基锡、醋酸、对甲苯磺酸、邻苯二甲酸、月桂酸、异辛酸中的一种或多种按任意配比混合组成。
6.根据权利要求2所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述多元醇由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇、1,9-壬二醇、1,10-癸二醇、新戊二醇、异戊二醇、季戊二醇、季戊四醇、2-甲基-2,4-戊二醇、2-乙基-2-羟甲基-1,3-丙二醇、2-甲基-2-羟甲基-1,3-丙二醇、二乙二醇、一缩二乙二醇、三乙二醇、二缩三乙二醇中的一种或多种按任意配比混合组成。
7.根据权利要求2所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述多元酸由间苯二甲酸、邻苯二甲酸、对苯二甲酸、草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二酸、月桂二酸、甲基丁二酸、3-异丁基戊二酸、3-乙基-3-甲基戊二酸中的一种或多种按任意配比混合组成。
8.根据权利要求2所述的复合型光伏背板用绝缘胶粘剂材料,其特征在于,所述催化剂B由对甲苯磺酸、辛酸亚锡、氯化亚锡、二月桂酸二辛基锡、氧化单丁基锡、单丁基三异辛酸锡、二月桂酸二丁基锡、丁基锡酸、钛酸四正丁酯、钛酸四异丙酯、四异丁基钛酸酯、乙二醇锑、三氧化二锑、醋酸锌、醋酸锑中的一种或多种按任意配比混合组成。
9.一种权利要求1所述的复合型光伏背板用绝缘胶粘剂材料的应用,其特征在于,所述绝缘胶粘剂材料用于聚对苯二甲酸乙二醇酯薄膜、聚偏氟乙烯薄膜、聚氟乙烯薄膜、聚烯烃薄膜、聚乙烯醋酸乙烯酯膜、聚酰胺薄膜之间相互粘结,制备复合型光伏背板。
10.根据权利要求9所述的复合型光伏背板用绝缘胶粘剂材料的应用,其特征在于,该应用具体为:使用时,将A组分溶解于酯类或酮类溶剂中配制成固含量为48-52wt%的溶液,B组分溶解于酯类或酮类溶剂配制成固含量为68-72wt%的溶液,A组分和B组分以重量比为3~20:1的比例混合,均匀涂覆在被粘接材料表面,施胶量约为3-15g/m2,固化温度约为40-60℃,固化时间约为2-4天。
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