CN116855209A - 一种阻燃uv固化高分子粘合剂 - Google Patents
一种阻燃uv固化高分子粘合剂 Download PDFInfo
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- CN116855209A CN116855209A CN202310951225.4A CN202310951225A CN116855209A CN 116855209 A CN116855209 A CN 116855209A CN 202310951225 A CN202310951225 A CN 202310951225A CN 116855209 A CN116855209 A CN 116855209A
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Abstract
本发明涉及粘合剂技术领域,具体涉及一种阻燃UV固化高分子粘合剂,所述高分子粘合剂包含如下重量份组分:20‑30份氢氧化铝、40‑60份聚氨酯改性树脂、50‑70份环氧树脂、10‑20份改性丙烯酸活性单体、5‑10份光敏固化剂、3‑6份疏水性气相二氧化硅、1‑3份光引发剂、0.1‑0.5份助引发剂、1‑3份阻燃剂、40‑60份溶剂。本发明中,通过添加制备的聚氨酯改性树脂,可以提升高分子粘合剂体系的交联密度,使得粘合剂的粘结性能得到显著提升,使其具有高粘合性能,同时,配合添加的阻燃剂,有助于提高粘合剂的耐热性,使其在高温甚至燃烧状态下,依然可以与基材之间形成很好的粘合性,从而使得高分子粘合剂具有优异的阻燃以及高粘结性能,具有广泛的应用前景。
Description
技术领域
本发明涉及粘合剂技术领域,具体为一种阻燃UV固化高分子粘合剂。
背景技术
随着科技的发展,手机、笔记本电脑、平板电脑、超薄电视、导航仪等产品迅速发展,对电声器件的需求越来越大。而传统工艺中,电声器件的生产,主要靠溶剂胶来粘结支架、膜片及音圈等部件,但溶剂胶毒性大、对人体有害,很难满足无毒等新要求,且性能不稳定。
现有技术中,UV固化材料中的光引发剂(或光敏剂)在紫外线的照射下,吸收紫外光后产生活性自由基或阳离子,引发单体聚合、交联和节支化学反应,使粘合剂由液态转化为固态。例如公告号为CN113563807A的发明专利公开了一种可控UV固化型光学粘合剂及其制备方法,该光学粘合剂由0-80份的丙烯酸酯类烷基单体、0-30份的丙烯酸酯类烷基单体、0-10份的丙烯酸酯类烷基单体和0-0.1份的光引发剂组成,制成的光学粘合剂的固化率可以根据不同的需求进行控制,可以适用于不同的固化率的需求,但是该光学粘合剂的粘合强度一般,只能应用于小体积的电子产品的粘合中,对于一些大体积的基材,不能实现良好的界面结合强度,而且该光学粘合剂的耐热性较差,在高温甚至燃烧状态下,则无法正常使用。
发明内容
针对现有技术中存在的问题,本发明的目的在于提供一种阻燃UV固化高分子粘合剂。
为实现上述目的,本发明提供如下技术方案:
一种阻燃UV固化高分子粘合剂,所述高分子粘合剂包含如下重量份组分:20-30份氢氧化铝、40-60份聚氨酯改性树脂、50-70份环氧树脂、10-20份改性丙烯酸活性单体、5-10份光敏固化剂、3-6份疏水性气相二氧化硅、1-3份光引发剂、0.1-0.5份助引发剂、1-3份阻燃剂、40-60份溶剂;
所述光敏固化剂为安息香双甲醚;
所述光引发剂为阳离子型UV光引发剂;
所述助引发剂为2-异丙基硫杂蒽酮;
所述阻燃剂为磷系阻燃剂;
所述溶剂选自环己酮、乙酸乙酯、丁酸丁酯中至少一种。
作为本发明的进一步优选方案,所述改性丙烯酸活性单体是以含端烯基的硅烷偶联剂对丙烯酸进行改性得到;
其中,含端烯基的硅烷偶联剂为甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷中任意一种。
作为本发明的进一步优选方案,所述聚氨酯改性树脂的制备方法如下:
1)将环氧衣康酸酯树脂的异丙醇溶液加入到容器中,加入卡斯特催化剂,搅拌均匀后加热至70-75℃,之后缓慢加入端氢基聚硅氧烷,在90-95℃下恒温反应8-10h,待反应结束后,减压蒸馏回收溶剂,得到改性环氧衣康酸酯树脂;
2)将改性环氧衣康酸酯树脂和封端异氰酸酯加入到丙酮中,充分搅拌后,在56-60℃下回流反应3-6h,待反应结束后,滴加蒸馏水稀释至固含量50-60%,以2000-5000r/min搅拌30-50min,经减压蒸馏回收溶剂,得到水分散体;
3)将木质素分散于水分散体中,超声分散6-8h后形成均匀分散体,然后加入改性聚氨酯乳液,充分混合均匀后静置2-5h,然后置于50-60℃烘箱中干燥固化30-50min,再经120-130℃烘箱内干燥2-5h,即可得到所需的聚氨酯改性树脂。
作为本发明的进一步优选方案,所述环氧衣康酸酯树脂的异丙醇溶液、卡斯特催化剂、端氢基聚硅氧烷的用量比例为(10-20)g:(2-8)mg:(0.5-1.3)g;
所述环氧衣康酸酯树脂的异丙醇溶液中,固含量为62-68%。
作为本发明的进一步优选方案,所述改性环氧衣康酸酯树脂、封端异氰酸酯、丙酮的用量比例为(2-8)g:(3-10)g:(80-150)mL。
作为本发明的进一步优选方案,所述木质素、水分散体、改性聚氨酯乳液的用量比例为(3-8)g:(15-30)g:(60-100)mL。
作为本发明的进一步优选方案,所述改性聚氨酯乳液的制备方法如下:
1)将10-20g聚碳酸亚丙酯二醇和13-26g聚四氢呋喃醚二醇在真空条件下和110-115℃下脱水处理1-2h,然后溶于80-120mL二甲基甲酰胺中,搅拌下加入8-15g4,4'-二苯基甲烷二异氰酸酯,在68-73℃下反应50-70min,生成预聚体,然后向预聚体中加入20-30mL二甲基甲酰胺、8-15mL1,4-丁二醇和10-18mL1,6-己二醇,继续反应30-40min,形成浆料,备用;
2)将真空干燥后的蓖麻油和2-巯基乙醇混合,在氮气保护下,加入偶氮二异丁腈,先加热至80-86℃并反应4-6h,然后将温度调至100-110℃继续反应2-3h,冷却至室温后,加入乙酸乙酯,收集产物并用去离子水和盐水反复洗涤,干燥后除去乙酸乙酯,得到改性蓖麻油;
3)将改性蓖麻油和甘油加入到容器中,再加入氢氧化钠,混合均匀后升温至180-200℃,在氮气保护下反应1-2h,得到改性蓖麻油多元醇;
4)将改性蓖麻油多元醇加入到容器中,加入异氰酸酯,充分混合后加热至85-90℃,加入丙酮、浆料、2,2-二羟甲基丁酸以及二丁基锡二月桂酸,反应1-3h,然后加入丁二酮肟继续反应6-8h,然后加入三乙胺反应30-50min,待反应结束后,将产物倒出,然后缓慢多次的添加入等质量的去离子水,在20000-50000r/min下高速搅拌30-50min,即可形成所需的改性聚氨酯乳液。
作为本发明的进一步优选方案,所述蓖麻油、2-巯基乙醇、偶氮二异丁腈、乙酸乙酯的用量比例为(50-70)g:(10-16)g:(4-6)g:(50-80)g;
所述改性蓖麻油、甘油、氢氧化钠的质量比为(50-60):(9-12):(0.05-0.08)。
作为本发明的进一步优选方案,所述改性蓖麻油多元醇、异氰酸酯、丙酮、浆料,2,2-二羟甲基丁酸、二丁基锡二月桂酸、丁二酮肟、三乙胺的用量比例为(6-12)g:(30-40)g:(30-50)mL:(15-20)g:(1-2)g:(40-60)μL:(1-2)g:(2-5)g。
作为本发明的进一步优选方案,所述高分子粘合剂的制备方法包括如下步骤:
按照重量份数计,将聚氨酯改性树脂、环氧树脂以及改性丙烯酸活性单体充分混合,形成光学预聚物,将氢氧化铝、光敏固化剂、疏水性气相二氧化硅、光引发剂、助引发剂以及阻燃剂充分混合,形成助剂,将光学预聚物和助剂依次加入到溶剂中,充分混合均匀后,即可得到高分子粘合剂。
与现有技术相比,本发明的有益效果是:
本发明中,利用衣康酸与环氧树脂开环酯化制备环氧衣康酸酯树脂的基础上,通过硅氢加成接枝聚硅氧烷进一步改善了树脂韧性不足的缺陷,再与含甲基丙烯酰氧基的封端异氰酸酯接枝共聚以提高树脂光固化活性,制备了含有高活性聚硅氧烷改性环氧衣康酸酯树脂的水分散体,以期通过环氧树脂和有机硅两者优势互补,从而实现粘合层韧性的提升;同时,将制备的水分散体与木质素引入到配置的改性聚氨酯乳液中,木质素一方面可以作为填料,增加体系的交联密度,另一方面,木质素具有刚性苯环结构,可以作为聚氨酯的硬段,增加了聚氨酯的硬段含量,分子链段增加,分子间的作用力增强,同时,体系中刚性结构增多,聚集程度增加,链段间运动性降低,聚氨酯的有序结构破坏愈加困难,而且也限制了体系中分子链段滑移,有限延缓松弛行为的发生,从而可以显著提高粘合层的极限粘结强度,使得高分子粘合剂具有优异的粘结性能。
聚氨酯改性树脂中使用的改性聚氨酯乳液,是以聚碳酸亚丙酯二醇和二苯基甲烷二异氰酸酯为主要原料,采用预聚法制备形成的浆料,该浆料的分子间同时含有大量的醚键和碳酸酯键,分子内聚能高,具有很好的粘结强度,然后以蓖麻油、2-巯基乙醇和甘油为原料,通过酯交换和巯烯基点击反应,在蓖麻油分子链上引入羟基,使得改性蓖麻油多元醇含有更高的羟基值,且具有更强的分子间作用力,然后将改性蓖麻油多元醇与异氰酸酯进行合成,并加入制备的浆料,从而制得改性聚氨酯乳液;通过对蓖麻油进行改性后,增加了其羟基含量,同时蓖麻油分子链上的酯基使得聚氨酯内部基团之间的作用力更强,从而有助于提高聚合物的交联密度,从而使得粘合剂的粘结性能得到进一步的提升。
本发明中,通过添加制备的聚氨酯改性树脂,可以提升高分子粘合剂体系的交联密度,使得粘合剂的粘结性能得到显著提升,使其具有高粘合性能,同时,配合添加的阻燃剂,有助于提高粘合剂的耐热性,使其在高温甚至燃烧状态下,依然可以与基材之间形成很好的粘合性,从而使得高分子粘合剂具有优异的阻燃以及高粘结性能,具有广泛的应用前景。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
本发明实施例中,
改性丙烯酸活性单体是由丙烯酸与甲基丙烯酰氧基丙基三甲氧基硅烷按照质量比10:1充分搅拌均匀而制得;
光敏固化剂为安息香双甲醚;光引发剂为阳离子型UV光引发剂UVI-6976;助引发剂为2-异丙基硫杂蒽酮;阻燃剂为磷酸三(二甲苯)酯;溶剂为环己酮;
环氧树脂为中国石化集团巴陵石油化工有限责任公司生产的型号为CYD-011的环氧树脂;
疏水性气相二氧化硅为日本德山株式会社生产的型号为MT-10C的疏水性气相二氧化硅。
实施例1
一种阻燃UV固化高分子粘合剂,该高分子粘合剂包含如下重量份组分:20份氢氧化铝、40份聚氨酯改性树脂、50份环氧树脂、10份改性丙烯酸活性单体、5份光敏固化剂、3份疏水性气相二氧化硅、1份光引发剂、0.1份助引发剂、1份阻燃剂、40份溶剂;
该高分子粘合剂的制备方法包括如下步骤:
按照重量份数计,将聚氨酯改性树脂、环氧树脂以及改性丙烯酸活性单体充分混合,形成光学预聚物,将氢氧化铝、光敏固化剂、疏水性气相二氧化硅、光引发剂、助引发剂以及阻燃剂充分混合,形成助剂,将光学预聚物和助剂依次加入到溶剂中,充分混合均匀后,即可得到高分子粘合剂。
其中,聚氨酯改性树脂的制备方法如下:
1)将10g聚碳酸亚丙酯二醇和13g聚四氢呋喃醚二醇在真空条件下和110℃下脱水处理1h,然后溶于80mL二甲基甲酰胺中,搅拌下加入8g4,4'-二苯基甲烷二异氰酸酯,在68℃下反应50min,生成预聚体,然后向预聚体中加入20mL二甲基甲酰胺、8mL1,4-丁二醇和10mL1,6-己二醇,继续反应30min,形成浆料,备用;
2)将真空干燥后的50g蓖麻油和10g2-巯基乙醇混合,在氮气保护下,加入4g偶氮二异丁腈,先加热至80℃并反应4h,然后将温度调至100℃继续反应2h,冷却至室温后,加入50g乙酸乙酯,收集产物并用去离子水和盐水反复洗涤,干燥后除去乙酸乙酯,得到改性蓖麻油;
3)将50g改性蓖麻油和9g甘油加入到容器中,再加入0.05g氢氧化钠,混合均匀后升温至180℃,在氮气保护下反应1h,得到改性蓖麻油多元醇;
4)将6g改性蓖麻油多元醇加入到容器中,加入30g异氰酸酯,充分混合后加热至85℃,加入30mL丙酮、15g浆料、1g2,2-二羟甲基丁酸以及40μL二丁基锡二月桂酸,反应1h,然后加入1g丁二酮肟继续反应6h,然后加入2g三乙胺反应30min,待反应结束后,将产物倒出,然后缓慢多次的添加入等质量的去离子水,在20000r/min下高速搅拌30min,即可形成改性聚氨酯乳液;
5)将10g固含量为62%的环氧衣康酸酯树脂的异丙醇溶液加入到容器中,加入2mg卡斯特催化剂,搅拌均匀后加热至70℃,之后缓慢加入0.5g端氢基聚硅氧烷,在90℃下恒温反应8h,待反应结束后,减压蒸馏回收溶剂,得到改性环氧衣康酸酯树脂;
6)将2g改性环氧衣康酸酯树脂和3g封端异氰酸酯加入到80mL丙酮中,充分搅拌后,在56℃下回流反应3h,待反应结束后,滴加蒸馏水稀释至固含量50%,以2000r/min搅拌30min,经减压蒸馏回收溶剂,得到水分散体;
7)将3g木质素分散于15g水分散体中,经200W超声分散6h,形成均匀分散体,然后加入60mL改性聚氨酯乳液,充分混合均匀后静置2h,然后置于50℃烘箱中干燥固化30min,再经120℃烘箱内干燥2h,即可得到所需的聚氨酯改性树脂。
实施例2
一种阻燃UV固化高分子粘合剂,该高分子粘合剂包含如下重量份组分:25份氢氧化铝、50份聚氨酯改性树脂、60份环氧树脂、15份改性丙烯酸活性单体、7份光敏固化剂、5份疏水性气相二氧化硅、2份光引发剂、0.3份助引发剂、2份阻燃剂、50份溶剂;
该高分子粘合剂的制备方法包括如下步骤:
按照重量份数计,将聚氨酯改性树脂、环氧树脂以及改性丙烯酸活性单体充分混合,形成光学预聚物,将氢氧化铝、光敏固化剂、疏水性气相二氧化硅、光引发剂、助引发剂以及阻燃剂充分混合,形成助剂,将光学预聚物和助剂依次加入到溶剂中,充分混合均匀后,即可得到高分子粘合剂。
其中,聚氨酯改性树脂的制备方法如下:
1)将15g聚碳酸亚丙酯二醇和20g聚四氢呋喃醚二醇在真空条件下和112℃下脱水处理1.5h,然后溶于100mL二甲基甲酰胺中,搅拌下加入12g4,4'-二苯基甲烷二异氰酸酯,在70℃下反应60min,生成预聚体,然后向预聚体中加入25mL二甲基甲酰胺、12mL1,4-丁二醇和15mL1,6-己二醇,继续反应35min,形成浆料,备用;
2)将真空干燥后的60g蓖麻油和13g2-巯基乙醇混合,在氮气保护下,加入5g偶氮二异丁腈,先加热至82℃并反应5h,然后将温度调至105℃继续反应2.5h,冷却至室温后,加入70g乙酸乙酯,收集产物并用去离子水和盐水反复洗涤,干燥后除去乙酸乙酯,得到改性蓖麻油;
3)将55g改性蓖麻油和10g甘油加入到容器中,再加入0.07g氢氧化钠,混合均匀后升温至190℃,在氮气保护下反应1.5h,得到改性蓖麻油多元醇;
4)将10g改性蓖麻油多元醇加入到容器中,加入35g异氰酸酯,充分混合后加热至87℃,加入40mL丙酮、18g浆料、1.5g2,2-二羟甲基丁酸以及50μL二丁基锡二月桂酸,反应2h,然后加入1.5g丁二酮肟继续反应7h,然后加入3g三乙胺反应40min,待反应结束后,将产物倒出,然后缓慢多次的添加入等质量的去离子水,在30000r/min下高速搅拌40min,即可形成改性聚氨酯乳液;
5)将15g固含量为65%的环氧衣康酸酯树脂的异丙醇溶液加入到容器中,加入5mg卡斯特催化剂,搅拌均匀后加热至72℃,之后缓慢加入1.2g端氢基聚硅氧烷,在93℃下恒温反应9h,待反应结束后,减压蒸馏回收溶剂,得到改性环氧衣康酸酯树脂;
6)将5g改性环氧衣康酸酯树脂和7g封端异氰酸酯加入到120mL丙酮中,充分搅拌后,在58℃下回流反应8h,待反应结束后,滴加蒸馏水稀释至固含量55%,以3000r/min搅拌40min,经减压蒸馏回收溶剂,得到水分散体;
7)将5g木质素分散于20g水分散体中,经250W超声分散7h,形成均匀分散体,然后加入80mL改性聚氨酯乳液,充分混合均匀后静置3h,然后置于55℃烘箱中干燥固化40min,再经125℃烘箱内干燥3h,即可得到所需的聚氨酯改性树脂。
实施例3
一种阻燃UV固化高分子粘合剂,该高分子粘合剂包含如下重量份组分:30份氢氧化铝、60份聚氨酯改性树脂、70份环氧树脂、20份改性丙烯酸活性单体、10份光敏固化剂、6份疏水性气相二氧化硅、3份光引发剂、0.5份助引发剂、3份阻燃剂、60份溶剂;
该高分子粘合剂的制备方法包括如下步骤:
按照重量份数计,将聚氨酯改性树脂、环氧树脂以及改性丙烯酸活性单体充分混合,形成光学预聚物,将氢氧化铝、光敏固化剂、疏水性气相二氧化硅、光引发剂、助引发剂以及阻燃剂充分混合,形成助剂,将光学预聚物和助剂依次加入到溶剂中,充分混合均匀后,即可得到高分子粘合剂。
其中,聚氨酯改性树脂的制备方法如下:
1)将20g聚碳酸亚丙酯二醇和26g聚四氢呋喃醚二醇在真空条件下和115℃下脱水处理2h,然后溶于120mL二甲基甲酰胺中,搅拌下加入15g4,4'-二苯基甲烷二异氰酸酯,在73℃下反应70min,生成预聚体,然后向预聚体中加入30mL二甲基甲酰胺、15mL1,4-丁二醇和18mL1,6-己二醇,继续反应40min,形成浆料,备用;
2)将真空干燥后的70g蓖麻油和16g2-巯基乙醇混合,在氮气保护下,加入6g偶氮二异丁腈,先加热至86℃并反应6h,然后将温度调至110℃继续反应3h,冷却至室温后,加入80g乙酸乙酯,收集产物并用去离子水和盐水反复洗涤,干燥后除去乙酸乙酯,得到改性蓖麻油;
3)将60g改性蓖麻油和12g甘油加入到容器中,再加入0.08g氢氧化钠,混合均匀后升温至200℃,在氮气保护下反应2h,得到改性蓖麻油多元醇;
4)将12g改性蓖麻油多元醇加入到容器中,加入40g异氰酸酯,充分混合后加热至90℃,加入50mL丙酮、20g浆料、2g2,2-二羟甲基丁酸以及60μL二丁基锡二月桂酸,反应3h,然后加入2g丁二酮肟继续反应8h,然后加入5g三乙胺反应50min,待反应结束后,将产物倒出,然后缓慢多次的添加入等质量的去离子水,在50000r/min下高速搅拌50min,即可形成改性聚氨酯乳液;
5)将20g固含量为68%的环氧衣康酸酯树脂的异丙醇溶液加入到容器中,加入8mg卡斯特催化剂,搅拌均匀后加热至75℃,之后缓慢加入1.3g端氢基聚硅氧烷,在95℃下恒温反应10h,待反应结束后,减压蒸馏回收溶剂,得到改性环氧衣康酸酯树脂;
6)将8g改性环氧衣康酸酯树脂和10g封端异氰酸酯加入到150mL丙酮中,充分搅拌后,在60℃下回流反应6h,待反应结束后,滴加蒸馏水稀释至固含量60%,以5000r/min搅拌50min,经减压蒸馏回收溶剂,得到水分散体;
7)将8g木质素分散于30g水分散体中,经300W超声分散8h,形成均匀分散体,然后加入100mL改性聚氨酯乳液,充分混合均匀后静置5h,然后置于60℃烘箱中干燥固化50min,再经130℃烘箱内干燥5h,即可得到所需的聚氨酯改性树脂。
对比例1:本对比例与实施例1基本相同,不同之处在于,使用常规的聚氨酯替代聚氨酯改性树脂。
对比例2:本对比例与实施例1基本相同,不同之处在于,聚氨酯改性树脂的制备中,省去步骤1)。
对比例3:本对比例与实施例1基本相同,不同之处在于,聚氨酯改性树脂的制备中,省去步骤2)。
对比例4:本对比例与实施例1基本相同,不同之处在于,聚氨酯改性树脂的制备中,省去步骤2)-3)。
对比例5:本对比例与实施例1基本相同,不同之处在于,聚氨酯改性树脂的制备中,使用常规的聚氨酯乳液替代改性聚氨酯乳液。
测试实验:
采用实施例1-3和对比例1-5提供的方法,分别制得UV固化高分子粘合剂试样,上述UV固化高分子粘合剂试样涂布制成UV固化粘合膜(PET36μm、胶厚25μm、白色离型纸120μm),50℃放置3天,室温放置1天;然后将上述UV固化粘合膜裁成25mm*75mm样条贴于不锈钢板,经UV照射,再室温放置4小时后测试高温持粘力(80℃GB/T4851-2014),计算高温前后的粘力损失率;结果如表1所示。
表1
通过表1可知,本发明中的UV固化高分子粘合剂,具有很好的粘合性能,并且在高温下粘力损失率低,具有很好的高温稳定性。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为所述的具体实施方式。显然,根据本说明书的内容,可作很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (10)
1.一种阻燃UV固化高分子粘合剂,其特征在于,所述高分子粘合剂包含如下重量份组分:20-30份氢氧化铝、40-60份聚氨酯改性树脂、50-70份环氧树脂、10-20份改性丙烯酸活性单体、5-10份光敏固化剂、3-6份疏水性气相二氧化硅、1-3份光引发剂、0.1-0.5份助引发剂、1-3份阻燃剂、40-60份溶剂;
所述光敏固化剂为安息香双甲醚;
所述光引发剂为阳离子型UV光引发剂;
所述助引发剂为2-异丙基硫杂蒽酮;
所述阻燃剂为磷系阻燃剂;
所述溶剂选自环己酮、乙酸乙酯、丁酸丁酯中至少一种。
2.根据权利要求1所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述改性丙烯酸活性单体是以含端烯基的硅烷偶联剂对丙烯酸进行改性得到;
其中,含端烯基的硅烷偶联剂为甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷中任意一种。
3.根据权利要求1所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述聚氨酯改性树脂的制备方法如下:
1)将环氧衣康酸酯树脂的异丙醇溶液加入到容器中,加入卡斯特催化剂,搅拌均匀后加热至70-75℃,之后缓慢加入端氢基聚硅氧烷,在90-95℃下恒温反应8-10h,待反应结束后,减压蒸馏回收溶剂,得到改性环氧衣康酸酯树脂;
2)将改性环氧衣康酸酯树脂和封端异氰酸酯加入到丙酮中,充分搅拌后,在56-60℃下回流反应3-6h,待反应结束后,滴加蒸馏水稀释至固含量50-60%,以2000-5000r/min搅拌30-50min,经减压蒸馏回收溶剂,得到水分散体;
3)将木质素分散于水分散体中,超声分散6-8h后形成均匀分散体,然后加入改性聚氨酯乳液,充分混合均匀后静置2-5h,然后置于50-60℃烘箱中干燥固化30-50min,再经120-130℃烘箱内干燥2-5h,即可得到所需的聚氨酯改性树脂。
4.根据权利要求3所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述环氧衣康酸酯树脂的异丙醇溶液、卡斯特催化剂、端氢基聚硅氧烷的用量比例为(10-20)g:(2-8)mg:(0.5-1.3)g;
所述环氧衣康酸酯树脂的异丙醇溶液中,固含量为62-68%。
5.根据权利要求3所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述改性环氧衣康酸酯树脂、封端异氰酸酯、丙酮的用量比例为(2-8)g:(3-10)g:(80-150)mL。
6.根据权利要求3所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述木质素、水分散体、改性聚氨酯乳液的用量比例为(3-8)g:(15-30)g:(60-100)mL。
7.根据权利要求3所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述改性聚氨酯乳液的制备方法如下:
1)将10-20g聚碳酸亚丙酯二醇和13-26g聚四氢呋喃醚二醇在真空条件下和110-115℃下脱水处理1-2h,然后溶于80-120mL二甲基甲酰胺中,搅拌下加入8-15g4,4'-二苯基甲烷二异氰酸酯,在68-73℃下反应50-70min,生成预聚体,然后向预聚体中加入20-30mL二甲基甲酰胺、8-15mL1,4-丁二醇和10-18mL1,6-己二醇,继续反应30-40min,形成浆料,备用;
2)将真空干燥后的蓖麻油和2-巯基乙醇混合,在氮气保护下,加入偶氮二异丁腈,先加热至80-86℃并反应4-6h,然后将温度调至100-110℃继续反应2-3h,冷却至室温后,加入乙酸乙酯,收集产物并用去离子水和盐水反复洗涤,干燥后除去乙酸乙酯,得到改性蓖麻油;
3)将改性蓖麻油和甘油加入到容器中,再加入氢氧化钠,混合均匀后升温至180-200℃,在氮气保护下反应1-2h,得到改性蓖麻油多元醇;
4)将改性蓖麻油多元醇加入到容器中,加入异氰酸酯,充分混合后加热至85-90℃,加入丙酮、浆料、2,2-二羟甲基丁酸以及二丁基锡二月桂酸,反应1-3h,然后加入丁二酮肟继续反应6-8h,然后加入三乙胺反应30-50min,待反应结束后,将产物倒出,然后缓慢多次的添加入等质量的去离子水,在20000-50000r/min下高速搅拌30-50min,即可形成所需的改性聚氨酯乳液。
8.根据权利要求7所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述蓖麻油、2-巯基乙醇、偶氮二异丁腈、乙酸乙酯的用量比例为(50-70)g:(10-16)g:(4-6)g:(50-80)g;
所述改性蓖麻油、甘油、氢氧化钠的质量比为(50-60):(9-12):(0.05-0.08)。
9.根据权利要求7所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述改性蓖麻油多元醇、异氰酸酯、丙酮、浆料,2,2-二羟甲基丁酸、二丁基锡二月桂酸、丁二酮肟、三乙胺的用量比例为(6-12)g:(30-40)g:(30-50)mL:(15-20)g:(1-2)g:(40-60)μL:(1-2)g:(2-5)g。
10.根据权利要求1-9任意一项所述的一种阻燃UV固化高分子粘合剂,其特征在于,所述高分子粘合剂的制备方法包括如下步骤:
按照重量份数计,将聚氨酯改性树脂、环氧树脂以及改性丙烯酸活性单体充分混合,形成光学预聚物,将氢氧化铝、光敏固化剂、疏水性气相二氧化硅、光引发剂、助引发剂以及阻燃剂充分混合,形成助剂,将光学预聚物和助剂依次加入到溶剂中,充分混合均匀后,即可得到高分子粘合剂。
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