CN111040712A - 一种高强度耐汗液聚氨酯热熔胶的制备方法 - Google Patents
一种高强度耐汗液聚氨酯热熔胶的制备方法 Download PDFInfo
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- CN111040712A CN111040712A CN201911325520.9A CN201911325520A CN111040712A CN 111040712 A CN111040712 A CN 111040712A CN 201911325520 A CN201911325520 A CN 201911325520A CN 111040712 A CN111040712 A CN 111040712A
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Abstract
本发明涉及一种高强度耐汗液聚氨酯热熔胶的制备方法，制备步骤包括：将聚酯多元醇15‑30份、聚醚多元醇30‑60份、丙烯酸树脂15‑30份、扩链接5‑10份，在120℃、‑0.095MPa进行脱水2h，脱水完毕后，加入异氰酸酯15‑20份，抗氧剂0.2‑1.0份，催化剂0.001‑0.1份以500‑1000转/分钟的转速搅拌，于100‑120℃下反应1‑3h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶；本发明可以体现出几大优势：（1）优良的耐汗液腐蚀性能；（2）对地表面能材料具有优异的粘接强度（3）耐跌落性能好：（4）初粘强度高。
Description
技术领域
本发明涉及一种高强度耐汗液聚氨酯热熔胶的制备方法，属于化学胶黏剂领域。
技术背景
众所周知，PUR具有优异的耐高低温和耐候性能，而且其能够点出1mm一下的胶线，因此被广泛用于窄边框手机或平板的粘接。
但是传统的聚氨酯热熔胶存在许多严重的缺陷，初始粘接强度低，对难粘材料例如PP、PA、不锈钢、镀镍金属等附着力低，耐老化性能差，还有一个核心缺陷是耐汗液腐蚀性能较差，这大大影响了其应用范围。随着手机等穿戴产品的日益普及化、微型化、轻型化的趋势，汗液腐蚀对产品质量提出了更高的挑战，截至目前，已发生多例因汗液腐蚀致使手机密封失效的案例。因此国内外各大手机品牌生产商，已经对胶黏剂提出了耐汗液腐蚀的要求。
因此，开发一种高强度耐汗液并且同时对难粘材料具有优异粘接的材料，成为该领域的迫切需求，也具有巨大的市场潜力。
发明内容
为了解决现有技术中聚氨酯热熔胶存在耐汗液差、对难粘材料附着力差，本发明提供一种高强度耐汗液的聚氨酯热熔胶及其制备方法，制备的聚氨酯热熔胶为单组份湿气固化聚氨酯胶黏剂，不仅具有优良的耐汗液腐蚀性能，同时，该胶黏剂具有对难粘材料良好的附着力和优异的柔韧性、抗冷热冲击性等优点。
本发明的聚氨酯热熔胶对各种难粘基材附着力优异以及耐汗液的机理是如下：
众所周知，海洋生物贻贝所分泌的贻贝黏附蛋白粘液，使之能够牢固的黏附与各种基材表面，即时在巨浪冲刷下依然能够牢固地黏附。研究发现，贻贝之所以能够实现牢固的黏附和优异的耐盐雾性能，是因为它所分泌的贻贝黏附蛋白含有邻苯二酚基团的原因。
本发明采用多巴胺为原料将邻苯二酚结构引入聚氨酯结构中以实现对各种难粘基材的附着以及耐汗液性能的同时在分子量中引入聚己内酯结构，它与邻苯二酚结构互相发挥协同作用，经与多异氰酸酯反应后使其具有高强度的同时具有优异的柔韧性、抗冲击跌落性能。采用的丙烯酸树脂含有可与异氰酸酯反应的活性基团，其接枝聚合到分子结构当中，有效地改善了热熔胶的结晶性，从而实现快速定位的功能。从此看出，本发明的聚氨酯热熔胶不仅具有对各种基材包括各种难粘基材优异的附着力的同时还具有优良的耐汗液腐蚀性能，其综合性能都十分优秀。
本发明的技术方案如下：一种高强度耐汗液聚氨酯热熔胶的制备方法，制备步骤为：a.将1mol的聚己内酯三醇、2mol的AC2O、1mol乙二酸和0.1mol的DMAP溶解在CH2CL2中，并在20℃环境下搅拌反应96h，反应结束后将此溶液用盐酸、碳酸氢钠溶液、水洗涤干燥，经色谱分离后用乙酸乙酯-环己烷溶液洗脱，得目标产物1
b.将目标产物1与多巴胺溶解在二氯甲烷中，在180-240℃和-0.1MPa下反应4h，经洗脱得目标产物2
c.目标产物2在甲醇，碳酸氢钠作用下脱保护，经洗脱得到目标产物3
即自制扩链剂，L，m，n＝0,1,2,3,4，反应过程如下：
d.将聚酯多元醇15-30份、聚醚多元醇30-60份、丙烯酸树脂15-30份、步骤C中得到的目标产物5-10份，在120℃、-0.095MPa进行脱水2h，脱水完毕后，加入异氰酸酯15-20份，抗氧剂0.2-1.0份，催化剂0.001-0.1份以500-1000转/分钟的转速搅拌，于100-120℃下反应1-3h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶。
使用时，先开启加热系统，温度设置为100-140℃，用胶枪涂胶，在开放时间内尽快压合，室温7d可达最终强度。
进一步，所述步骤d中的异氰酸酯为甲苯二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、苯二亚甲基二异氰酸酯、六甲撑二异氰酸酯、氢化MDI中的至少一种。优选为万华股份有限公司市售的4,4’-二苯基甲烷二异氰酸酯、甲苯二异氰酸酯TDI-80/TDI-100，德国拜耳公司生产的HDI三聚体Desmodur N330中的一种或几种的混合物。
进一步，步骤d中所述的催化剂为二月桂酸二丁基锡、辛酸亚锡、三乙胺、三亚乙基二胺、环烷酸锌中的至少一种。
进一步，步骤d中所述的聚酯多元醇为己二酸与1,4-丁二醇、新戊二醇、二甘醇、1,6-己二醇、1,4-环己烷二甲醇、2，2，4-三甲基-1，3-戊二醇(TMPD)系列聚酯多元醇、3-甲基-1,5-戊二醇和3-甲基-1,5-戊二醇中的至少一种二元醇聚合而成。所述聚己二酸己二醇优选为江苏旭川化学公司市售的XCP-3000H，其羟值为35-39mgKOH/g，酸值为0.1-0.8mgKOH/g，所述聚己二酸-1,4丁二醇酯二醇优选为青岛宇田市售的POL-356T,其羟值为35-39mgKOH/g，酸值为0.1-0.8mgKOH/g，所述聚己二酸-2，2，4-三甲基-1，3-戊二醇至二醇优选为恒久大富市售的HJ-7200,其羟值为53-59mgKOH/g，酸值小于0.5mgKOH/g，进一步，步骤d中所述的聚醚多元醇为分子量在1000-4000的聚氧化丙烯二元醇、聚氧化丙烯-氧化乙烯二元醇、聚四氢呋喃醚二醇、聚己内酯二醇、聚碳酸酯二醇，优选为市售的PTMG2000、PTMG3000、PPG240、PPG220、PPG210中的一种或两种的混合物。
采用上述进一步方案的有益效果是，本发明采用的多元醇有多种结晶型或非结晶型多元醇混合组成，能够平衡初始粘接强度和开放时间的关系，以获得优异的性能。
进一步，步骤d中所述的丙烯酸树脂为烟台联邦公司生产的DB808、DB69、DB29中的一种。
采用上述进一步方案的有益效果是，本发明采用的丙烯酸树脂具有特殊的结构，其活性基团能过和异氰酸酯反应接枝到分子链上，改善初始粘接强度的同时不降低最终强度。
进一步，步骤d中所述的抗氧剂为市售的抗氧剂264、抗氧剂1010、抗氧剂1076中的至少一种。
本发明设涉及一种高强度耐汗液的聚氨酯热熔胶，不仅具有优异的耐汗液腐蚀性能，同时具有对各种材质优异的附着更重要的是它对极低表面能材料也表现出良好的附着，其综合性能超过市售的同类胶黏剂，完全能够满足手机、通讯设备等高端电子产品的苛刻要求。
本发明的高强度耐汗液聚氨酯热熔胶可以体现出几大优势：(1)优良的耐汗液腐蚀性能，在模拟汗液的环境中浸泡21d，其强度衰减小于5％；(2)对地表面能材料具有优异的粘接强度：PP材料粘接高于5MPa,含玻纤的PA粘接强度高于5MPa；(3)耐跌落性能好：滚筒跌落高于500次；(4)初粘强度高：施胶5min的粘接强度高于0.5MPa。以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
具体实施方式
实施例1：
1)以分子量为310的聚己内酯三元醇为起始剂经如下3步反应制得扩链剂，
2)将聚酯多元醇XCP-3000H计10份、HJ-7200计5份，聚醚多元醇PPG220计60份，丙烯酸树脂DB808计30份，自制扩链剂5份与120℃、-0.095MPa进行脱水2h，脱水完毕后，加入4,4‘-二苯基甲烷二异氰酸酯MDI-100计15份，抗氧剂264 0.2份，二吗啉基二乙基醚(DMDEE)0.1份于110℃下反应1h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶。
实施例2：
1)以分子量为500的聚己内酯三元醇为起始剂经如下3步反应制得扩链剂，
2)将聚酯多元醇POL-356T计30份，聚醚多元醇PPG210计20份，聚醚多元醇PPG240计10份，丙烯酸树脂DB69计15份，自制扩链剂10份与120℃、-0.095MPa进行脱水2h，脱水完毕后，加入4,4‘-二苯基甲烷二异氰酸酯MDI-100计,15份，甲苯二异氰酸酯TDI-100计2份，抗氧剂1010计1份，三亚乙基二胺计0.001份于110℃下反应1h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶。
实施例3：
1)以分子量为500的聚己内酯三元醇为起始剂经如下3步反应制得扩链剂，
2)将聚酯多元醇POL-3000H计20份，HJ-7200计5份，聚醚多元醇PPG210计20份，聚醚多元醇PPG220计25份，丙烯酸树脂DB29计20份，自制扩链剂8份于120℃、-0.095MPa进行脱水2h，脱水完毕后，加入4,4‘-二苯基甲烷二异氰酸酯MDI-100计20份，抗氧剂1076计0.5份，三亚乙基二胺计0.005份于110℃下反应1h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶。
对比例：
传统湿气固化PUR胶的配方及生产工艺如下：将聚醚多元醇PPG210计20份，聚酯多元醇POL-356T计45份加入反应釜中，以500转/分钟的转速搅拌，于120℃下真空脱水2小时，真空度保持在-0.09MPa。然后冷却到80℃，边搅拌遍加入4,4'二苯基甲烷二异氰酸酯MDI计15份，然后缓慢升温，控制温度在80℃，同时充氮气保护，反应2.5小时。待取样分析NCO％含量达到设计值后，再加入萜烯增粘树脂15份，催化剂二月桂酸二丁基锡0.1份和三乙烯二胺0.4份。在温度为110℃的条件下抽真空至无气泡出现，然后出料，密闭包装，放置待用。此胶在工艺使用时，先开启加热系统，温度设置为100～130℃，用胶枪涂胶，涂胶过程确保在开放时间内完成，再按规定进行测试。粘接强度由涂胶后放置7天后测试。一般室温固化7天可以达到最高强度。
将上述实施例1～3制得的聚氨酯热熔胶与对比实施例制备的聚氨酯热熔胶按胶粘剂试验标准进行对比测试，分别测试：粘接强度随人造汗液浸泡时间的衰减率、对PP和含玻纤的PA粘接强度、拉伸强度、断裂伸长率、剥离强度、冷热冲击性、盐雾测试和双85老化后，数据结果如表1、表2、表3所示。其中用粘接强度随人造汗液浸泡时间的衰减率来表征耐汗液腐蚀性能，这是本发明的核心考量指标。另外，本发明所述的柔韧性、粘接强度、抗冲击性能分别由表2的拉伸强度、断裂伸长率、剪切强度、剥离强度、冷热冲击性的数值进行表征；耐盐雾和耐热老化性能由表3检测项目的数值进行表征。
表1粘接强度随人造汗液浸泡时间的衰减率(耐汗液性能)测试对比:
| 样品 | 浸泡1d | 浸泡5d | 浸泡7d | 浸泡15d |
| 实施例1 | 100％ | 1％ | 2.2％ | 2.3％ |
| 实施例2 | 100％ | 0.3％ | 0.7％ | 0.8％ |
| 实施例3 | 100％ | 0.4％ | 1％ | 1.3％ |
| 对比例 | 100％ | 30.5％ | 55.7％ | 70.2％ |
测试方法：样件浸泡在人造模拟汗液中，用PE袋封装(封口)，置入45℃，55％RH的恒温恒湿箱中，取出晾干，测试相应的剪切强度，计算出衰减率。
表2实施例与对比实施例机械性能测试对照:
表3实施例与对比实施例耐盐雾耐老化性能测试对比:
实施例1～3与对比实施例的性能测试分析表明，本发明制备的高强度耐汗液的聚氨酯热熔胶，不仅具有良好的耐汗液腐蚀性能、良好的粘接强度、优异的柔韧性、抗冷热冲击性及耐盐雾耐老化性能，同时，对难粘材料表现出优异的粘接性能，所以，本发明所提供的聚氨酯热熔胶，能够满足手机、手持通讯设备、穿戴产品等制造领域需要耐汗液、高粘接强度和高可靠性的严格要求，同时也解决了对难粘材料附着力差的问题。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，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，均应包含在保护范围之内。
Claims (4)
1.一种高强度耐汗液聚氨酯热熔胶的制备方法，其特征在于，制备步骤包括：将聚酯多元醇15-30份、聚醚多元醇30-60份、丙烯酸树脂15-30份、扩链接5-10份，在120℃、-0.095MPa进行脱水2h，脱水完毕后，加入异氰酸酯15-20份，抗氧剂0.2-1.0份，催化剂0.001-0.1份以500-1000转/分钟的转速搅拌，于100-120℃下反应1-3h，脱泡30min，出料，密封包装，制得高强度耐汗液的聚氨酯热熔胶；
所述扩链剂的制备步骤包括：
a.将1mol的聚己内酯三醇、2mol的 AC2O、1mol 乙二酸和0.1mol的DMAP溶解在CH2CL2中，并在20℃环境下搅拌反应96h，反应结束后将此溶液用盐酸、碳酸氢钠溶液、水洗涤干燥，经色谱分离后用乙酸乙酯-环己烷溶液洗脱，得目标产物1；
b.将1mol目标产物1与1mol多巴胺溶解在二氯甲烷中，在180-240℃ 和 -0.1MPa下反应4h，经洗脱得目标产物2；
c.1mol目标产物2与2mol甲醇在0.01mol碳酸氢钠作用下脱保护，经洗脱得到目标产物3扩链剂；
所述扩链剂的分子式为：
其中R为 
, 其中L，m，n=0,1,2,3,4。
2.根据权利要求1所述高强度耐汗液聚氨酯热熔胶的制备方法，其特征在于，所述异氰酸酯为甲苯二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、苯二亚甲基二异氰酸酯、六甲撑二异氰酸酯、氢化MDI中的一种或几种混合物；所述催化剂为二月桂酸二丁基锡、辛酸亚锡、三乙胺、三亚乙基二胺、环烷酸锌中的一种。
3.根据权利要求1所述高强度耐汗液聚氨酯热熔胶的制备方法，其特征在于，所述聚酯多元醇为己二酸与1,4-丁二醇、新戊二醇、二甘醇、1,6-己二醇、1,4-环己烷二甲醇、2，2，4-三甲基-1，3-戊二醇系列聚酯多元醇、3-甲基-1,5-戊二醇和3-甲基-1,5-戊二醇中的至少一种二元醇聚合而成；所述聚醚多元醇为分子量在1000-4000的聚氧化丙烯二元醇、聚氧化丙烯-氧化乙烯二元醇、聚四氢呋喃醚二醇、聚己内酯二醇、聚碳酸酯二醇中的一种或两种的混合物。
4.根据权利要求1所述高强度耐汗液聚氨酯热熔胶的制备方法，其特征在于，所述丙烯酸树脂为烟台联邦公司生产的DB808、DB69、DB29中的一种。
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