CN108753214A - 一种防紫外线压敏胶及制备方法 - Google Patents
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Abstract
本发明公开了一种防紫外线压敏胶及制备方法,包括如下步骤:3)聚合反应操作:先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,且第一次聚合反应的时间控制在1小时,之后加入另一部分的引发剂,并升温至85度后开始引发第二次聚合反应,且第二次聚合反应的时间控制在3小时,之后将其恒温静置30分钟;4)防氧化操作:将步骤3)中制得的混合溶液降温至50度,之后加入按比例称量的抗氧化剂,该防紫外线压敏胶及制备方法,操作简单,便于大批量生产及具有产品质量高的特点。
Description
技术领域
本发明涉及化工领域的胶粘剂技术领域,具体为一种防紫外线压敏胶及制备方法。
背景技术
玻璃窗膜是一种多层多功能聚酯复合的光学级特种膜制品,一般以PET膜为基膜,通过丙烯酸酯压敏胶复合而成,贴在玻璃表面以改善玻璃的性能和强度,使其具有保温、隔热、节能、防爆、防紫外线、遮避私密及安全防护等功能,在汽车玻璃、建筑物门窗及顶棚等方面得到了广泛的应用。
一般来说,玻璃窗膜由隔热层、基膜、胶粘层和离型膜复合而成,为使玻璃窗膜达到较好的阻隔紫外线的效果,常规做法是在胶粘层中添加小分子紫外线吸收剂,但由于紫外线吸收剂分子量比较小,容易向表面迁移和挥发,从而污染基材表面,进而影响产品质量。于是如何控制小分子紫外线吸收剂在材料中的迁移和挥发,便成了大家研究的对象。且在现有的制备方法中,步骤复杂,工艺繁琐,不适用于大批量生产。
但本发明制备的防紫外线压敏胶很好的解决了此类问题,不仅便于大批量生产,且产品质量高。
发明内容
本发明的目的在于提供一种防紫外线压敏胶及制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种防紫外线压敏胶,包括原料:溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂。
一种防紫外线压敏胶的制备方法,包括如下步骤:
1)材料选取:以无明显杂质及沉淀的溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂作为反应的材料;
2)混合搅拌处理:将步骤1)中的溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂按比例称量,之后将除引发剂和抗氧化剂外的各材料导入搅拌釜中连续混合搅拌30分钟,且温度控制在常温即可,待混合溶液搅拌均匀后导出;
3)聚合反应操作:先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,且第一次聚合反应的时间控制在1小时,之后加入另一部分的引发剂,并升温至85度后开始引发第二次聚合反应,且第二次聚合反应的时间控制在3小时,之后将其恒温静置30分钟;
4)防氧化操作:将步骤3)中制得的混合溶液降温至50度,之后加入按比例称量的抗氧化剂,并进行连续混合搅拌操作,且搅拌时间控制在1小时,之后将其恒温静置15分钟,即制得防紫外线压敏胶;
5)过滤出料处理:将步骤4)中制得的防紫外线压敏胶经不锈钢过滤网后导出,并放入无尘环境下静置15分钟;
6)稀释处理:将步骤5)中制得的防紫外线压敏胶导入搅拌釜中进行连续搅拌稀释操作,且加入的溶剂与步骤5)中制得的防紫外线压敏胶的量为1:1,连续搅拌稀释的时间控制在30分钟,温度控制在常温即可,之后将其导出;
7)储存处理:将步骤6)中制得的防紫外线压敏胶均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可。
根据上述技术方案,所述溶剂由乙酸乙酯和醋酸丁酯构成,且两者混合的量分别为4:1。
根据上述技术方案,所述软单体由丙烯酸异辛酯和丙烯酸丁酯构成,且两者混合的量分别为1:1。
根据上述技术方案,所述硬单体由丙烯酸甲酯和醋酸乙烯酯构成,且两者混合的量分别为1:1。
根据上述技术方案,所述引发剂由过氧化二苯甲酰和乙酸乙酯构成,且两者混合的量分别为1:400。
根据上述技术方案,所述抗氧化剂由二丁基羟基甲苯和叔丁基对苯二酚构成,且两者混合的量分别为1:1。
根据上述技术方案,所述各材料的重量百分比分别为:50%-60%的溶剂、20%-30%的软单体、5%-15%的硬单体、1%-3%的丙烯酸、1%-3%的可聚合型防紫外线吸收剂、1%-3%的二乙烯基苯、1%-3%的引发剂和1%-3%的抗氧化剂。
根据上述技术方案,所述步骤2)和步骤6)中的搅拌釜均为一种3000L的搅拌釜。
根据上述技术方案,所述步骤5)中的不锈钢过滤网为一种400目的不锈钢过滤网。
与现有技术相比,本发明所达到的有益效果是:本发明,将可聚合型防紫外线吸收剂作为紫外线吸收剂基团引入压敏胶共聚物分子结构中,并加入了抗氧化剂,这样使得压敏胶共聚物本身聚合成大分子量的紫外线吸收剂,使其形成永久性耐紫外线的产品,并具有永久的耐候性,大大降低了反应时间,便于大批量生产,并能够有效地消除冬夏材料温度相差较大而导致的工艺不稳定性,提升了产品质量,步骤简单,适合推广及使用。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:
图1是本发明的一种防紫外线压敏胶的制备方法流程图;
具体实施方式
下面将结合本发明实施例中的附图,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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1,本发明提供一种技术方案:
实施例1:
1)将各材料按55%的溶剂、25%的软单体、10%的硬单体、2%的丙烯酸、2%的可聚合型防紫外线吸收剂、2%的二乙烯基苯、2%的引发剂和2%的抗氧化剂的重量百分称取;
2)之后将除2%的引发剂和2%的抗氧化剂外的各材料导入搅拌釜中连续混合搅拌30分钟,温度控制在常温即可,使其各组分混合搅拌均匀;
3)先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,反应时间控制在1小时,之后加入2%的引发剂,并升温至85度后开始引发第二次聚合反应,反应时间控制在3小时,之后恒温静置30分钟;
4)将制得的混合溶液降温至50度,之后加入2%的抗氧化剂,并进行连续混合搅拌操作,时间控制在1小时,再恒温静置15分钟,即制得防紫外线压敏胶;
5)将制得的防紫外线压敏胶经不锈钢过滤网后导出,并放入无尘环境下静置15分钟;
6)将制得的防紫外线压敏胶导入搅拌釜中进行连续搅拌稀释操作,并向其中加入溶剂,且量为1:1,之后连续搅拌稀释30分钟,温度控制在常温即可,之后将其导出;
7)将制得的防紫外线压敏胶均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可。
实施例2:
1)将各材料按55%的溶剂、25%的软单体、10%的硬单体、1%的丙烯酸、3%的可聚合型防紫外线吸收剂、2%的二乙烯基苯、2%的引发剂和2%的抗氧化剂的重量百分称取;
2)之后将除2%的引发剂和2%的抗氧化剂外的各材料导入搅拌釜中连续混合搅拌30分钟,温度控制在常温即可,使其各组分混合搅拌均匀;
3)先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,反应时间控制在1小时,之后加入2%的引发剂,并升温至85度后开始引发第二次聚合反应,反应时间控制在3小时,之后恒温静置30分钟;
4)将制得的混合溶液降温至50度,之后加入2%的抗氧化剂,并进行连续混合搅拌操作,时间控制在1小时,再恒温静置15分钟,即制得防紫外线压敏胶;
5)将制得的防紫外线压敏胶经不锈钢过滤网后导出,并放入无尘环境下静置15分钟;
6)将制得的防紫外线压敏胶导入搅拌釜中进行连续搅拌稀释操作,并向其中加入溶剂,且量为1:1,之后连续搅拌稀释30分钟,温度控制在常温即可,之后将其导出;
7)将制得的防紫外线压敏胶均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可。
实施例3:
1)将各材料按55%的溶剂、25%的软单体、10%的硬单体、3%的丙烯酸、1%的可聚合型防紫外线吸收剂、2%的二乙烯基苯、2%的引发剂和2%的抗氧化剂的重量百分称取;
2)之后将除2%的引发剂和2%的抗氧化剂外的各材料导入搅拌釜中连续混合搅拌30分钟,温度控制在常温即可,使其各组分混合搅拌均匀;
3)先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,反应时间控制在1小时,之后加入2%的引发剂,并升温至85度后开始引发第二次聚合反应,反应时间控制在3小时,之后恒温静置30分钟;
4)将制得的混合溶液降温至50度,之后加入2%的抗氧化剂,并进行连续混合搅拌操作,时间控制在1小时,再恒温静置15分钟,即制得防紫外线压敏胶;
5)将制得的防紫外线压敏胶经不锈钢过滤网后导出,并放入无尘环境下静置15分钟;
6)将制得的防紫外线压敏胶导入搅拌釜中进行连续搅拌稀释操作,并向其中加入溶剂,且量为1:1,之后连续搅拌稀释30分钟,温度控制在常温即可,之后将其导出;
7)将制得的防紫外线压敏胶均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可。
基于上述,本发明的优点在于,先将按比例选取好的除引发剂和抗氧化剂外的各材料进行连续混合搅拌处理,使得各组分混合均匀,之后将引发剂均分为两份,向混合溶液中导入一部分的引发剂,并升温使其发生第一次聚合反应,之后再加入另一部分的引发剂,并再次升温,使其发生第二次聚合反应,且通过连续的聚合反应,有利于提高产品的使用质量,之后将混合溶液降温并加入抗氧化剂后进行连续混合搅拌处理,即制得防紫外线压敏胶,再让防紫外线压敏胶经过400目的不锈钢过滤网后进行稀释处理,最后将其均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可,整个制备过程,步骤简单,便于大批量生产,且制得的防紫外线压敏胶,不易迁移和挥发,同时具有很好的粘合及抗剥离性能,大大提升了产品质量,适合推广及使用。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种防紫外线压敏胶,其特征在于:包括原料:溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂。
2.一种防紫外线压敏胶的制备方法,其特征在于:包括如下步骤:
1)材料选取:以无明显杂质及沉淀的溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂作为反应的材料;
2)混合搅拌处理:将步骤1)中的溶剂、软单体、硬单体、丙烯酸、可聚合型防紫外线吸收剂、二乙烯基苯、引发剂和抗氧化剂按比例称量,之后将除引发剂和抗氧化剂外的各材料导入搅拌釜中连续混合搅拌30分钟,且温度控制在常温即可,待混合溶液搅拌均匀后导出;
3)聚合反应操作:先将引发剂均分为两份,之后向一个装有搅拌装置、回流冷凝管、温度计和滴液漏斗的250ml四口烧瓶中加入步骤2)中制得的混合溶液及一部分的引发剂,并升温至75度后开始引发第一次聚合反应,且第一次聚合反应的时间控制在1小时,之后加入另一部分的引发剂,并升温至85度后开始引发第二次聚合反应,且第二次聚合反应的时间控制在3小时,之后将其恒温静置30分钟;
4)防氧化操作:将步骤3)中制得的混合溶液降温至50度,之后加入按比例称量的抗氧化剂,并进行连续混合搅拌操作,且搅拌时间控制在1小时,之后将其恒温静置15分钟,即制得防紫外线压敏胶;
5)过滤出料处理:将步骤4)中制得的防紫外线压敏胶经不锈钢过滤网后导出,并放入无尘环境下静置15分钟;
6)稀释处理:将步骤5)中制得的防紫外线压敏胶导入搅拌釜中进行连续搅拌稀释操作,且加入的溶剂与步骤5)中制得的防紫外线压敏胶的量为1:1,连续搅拌稀释的时间控制在30分钟,温度控制在常温即可,之后将其导出;
7)储存处理:将步骤6)中制得的防紫外线压敏胶均匀涂布于50微米的耐高温聚酯薄膜表面,经干燥后放入10至15度的无尘环境内进行保存即可。
3.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述溶剂由乙酸乙酯和醋酸丁酯构成,且两者混合的量分别为4:1。
4.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述软单体由丙烯酸异辛酯和丙烯酸丁酯构成,且两者混合的量分别为1:1。
5.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述硬单体由丙烯酸甲酯和醋酸乙烯酯构成,且两者混合的量分别为1:1。
6.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述引发剂由过氧化二苯甲酰和乙酸乙酯构成,且两者混合的量分别为1:400。
7.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述抗氧化剂由二丁基羟基甲苯和叔丁基对苯二酚构成,且两者混合的量分别为1:1。
8.根据权利要求1所述的一种防紫外线压敏胶,其特征在于:所述各材料的重量百分比分别为:50%-60%的溶剂、20%-30%的软单体、5%-15%的硬单体、1%-3%的丙烯酸、1%-3%的可聚合型防紫外线吸收剂、1%-3%的二乙烯基苯、1%-3%的引发剂和1%-3%的抗氧化剂。
9.根据权利要求2所述的一种防紫外线压敏胶的制备方法,其特征在于:所述步骤2)和步骤6)中的搅拌釜均为一种3000L的搅拌釜。
10.根据权利要求2所述的一种防紫外线压敏胶的制备方法,其特征在于:所述步骤5)中的不锈钢过滤网为一种400目的不锈钢过滤网。
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