CN116903824A - 塑胶颗粒超耐候性粘合剂用水性聚氨酯及其制备方法 - Google Patents
塑胶颗粒超耐候性粘合剂用水性聚氨酯及其制备方法 Download PDFInfo
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Abstract
本发明属于水性聚氨酯技术领域，具体涉及塑胶颗粒超耐候性粘合剂用水性聚氨酯及其制备方法。所述塑胶颗粒超耐候性粘合剂用水性聚氨酯，包括以下重量份数的原料：聚醚多元醇25‑27份，聚酯多元醇8‑10份，亲水单体3‑4份，全氟聚醚多元醇改性剂7‑8份，二异氰酸酯22‑25份，多羟基扩链剂0.8‑1.0份，多氨基扩链剂0.5‑0.7份，助溶剂15‑20份，催化剂0.01‑0.02份，中和剂1.7‑1.9份，消泡剂0.05‑0.1份，防腐剂0.3‑0.4份，去离子水150‑170份。本发明制备的水性聚氨酯具有优异的耐候性和耐水性，同时与EPDM塑胶颗粒的粘结力高，力学性能好。
Description
技术领域
本发明属于水性聚氨酯技术领域，具体涉及塑胶颗粒超耐候性粘合剂用水性聚氨酯及其制备方法。
背景技术
随着国民生活水平的提高以及全民健身的推广，塑胶跑道成为城市配套设施的主要项目，对塑胶跑道的材料使用也提出了更高的要求。目前市场上使用的塑胶颗粒粘合剂大多为油性聚氨酯或丙烯酸材料，此类材料使用MDI或TDI体系，会影响环境的VOC，尤其是一些异氰酸酯组分缓慢释放会长期对使用人群的健康构成一定威胁，随着环保理念的推广，亟需开发水性环保颗粒粘合剂材料，而目前市场上的水性粘合剂多为常规聚氨酯分散体，耐候性耐水性差，寿命一般为1-2年，维护成本高，难以大范围推广使用。
当前已有部分类似技术的研究，如专利CN111621259A公开了一种透气式塑胶跑道用的水性聚氨酯胶黏剂，其采用特定的低分子量非亲水醇类扩链剂1,4-丁烯二醇和辅交联剂有机过氧化物配合，1,4-丁烯二醇用于在聚氨酯硬段扩链剂中引入不饱和双键，有机过氧化物用于引发2个聚氨酯硬段扩链剂的双键聚合，使聚氨酯硬段形成分子间交联的互穿网络结构，增强其刚性，促使软硬段相分离更加完全，提高共聚物的抗拉伸性能和耐水性。但这种互穿网络结构虽然提高了耐水性，但机械性能提高的同时会影响其断裂伸长率即弹性效果。
专利CN108329455A公开了一种用于EPDM球场跑道的水性聚氨酯材料，由如下重量份数的原料组成：异佛尔酮二异氰酸酯5-10份，异氰酸酯3-5份，聚醚多元醇30-40份，亲水交联剂2-5份，中和剂1-2份，扩链剂0.5-1份，去离子水50-60份，催化剂0.1-0.2份，抗氧剂含量0.1-0.2ppm；以水为溶剂。该工艺为常规水性聚氨酯制备方法，可以提供环保性，但亲水性的提高往往会影响其耐水性。
发明内容
本发明的目的是：提供一种塑胶颗粒超耐候性粘合剂用水性聚氨酯，具有优异的耐候性和耐水性，同时与EPDM塑胶颗粒的粘结力高，力学性能好；本发明还提供其制备方法，工艺简单，生产高效。
本发明所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，包括以下重量份数的原料：
聚醚多元醇 25-27份，
聚酯多元醇 8-10份，
亲水单体 3-4份，
全氟聚醚多元醇改性剂 7-8份，
二异氰酸酯 22-25份，
多羟基扩链剂 0.8-1.0份，
多氨基扩链剂 0.5-0.7份，
助溶剂 15-20份，
催化剂 0.01-0.02份，
中和剂 1.7-1.9份，
消泡剂 0.05-0.1份，
防腐剂 0.3-0.4份，
去离子水 150-170份。
所述聚醚多元醇为聚四氢呋喃醚多元醇、聚环氧丙烷多元醇中的至少一种，其数均分子量为1000-1200；其中，聚四氢呋喃醚多元醇优选为济宁棠邑化工有限公司的聚四氢呋喃醚多元醇P1000，聚环氧丙烷多元醇优选为江苏海安石油化工厂的聚环氧丙烷多元醇PPG1000。
所述聚酯多元醇为聚碳酸酯多元醇、聚己内酯多元醇中的至少一种，其数均分子量为500-600；其中，聚碳酸酯多元醇优选为日本旭化成株式会社的聚碳酸酯多元醇T4692，聚己内酯多元醇优选为济宁利多化工有限公司的聚己内酯多元醇PCL2000。
所述亲水单体为二羟甲基丙酸、二羟甲基丁酸、1,4-丁二醇-2-磺酸钠中的至少一种。
所述全氟聚醚多元醇改性剂优选为苏威特种聚合物(常熟)有限公司的含氢氟聚醚二元醇E10H。
所述二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯中的至少一种；优选为山东同蓝化工有限公司的IPDI、万华化学集团股份有限公司的HDI中的至少一种。
所述多羟基扩链剂为二甘醇和甘油的混合物；优选的，二甘醇和甘油的混合质量比为1:（1.5-2.5）。
所述多氨基扩链剂为异佛尔酮二胺。
所述助溶剂为N-甲基吡咯烷酮、丙酮、丁酮、碳酸二甲酯中的至少一种。
所述催化剂为二丁基锡二月桂酸酯、辛酸亚锡中的一种。
所述中和剂为二甲基乙醇胺、二乙醇胺的一种。
所述消泡剂为矿物油类消泡剂；优选为巴斯夫化工有限公司的消泡剂A10。
所述防腐剂为卡松。
本发明所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯的制备方法，包括以下步骤：
将聚醚多元醇、聚酯多元醇、全氟聚醚多元醇改性剂和亲水单体混合，升温至105-110℃进行脱水，脱水后降温至70-72℃，滴加二异氰酸酯，滴加完毕后升温至80-82℃反应1-3h，再降温至70-72℃，加入多羟基扩链剂、催化剂和助溶剂，保温反应3-5h，再降温至25-30℃，加入中和剂和去离子水进行乳化，最后加入多氨基扩链剂、消泡剂、防腐剂，混合均匀，得到塑胶颗粒超耐候性粘合剂用水性聚氨酯。
优选的，脱水时间为1-2h。
优选的，乳化搅拌速率为800-1200r/min，乳化时间为5-15min。
与现有技术相比，本发明的有益效果如下：
（1）本发明制备的水性聚氨酯自身含有氟碳结构，具有优异的耐候性和耐水性，加入氟碳结构改性后的树脂与塑胶EPDM颗粒的粘结力下降明显，为了解决粘结力问题，本发明通过外交联法使用多氨基交联剂对树脂乳液改性，提高了与EPDM塑胶颗粒的粘结力，同时也提高了其机械强度；
（2）本发明采用二羟基和三羟基扩链剂组合内交联的方式进行改性，赋予分子长链结构和互穿网络结构，同时提高了树脂的抗拉强度和断裂伸长率，拉伸强度大于2.8MPa，断裂伸长率大于700%。
具体实施方式
下面结合实施例对本发明作进一步说明。实施例中所使用的原料，如无特别说明，均为市售常规原料；实施例中所使用的工艺方法，如无特别说明，均为本领域常规方法；实施例中所采用的原料用量，如无特别说明，均为重量份数。
实施例中所采用的部分原料说明如下：
聚四氢呋喃醚多元醇P1000：济宁棠邑化工有限公司；
聚环氧丙烷多元醇PPG1000：江苏海安石油化工厂；
聚碳酸酯多元醇T4692：日本旭化成株式会社；
聚己内酯多元醇PCL2000：济宁利多化工有限公司；
含氢氟聚醚二元醇E10H：苏威特种聚合物有限公司；
IPDI：山东同蓝化工有限公司；
HDI：万华化学集团股份有限公司；
消泡剂A10：巴斯夫化工有限公司。
实施例1
一种塑胶颗粒超耐候性粘合剂用水性聚氨酯，制备方法如下：
将25份聚四氢呋喃醚多元醇P1000、10份聚碳酸酯多元醇T4692、7份含氢氟聚醚二元醇E10H和3份二羟甲基丙酸混合，升温至105℃脱水1h，脱水后降温至70℃，滴加22份IPDI，滴加毕后升温至80℃反应2h，然后降温至70℃，加入0.8份多羟基扩链剂（质量比1:2的二甘醇和甘油的混合物）和0.01份二丁基锡二月桂酸酯，加入15份N-甲基吡咯烷酮保温反应4h；反应结束后降温至25℃，加入1.7份二甲基乙醇胺和150份去离子水，1000r/min乳化10min，最后加入0.7份异佛尔酮二胺、0.05份消泡剂A10、0.4份卡松，混合30min，得到塑胶颗粒超耐候性粘合剂用水性聚氨酯。
实施例2
一种塑胶颗粒超耐候性粘合剂用水性聚氨酯，制备方法如下：
将27份聚环氧丙烷多元醇PPG1000、8份聚己内酯多元醇PCL2000、8份含氢氟聚醚二元醇E10H和4份二羟甲基丁酸混合，升温至110℃脱水0.5h，脱水后降温至72℃，滴加25份HDI，滴加毕后升温至82℃反应1h，然后降温至72℃，加入1.0份多羟基扩链剂（质量比1:1.5的二甘醇和甘油的混合物）和0.02份辛酸亚锡，加入20份丙酮保温反应3h；反应结束后降温至30℃，加入1.9份二乙醇胺和160份去离子水，1200r/min乳化5min，最后加入0.5份异佛尔酮二胺、0.1份消泡剂A10、0.3份卡松，混合30min，得到塑胶颗粒超耐候性粘合剂用水性聚氨酯。
实施例3
一种塑胶颗粒超耐候性粘合剂用水性聚氨酯，制备方法如下：
将12份聚四氢呋喃醚多元醇P1000、14份聚环氧丙烷多元醇PPG1000、3份聚碳酸酯多元醇T4692、6份聚己内酯多元醇PCL2000、7.5份含氢氟聚醚二元醇E10H和3.5份1,4-丁二醇-2-磺酸钠混合，升温至105℃脱水2h，脱水后降温至70℃，滴加24份IPDI，滴加毕后升温至80℃反应3h，然后降温至70℃，加入1.0份多羟基扩链剂（质量比1:2.5的二甘醇和甘油的混合物）和0.01份二丁基锡二月桂酸酯，加入18份碳酸二甲酯保温反应5h；反应结束后降温至25℃，加入1.8份二甲基乙醇胺和170份去离子水，800r/min乳化15min，最后加入0.6份异佛尔酮二胺、0.1份消泡剂A10、0.35份卡松，混合30min，得到塑胶颗粒超耐候性粘合剂用水性聚氨酯。
对比例1
本对比例与实施例1的不同点仅在于，不添加多氨基扩链剂异佛尔酮二胺。
对比例2
本对比例与实施例1的不同点仅在于，将含氢氟聚醚二元醇e10h替换为等质量份数的聚四氢呋喃醚多元醇P1000。
对比例3
本对比例与实施例1的不同点仅在于，将多羟基扩链剂（质量比1:2的二甘醇和甘油的混合物）替换为等质量份数的二甘醇。
对比例4
本对比例与实施例1的不同点仅在于，将多羟基扩链剂（质量比1:2的二甘醇和甘油的混合物）替换为等质量份数的甘油。
对比例5
市售水性丙烯酸塑胶颗粒粘合剂。
将实施例1-3和对比例1-4制备的水性聚氨酯以及对比例5的市售水性丙烯酸塑胶颗粒粘合剂进行性能测试。其中，拉拉伸强度和断裂伸长率参照标准GB/T 1040.1-2006进行测试；耐人工紫外老化性能参照标准GB/T 1865-2009进行测试；附着力等级通过在EPDM平面材料上涂膜，采用划格法进行测试。
测试结果如表1所示。
表1
从表1可以看出，市售水性丙烯酸塑胶颗粒粘合剂产品的拉伸强度和断裂伸长率均明显低于本发明产品，并且耐人工老化和附着力均不如本发明产品；对比例2未进行全氟聚醚多元醇改性，其耐人工老化时间明显低于实施例1，说明全氟聚醚多元醇改性可以明显提高树脂的耐候性；对比例1采用全氟聚醚多元醇改性，但未进行外交联法改性，会明显影响聚氨酯与EPDM材料的粘结力；对比例3-4仅采用二元醇或三元醇扩链剂，会影响产品的拉伸强度或断裂伸长率，对比例3只使用二元醇扩链，断裂伸长率提高，但拉伸强度降低，对比例4只使用三元醇扩链，拉伸强度提高，但会损失断裂伸长率性能。
Claims (10)
1.一种塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：包括以下重量份数的原料：
聚醚多元醇 25-27份，
聚酯多元醇 8-10份，
亲水单体 3-4份，
全氟聚醚多元醇改性剂 7-8份，
二异氰酸酯 22-25份，
多羟基扩链剂 0.8-1.0份，
多氨基扩链剂 0.5-0.7份，
助溶剂 15-20份，
催化剂 0.01-0.02份，
中和剂 1.7-1.9份，
消泡剂 0.05-0.1份，
防腐剂 0.3-0.4份，
去离子水 150-170份；
所述多羟基扩链剂为二甘醇和甘油的混合物。
2.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述聚醚多元醇为聚四氢呋喃醚多元醇、聚环氧丙烷多元醇中的至少一种，其数均分子量为1000-1200。
3.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述聚酯多元醇为聚碳酸酯多元醇、聚己内酯多元醇中的至少一种，其数均分子量为500-600。
4.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述亲水单体为二羟甲基丙酸、二羟甲基丁酸、1,4-丁二醇-2-磺酸钠中的至少一种。
5.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯中的至少一种。
6.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述二甘醇和甘油的混合质量比为1:（1.5-2.5）。
7.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述多氨基扩链剂为异佛尔酮二胺。
8.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述助溶剂为N-甲基吡咯烷酮、丙酮、丁酮、碳酸二甲酯中的至少一种。
9.根据权利要求1所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯，其特征在于：所述催化剂为二丁基锡二月桂酸酯、辛酸亚锡中的一种；
所述中和剂为二甲基乙醇胺、二乙醇胺的一种；
所述消泡剂为矿物油类消泡剂；
所述防腐剂为卡松。
10.一种权利要求1-9任一项所述的塑胶颗粒超耐候性粘合剂用水性聚氨酯的制备方法，其特征在于：包括以下步骤：
将聚醚多元醇、聚酯多元醇、全氟聚醚多元醇改性剂和亲水单体混合，升温至105-110℃进行脱水，脱水后降温至70-72℃，滴加二异氰酸酯，滴加完毕后升温至80-82℃反应1-3h，再降温至70-72℃，加入多羟基扩链剂、催化剂和助溶剂，保温反应3-5h，再降温至25-30℃，加入中和剂和去离子水进行乳化，最后加入多氨基扩链剂、消泡剂、防腐剂，混合均匀，得到塑胶颗粒超耐候性粘合剂用水性聚氨酯。
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