CN111117550A - 一种镜面基片复合用粘合剂的制备方法 - Google Patents
一种镜面基片复合用粘合剂的制备方法 Download PDFInfo
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- CN111117550A CN111117550A CN201911417656.2A CN201911417656A CN111117550A CN 111117550 A CN111117550 A CN 111117550A CN 201911417656 A CN201911417656 A CN 201911417656A CN 111117550 A CN111117550 A CN 111117550A
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
本发明提供一种镜面基片复合用粘合剂的制备方法。该方法制备步骤如下:由二环己基甲烷二异氰酸酯和聚四亚甲基醚二醇聚合反应,反应体系中加入适量的环氧树脂进行嵌段改性,形成网状结构,选用甲乙酮肟作为封闭剂对端‑NCO进行封闭,经亲水扩链剂制得改性聚氨酯预聚物,加入三乙胺进行中和,加水乳化后,采用水合肼进行再次扩链,最后进行消泡、增稠、流平、抗粘等处理,得到镜面基片复合用粘合剂。该方法获得的粘合剂在镜面基片常温复合时具有较好的初粘,得到的镜面基片镭射效果好,热压制卡后剥离强度高。
Description
技术领域
本发明属于粘合剂技术领域,具体的涉及一种镜面基片复合用粘合剂的制备方法。
背景技术
科学技术和社会经济的发展使得信息技术产业迅速繁荣,也为智能卡产业带来新的契机和平台,其应用领域也愈趋广泛。目前已在安全证件、交通、金融、通信、社保、医疗健康、教育、电子政务等多个方面得到规模化的发展与应用,极大地提高了人们工作与生活的便利程度。随着智能卡行业的不断发展,卡片技术获得提升,不仅内含信息容量增大,外观也发生了巨大变化,具有特殊外观的个性化卡深受市场青睐。目前制作个性化卡常采用凹凸码打印、烫金、正反面平印、激光雕刻等工艺,实现了智能卡外观个性化制作,带动了智能卡从常规卡向个性化卡的发展,但这些工艺无法获得激光镭射效果。
镜面基片是新一代个性化智能卡基材,该基片运用计算机点阵光刻技术、3D真彩全息技术、多重与动态成像技术等,将具有彩虹动态、三维立体效果的全息图像通过模压,转移到PET基材上,然后与PVC进行复合得到,镜面基片能够使制备的智能卡表面获得激光镭射效果。
在镜片基片中,由于PVC是极性材料,PET是非极性聚酯,且PET表面具有极薄的镀铝层,因此两种材料无法直接贴合,需要采用粘合剂进行复合。镜片基片的复合过程为:将粘合剂涂布到PVC薄膜上,干燥后与PET镭射镀铝膜复合,镀铝面向内与粘合剂接触。为了使PVC薄膜上的粘合剂在复合时具有一定的初粘,复合需在烘道中进行,但当烘道内超过40℃时,复合得到的镜面基片在收卷时发生翘曲,温度越高翘曲越明显。因此需要粘合剂能够在常温下实现复合,且两种材料之间还要较好的粘结力。由于智能卡制作过程中需要采用140℃进行热压,因此镜面基片的PVC与PET之间剥离强度在热压后应能够符合智能卡的相应要求。
目前镜面基片复合用粘合剂,常温复合时初粘较好的,热压后剥离强度不能达标;热压后剥离强度较好的,镜面基片的镭射面无法像镜面一样平滑,影响成卡的激光镭射效果,难以达到个性化智能卡的预期目标。
发明内容
本发明的目的在于提供一种镜面基片复合用粘合剂的制备方法,该方法获得的粘合剂在镜面基片常温复合时具有较好的初粘,热压制卡后剥离强度高,得到的镜面基片镭射效果好。
为了实现上述目的,本发明采用如下技术方案:
镜面基片复合用粘合剂的制备方法,包括如下步骤:
(1)制备改性封端-NCO的聚氨酯预聚物
将聚四亚甲基醚二醇在80~90℃真空干燥1~2小时,降温至50~60℃,加入二环己基甲烷二异氰酸酯,形成原料混合物,混合物中二环己基甲烷二异氰酸酯和聚四亚甲基醚二醇的质量比为1:(1.5~2.0),然后逐步升温至80~85℃,反应1.5~2小时后,降温至40~50℃,加入有机铋催化剂、亲水扩链剂、交联剂和环氧树脂,逐步升温至60~65℃,然后加入占原料混合物质量20%~30%的丙酮,反应3~4小时,降温至40~50℃,加入甲乙酮肟,在此温度下保温反应0.5~1小时,升温至65~70℃继续反应1.5~2.5小时,体系粘度采用丙酮调节,制得改性封端-NCO的聚氨酯预聚物。
所述有机铋催化剂为铋锌复合催化剂,加入量为原料混合物质量的0.2%~0.4%;亲水扩链剂为二羟甲基丁酸,占原料混合物质量的4.0%~5.0%;交联剂为1,4-丁二醇和三羟甲基丙烷,二者分别占原料混合物质量的2.0%~4.0%和0.8%~1.0%;环氧树脂的环氧值为0.48~0.54,占原料混合物质量的3.0%~5.0%,甲乙酮肟占原料混合物质量的6.0%~8.0%。
(2)中和反应
将上述改性封端-NCO的聚氨酯预聚物降温至20~25℃,加入中和剂进行中和反应,所加入中和剂与所加入的亲水扩链剂质量比为1:(2.0~2.5),反应15~20分钟,使其中的羧基结构中和成盐,中和剂为三乙胺。
(3)制备改性聚氨酯
将中和后的改性封端-NCO的聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3500~4000r/min,至改性封端-NCO的聚氨酯预聚物均匀分散到去离子水中,原料混合物与去离子水的质量比为1:(1.2~1.4),得到水性分散体。在上述水性分散体中以0.05~0.1g/min的速率滴加水合肼进行后扩链反应,所加入水合肼与原料中二环己基甲烷二异氰酸酯的质量比为1:(25~30),反应时间持续15~20分钟,制得改性聚氨酯。
(4)镜面基片复合用粘合剂的制备
将制得的改性聚氨酯与消泡剂、增稠剂、反粘剂、流平剂和紫外线吸收剂按质量比为100:(1.0~1.5):(1~3):(0.5~1):(0.5~1):(0.2~0.5)的比例混合均匀,即制得镜面基片复合用粘合剂。
所述消泡剂为聚氧乙烯季戊四醇醚或聚氧丙烯甘油醚;
所述增稠剂为羟丙基甲基纤维素、羧甲基纤维素钠和羟乙基纤维素的任意一种;
所述反粘剂为微米级氧化硅粉S620;
所述流平剂为聚醚改性聚二甲基硅氧烷BYK-300或BYK-306;
所述紫外线吸收剂为2,2-二羟基-4-甲氧基二苯甲酮。
与现有技术相比,本发明:
1、采用甲乙酮肟进行封端,当PET镭射镀铝膜和PVC膜常温下复合时,由于-NCO被稳定封端,不参与主要反应,改性聚氨酯中的游离NCO、氨酯键和膜中的极性基团起到粘结作用;在制卡热压时段,甲乙酮肟封端的-NCO,在110-125℃解封,-NCO开始参与反应,配合其他极性共价键粘结界面,当达到制卡最高温度时,反应完全,粘结力达到最大。通过不同温度和不同时间段发挥不同分子链的粘结强度,使粘合剂常温下具有一定的初粘,热压后具有较高的剥离强度,而且采用甲乙酮肟进行封端,使得制备的粘合剂储存稳定性好。
2、水合肼对二环己基二异氰酸酯和聚四亚甲基醚二醇为主料的聚合反应进行后扩链,制备的水性聚氨酯链段更加柔软,内聚能低,玻璃化温度低,常温下物理粘性大,与基材表面常温初粘效果好,在经复合冷辊碾压时容易被展平,不对PET镭射镀铝膜表面产生破坏,因此得到的镜面基片表面平滑,收卷时不会发生卷边和翘曲,后续分切和在镭射膜表面印刷图案作业流畅。
3、采用环氧树脂进行改性,增加水性聚氨酯的交联度,提高涂膜的耐水性。由于环氧树脂是多羟基化合物,在共聚改性中参与缩聚反应,使得合成的改性聚氨酯分子网状交联,嵌段共聚,能够进一步提高热压制卡后的剥离强度。
具体实施方式
下面对本发明进行详细说明。本发明选用的原料来源如下:
聚四亚甲基醚二醇:(PTMEG2000)工业级日本三菱化学株式会社
二环己基甲烷-4,4-二异氰酸酯:(HMDI)工业级烟台万华聚氨酯股份有限公司
铋锌复合催化剂:分析纯美国领先化学品公司
二羟甲基丁酸:(DMBA)工业级上海和氏璧化工有限公司
1,4-丁二醇:(1,4-BG)分析纯国药集团化学试剂有限公司
环氧树脂:(E-51)工业级天津市合成材料工业研究所
三羟甲基丙烷:(TMP)分析纯天津博迪化工有限公司
甲乙酮肟(MEKO):工业级浙江锦华新材料股份有限公司
丙酮:氨酯级上海振企化学试剂有限公司
三乙胺:(TEA)分析纯上海国药集团
水合肼:(80%)分析纯天津市大茂化学试剂厂
聚氧乙烯季戊四醇醚:工业级武汉大华伟业医药化工有限公司
聚氧丙烯甘油醚:工业级湖北信宜合化工有限公司
羟丙基甲基纤维素:工业级河北兴泰纤维素有限公司
羟乙基纤维素:工业级河北兴泰纤维素有限公司
羧甲基纤维素钠:工业级上海耐今实业有限公司
硅粉S620:微米级美国杜邦公司
聚醚改性聚二甲基硅氧烷BYK-300:工业级德国毕克化学公司
聚醚改性聚二甲基硅氧烷BYK-306:工业级德国毕克化学公司
2,2-二羟基-4-甲氧基二苯甲酮:工业级德州信达化工有限公司。
一种镜面基片复合用粘合剂的制备方法,包括如下步骤:
(1)制备改性封端-NCO的聚氨酯预聚物
将聚四亚甲基醚二醇在80-90℃真空干燥1~2小时,降温至50~60℃,加入二环己基甲烷二异氰酸酯,形成原料混合物,混合物中二环己基甲烷二异氰酸酯和聚四亚甲基醚二醇的质量比为1:(1.5~2.0),然后逐步升温至80~85℃,反应1.5~2小时后,降温至40~50℃,加入有机铋催化剂、亲水扩链剂、交联剂和环氧树脂,逐步升温至60~65℃,然后加入占原料混合物质量20%~30%的丙酮,反应3~4小时,降温至40~50℃,加入甲乙酮肟,在此温度下保温反应0.5~1小时,升温至65~70℃继续反应1.5~2.5小时,体系粘度采用丙酮调节,制得改性封端-NCO的聚氨酯预聚物。
所述有机铋催化剂为铋锌复合催化剂,加入量为原料混合物质量的0.2%~0.4%,;亲水扩链剂为二羟甲基丁酸,占原料混合物质量的4.0%~5.0%;交联剂为1,4-丁二醇和三羟甲基丙烷,二者分别占原料混合物质量的2.0%~4.0%和0.8%~1.0%;环氧树脂的环氧值为0.48~0.54,占原料混合物质量的3.0%~5.0%,甲乙酮肟占原料混合物质量的6.0%~8.0%。
采用聚四亚甲基醚二醇制备的聚氨酯中醚基柔软,成膜后刚性小,易于平滑;二环己基甲烷二异氰酸酯制备的聚氨酯耐黄变,粘结力强,符合后续制卡的行业标准;环氧树脂是多羟基化合物,在共聚改性中参与缩聚反应,使得合成的改性聚氨酯分子网状交联,提高粘结强度;甲乙酮肟用于-NCO的封端,使-NCO只有达到一定温度才能参与反应,产生粘结作用。
(2)中和反应
将上述改性封端-NCO的聚氨酯预聚物降温至20~25℃,加入中和剂进行中和反应,所加入中和剂与所加入的亲水扩链剂质量比为1:(2.0~2.5),反应15~20分钟,使其中的羧基结构中和成盐,中和剂为三乙胺。
(3)制备改性聚氨酯
将中和后的改性封端-NCO的聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3500~4000r/min,至改性封端-NCO的聚氨酯预聚物均匀分散到去离子水中,原料混合物与去离子水的质量比为1:(1.2~1.4),得到水性分散体。在上述水性分散体中以0.05~0.1g/min的速率滴加水合肼进行后扩链反应,所加入水合肼与原料中二环己基甲烷二异氰酸酯的质量比为1:(25~30),反应时间持续15~20分钟,制得改性聚氨酯。
为了进一步降低粘合剂玻璃化温度更低,提高常温下的物理粘性,采用水合肼对水性分散体进行扩链。
(4)镜面基片复合用粘合剂的制备
将制得的改性聚氨酯与消泡剂、增稠剂、反粘剂、流平剂和紫外线吸收剂按质量比为100:(1.0~1.5):(1~3):(0.5~1):(0.5~1):(0.2~0.5)的比例混合均匀,即制得镜面基片复合用粘合剂。
所述消泡剂为聚氧乙烯季戊四醇醚或聚氧丙烯甘油醚;
所述增稠剂为羟丙基甲基纤维素、羧甲基纤维素钠和羟乙基纤维素的任意一种;
为了使涂布后的产品便于收卷,存放时避免粘连,所述反粘剂为微米级氧化硅粉;
所述流平剂为聚醚改性聚二甲基硅氧烷;
所述紫外线吸收剂为2,2-二羟基-4-甲氧基二苯甲酮。
实施例1
将120g聚四亚甲基醚二醇加入到500ml的四口烧瓶中,放置在90℃的真空干燥箱内真空干燥1小时,降温至50℃移出干燥箱。在干燥氮气保护下,将80g二环己基甲烷二异氰酸酯加入到上述四口烧瓶中,形成原料混合物,然后逐步升温至80℃,反应1.5小时后,降温至40℃,加入铋锌复合催化剂0.4g,亲水扩链剂二羟甲基丁酸8.0g,交联剂1,4-丁二醇4.0g,三羟甲基丙烷1.6g,环氧树脂6.0g,逐步升温至60℃,然后加入50.0g丙酮,持续反应3小时。降温至40℃,加入甲乙酮肟12.0g,在此温度下保温反应0.5小时,升温至65℃继续反应1.5小时,然后降温至20℃,加入三乙胺4.0g进行中和,反应持续15min,中和后的改性聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3500r/min,在分散机内加入去离子水240.0g,搅拌15min至改性聚氨酯预聚物均匀分散到去离子水中。最后缓慢加入扩链剂水合肼3.2g进行二次扩链并持续15min,滴加速率控制在0.05g/min之间,即得到改性聚氨酯乳液475.6g。
在所得到的改性聚氨酯乳液中加入4.756g聚氧乙烯季戊四醇醚、4.756g羟丙基甲基纤维素、2.378g聚二甲基硅氧烷、2.378gBYK-300和0.9512g2,2-二羟基-4-甲氧基二苯甲酮混合均匀,即制得镜面基片复合用粘合剂。
实施例1粘合剂的主要性能检测
表1实施例1粘合剂分析测试主要指标
产品 | 测试温度(℃) | 粘度(mpa.s) | 固含量(%) | pH值 |
指标 | 25 | 102.6 | 34 | 7.3 |
实施例所制得的镜面基片复合用粘合剂,涂布到PVC薄膜上面,在常温循环风干燥后与PET镭射镀铝膜复合,镀铝面向内与粘合剂接触,收卷后得到镜面基片产品。对所得到的镜面基片进行热压,设置热压温度为140℃,热压压力为4MPa,热压时间为20min,冷却至室温后进行热压前后的覆膜剥离强度测试比较。剥离强度(T型)测试方法:按照GB/T14916-2006等同采用ISO/IEC7810:2003测定。各项测试结果如表2:
表2粘合剂的应用效果检测
项目 | 剥离强度 | 材料平整度 | 镭射效果 |
热压前 | 2.9N/CM | 无翘曲 | 表面平滑,镭射效果好 |
热压后 | 16.6N/CM | 无翘曲 | 表面平滑,镭射效果好 |
实施例2
将160g聚四亚甲基醚二醇加入到500ml的四口烧瓶中,放置在80℃的真空干燥箱内真空干燥2小时,降温至60℃移出干燥箱。在干燥氮气保护下,将80g二环己基甲烷二异氰酸酯加入到上述四口烧瓶中,形成原料混合物,然后逐步升温至85℃,反应2.0小时后,降温至50℃,加入铋锌复合催化剂0.96g,亲水扩链剂二羟甲基丁酸12.0g,交联剂1,4-丁二醇9.6g,三羟甲基丙烷2.4g,环氧树脂12.0g,逐步升温至65℃,然后加入72.0g丙酮,持续反应4小时。降温至50℃,加入甲乙酮肟19.2g,在此温度下保温反应1.0小时,升温至70℃继续反应2.5小时,然后降温至25℃,加入三乙胺6.0g进行中和,反应持续20min,中和后的改性聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为4000r/min,在分散机内加入去离子水336.0g,搅拌15min至改性聚氨酯预聚物均匀分散到去离子水中。最后缓慢加入扩链剂水合肼2.66g进行二次扩链并持续20min,滴加速率控制在0.1g/min之间,即得到改性聚氨酯乳液640.8g。
在所得到的改性聚氨酯乳液中加入9.612g聚氧乙烯季戊四醇醚、19.224g羟丙基甲基纤维素、6.408g聚二甲基硅氧烷、6.408gBYK-300和3.204g2,2-二羟基-4-甲氧基二苯甲酮混合均匀,即制得镜面基片复合用粘合剂。
实施例2粘合剂的主要性能检测:
表3实施例2粘合剂分析测试主要指标
产品 | 测试温度(℃) | 粘度(mpa.s) | 固含量(%) | pH值 |
指标 | 25 | 110.2 | 35 | 7.1 |
实施例所制得的镜面基片复合用粘合剂,涂布到PVC薄膜上面,在常温循环风干燥后与PET镭射镀铝膜复合,镀铝面向内与粘合剂接触,收卷后得到镜面基片产品。对所得到的镜面基片进行热压,设置热压温度为140℃,热压压力为4MPa,热压时间为20min,冷却至室温后进行热压前后的覆膜剥离强度测试比较。剥离强度(T型)测试方法:按照GB/T14916-2006等同采用ISO/IEC7810:2003测定。各项测试结果如表4:
表4粘合剂的应用效果检测
项目 | 剥离强度 | 材料平整度 | 镭射效果 |
热压前 | 2.7N/CM | 无翘曲 | 表面平滑,镭射效果好 |
热压后 | 15.9N/CM | 无翘曲 | 表面平滑,镭射效果好 |
实施例3
将130g聚四亚甲基醚二醇加入到500ml的四口烧瓶中,放置在85℃的真空干燥箱内真空干燥1.5小时,降温至55℃移出干燥箱。在干燥氮气保护下,将80g二环己基甲烷二异氰酸酯加入到上述四口烧瓶中,形成原料混合物,然后逐步升温至83℃,反应1.6小时后,降温至45℃,加入铋锌复合催化剂0.7g,亲水扩链剂二羟甲基丁酸8.9g,交联剂1,4-丁二醇6.8g,三羟甲基丙烷2.2g,环氧树脂7.5g,逐步升温至65℃,然后加入60.0g丙酮,持续反应3.5小时。降温至45℃,加入甲乙酮肟16.0g,在此温度下保温反应1.0小时,升温至70℃继续反应2.0小时,然后降温至25℃,加入三乙胺4.3g进行中和,反应持续15min,中和后的改性聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3800r/min,在分散机内加入去离子水280.0g,搅拌18min至改性聚氨酯预聚物均匀分散到去离子水中。最后缓慢加入扩链剂水合肼3.0g进行二次扩链并持续17min,滴加速率控制在0.09g/min之间,即得到改性聚氨酯乳液539.4g。
在所得到的改性聚氨酯乳液中加入6.472g聚氧乙烯季戊四醇醚、6.536g羟丙基甲基纤维素、4.315g聚二甲基硅氧烷、4.394gBYK-300和1.618g2,2-二羟基-4-甲氧基二苯甲酮混合均匀,即制得镜面基片复合用粘合剂。
实施例3粘合剂的主要性能检测:
表5实施例3粘合剂分析测试主要指标
产品 | 测试温度(℃) | 粘度(mpa.s) | 固含量(%) | pH值 |
指标 | 25 | 112.8 | 37 | 7.1 |
将所制得的镜面基片复合用粘合剂,涂布到PVC薄膜上面,在常温循环风干燥后与PET镭射镀铝膜复合,镀铝面向内与粘合剂接触,收卷后得到镜面基片产品。对所得到的镜面基片进行热压,设置热压温度为140℃,热压压力为4MPa,热压时间为20min,冷却至室温后进行热压前后的覆膜剥离强度测试比较。剥离强度(T型)测试方法:按照GB/T14916-2006等同采用ISO/IEC7810:2003测定。各项测试结果如表6:
表6粘合剂的应用效果检测
项目 | 剥离强度 | 材料平整度 | 镭射效果 |
热压前 | 2.6N/CM | 无翘曲 | 表面平滑,镭射效果好 |
热压后 | 17.8N/CM | 无翘曲 | 表面平滑,镭射效果好 |
实施例4
将140g聚四亚甲基醚二醇加入到500ml的四口烧瓶中,放置在85℃的真空干燥箱内真空干燥1小时,降温至55℃移出干燥箱。在干燥氮气保护下,将80g二环己基甲烷二异氰酸酯加入到上述四口烧瓶中,形成原料混合物,然后逐步升温至85℃,反应1.5小时后,降温至40℃,加入铋锌复合催化剂0.7g,亲水扩链剂二羟甲基丁酸11.0g,交联剂1,4-丁二醇5.2g,三羟甲基丙烷1.9g,环氧树脂10.0g,逐步升温至63℃,然后加入66.0g丙酮,持续反应3小时。降温至42℃,加入甲乙酮肟15.0g,在此温度下保温反应0.5小时,升温至68℃继续反应1.5小时,然后降温至25℃,加入三乙胺4.4g进行中和,反应持续15min,中和后的改性聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3600r/min,在分散机内加入去离子水265.0g,搅拌17min至改性聚氨酯预聚物均匀分散到去离子水中。最后缓慢加入扩链剂水合肼3.0g进行二次扩链并持续15min,滴加速率控制在0.06g/min之间,即得到改性聚氨酯乳液526.6g。
在所得到的改性聚氨酯乳液中加入5.266g聚氧乙烯季戊四醇醚、10.532g羟丙基甲基纤维素、4.212g聚二甲基硅氧烷、4.463gBYK-300和1.515g2,2-二羟基-4-甲氧基二苯甲酮混合均匀,即制得镜面基片复合用粘合剂。
实施例4粘合剂的主要性能检测:
表7实施例4粘合剂分析测试主要指标
产品 | 测试温度(℃) | 粘度(mpa.s) | 固含量(%) | pH值 |
指标 | 25 | 109.5 | 33 | 7.2 |
实施例所制得的镜面基片复合用粘合剂,涂布到PVC薄膜上面,在常温循环风干燥后与PET镭射镀铝膜复合,镀铝面向内与粘合剂接触,收卷后得到镜面基片产品。对所得到的镜面基片进行热压,设置热压温度为140℃,热压压力为4MPa,热压时间为20min,冷却至室温后进行热压前后的覆膜剥离强度测试比较。剥离强度(T型)测试方法:按照GB/T14916-2006等同采用ISO/IEC7810:2003测定。各项测试结果如表8:
表8粘合剂的应用效果检测
项目 | 剥离强度 | 材料平整度 | 镭射效果 |
热压前 | 2.8N/CM | 无翘曲 | 表面平滑,镭射效果好 |
热压后 | 17.1N/CM | 无翘曲 | 表面平滑,镭射效果好 |
对比例
将采用现有两种粘合剂制得的镜面基片进行热压,设置热压温度为140℃,热压压力为4MPa,热压时间为20min,冷却至室温后进行热压前后的覆膜剥离强度测试比较。剥离强度(T型)测试方法:按照GB/T14916-2006等同采用ISO/IEC7810:2003,测定数据如表9:
表9对比例测试结果
从对比例可以看出,第一种虽然常温初粘较好,并具有较好的镭射效果,但热压后剥离强度较差;第二种具有较好的初粘及热压后的剥离强度,但表面粗糙,镭射效果较差。实施例与对比例测试结果可以看出,本发明的镜面基片复合用粘合剂常温复合时具有较好的初粘,得到的镜面基片镭射效果好,热压制卡后剥离强度高。
Claims (3)
1.一种镜面基片复合用粘合剂的制备方法,其特征在于:包括如下步骤:
(1)制备改性封端-NCO的聚氨酯预聚物
将聚四亚甲基醚二醇在80~90℃真空干燥1~2小时,降温至50~60℃,加入二环己基甲烷二异氰酸酯,形成原料混合物,混合物中二环己基甲烷二异氰酸酯和聚四亚甲基醚二醇的质量比为1:(1.5~2.0),然后逐步升温至80~85℃,反应1.5~2小时后,降温至40~50℃,加入有机铋催化剂、亲水扩链剂、交联剂和环氧树脂,逐步升温至60~65℃,然后加入占原料混合物质量20%~30%的丙酮,反应3~4小时,降温至40~50℃,加入甲乙酮肟,在此温度下保温反应0.5~1小时,升温至65~70℃继续反应1.5~2.5小时,体系粘度采用丙酮调节,制得改性封端-NCO的聚氨酯预聚物;
所述有机铋催化剂为铋锌复合催化剂,加入量为原料混合物质量的0.2%~0.4%;亲水扩链剂为二羟甲基丁酸,占原料混合物质量的4.0%~5.0%;交联剂为1,4-丁二醇和三羟甲基丙烷,二者分别占原料混合物质量的2.0%~4.0%和0.8%~1.0%;环氧树脂占原料混合物质量的3.0%~5.0%,甲乙酮肟占原料混合物质量的6.0%~8.0%;
(2)中和反应
将上述改性封端-NCO的聚氨酯预聚物降温至20~25℃,加入中和剂进行中和反应,所加入中和剂与所加入的亲水扩链剂质量比为1:(2.0~2.5),反应15~20分钟,使其中的羧基结构中和成盐,中和剂为三乙胺;
(3)制备改性聚氨酯
将中和后的改性封端-NCO的聚氨酯预聚物转移入高速分散机中,并设置分散机的剪切转速为3500~4000r/min,至改性封端-NCO的聚氨酯预聚物均匀分散到去离子水中,原料混合物与去离子水的质量比为1:(1.2~1.4),得到水性分散体;在上述水性分散体中以0.05~0.1g/min的速率滴加水合肼进行后扩链反应,所加入水合肼与原料中二环己基甲烷二异氰酸酯的质量比为1:(25~30),反应时间持续15~20分钟,制得改性聚氨酯;
(4)镜面基片复合用粘合剂的制备
将制得的改性聚氨酯与消泡剂、增稠剂、反粘剂、流平剂和紫外线吸收剂按质量比为100:(1.0~1.5):(1~3):(0.5~1):(0.5~1):(0.2~0.5)的比例混合均匀,即制得镜面基片复合用粘合剂。
2.根据权利要求1所述的一种镜面基片复合用粘合剂的制备方法,其特征在于:所述环氧树脂的环氧值为0.48~0.54。
3.根据权利要求1所述的一种镜面基片复合用粘合剂的制备方法,其特征在于:所述消泡剂为聚氧乙烯季戊四醇醚或聚氧丙烯甘油醚;
所述增稠剂为羟丙基甲基纤维素、羧甲基纤维素钠和羟乙基纤维素中的任意一种;
所述反粘剂为微米级氧化硅粉;
所述流平剂为聚醚改性聚二甲基硅氧烷;
所述紫外线吸收剂为2,2-二羟基-4-甲氧基二苯甲酮。
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