CN112143320A - 一种紫外光固化丙烯酸树脂水性涂料及其制备方法 - Google Patents
一种紫外光固化丙烯酸树脂水性涂料及其制备方法 Download PDFInfo
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- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical class [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 3
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Abstract
本案涉及一种紫外光固化丙烯酸树脂水性涂料，按照重量份计由以下成分制成：丙烯酸树脂预聚体50‑60份、消泡剂1‑3份、乳化剂1‑3份、填料20‑30份、分散剂2‑4份、水100份。本发明将紫外光固化剂直接接枝到超支化聚合物结构中，可在分子内交联固化，形成三维网状结构，固化效率高；且固化反应仅在紫外光照下才开始交联固化，因而最终固化膜的性能易于控制，显著降低涂料的施工难度；以水代替有机溶剂，具有明显的环保、无毒、高效、降低成本的优点，具有显著的经济和社会效益；本发明制得的水性涂料具有极强的附着力，表干速度快，漆膜光泽度高，可广泛应用于木制品表面的涂装。
Description
技术领域
本发明涉及紫外光固化涂料领域，具体为一种紫外光固化丙烯酸树脂水性涂料其制备方法。
背景技术
涂料具有高装饰性、耐久的保护性、多功能性，被广泛应用于建筑、家装、汽车等各行各业。紫外光固化涂料具有节省能源、减轻空气污染、固化速度快等特点，特别适用于不能受热的基材涂装。与传统的线型涂料树脂相比，超支化聚合物具有三维结构、大量端基以及分子内和分子间无链缠结等特点，在紫外光辐射下能快速固化成膜，与其他官能团单体混合具有良好的相容性。
但目前紫外光固化涂料多为油性漆，甲苯、乙酸乙酯、丁酮等大量有机溶剂被使用，有机溶剂挥发，易对环境造成污染，多数有机溶剂对人体和动植物有毒有害。
发明内容
针对现有技术中的不足之处，本发明旨在将超支化技术与紫外光固化涂料结合，制备环保型水性涂料。
为实现上述目的，本发明提供如下技术方案：
一种紫外光固化丙烯酸树脂水性涂料，按照重量份计由以下成分制成：丙烯酸树脂预聚体50-60份、消泡剂1-3份、乳化剂1-3份、填料20-30份、分散剂2-4份、水100份；其中所述丙烯酸树脂预聚体由丙烯酸类单体、乙烯基三硫代碳酸酯、AIBN和7-甲基丙烯酰氧基-4-甲基香豆素聚合而成，所述乙烯基三硫代碳酸酯由以下步骤制得：
S1:在反应瓶中依次加入醋酸钯、2-溴丙酸和醋酸乙烯酯，90℃搅拌反应24h，反应液过滤除去醋酸钯，有机相用饱和碳酸钾溶液洗涤、无水硫酸钠干燥，经柱层析提纯中间体产物；
S2:反应瓶中加入氢氧化钠，丙酮/THF的混合溶剂，搅拌下缓慢滴加3- 巯基丙酸，滴加二硫化碳的丙酮溶液，滴毕，反应10min后再加入所述中间体产物，于室温反应30min，提纯得乙烯基三硫代碳酸酯。
进一步地，步骤S2中所述提纯步骤为，反应液经旋蒸除去溶剂，用二氯甲烷稀释后，水洗干燥，再在正己烷中重结晶，析出来的黄色晶体即乙烯基三硫代碳酸酯。
进一步地，所述丙烯酸树脂预聚体的制备方法，包括如下步骤：将乙烯基三硫代碳酸酯、AIBN、丙烯酸类单体和7-甲基丙烯酰氧基-4-甲基香豆素按照摩尔比为1:0.5:20～200:20～200投入到反应瓶中，加入1,4-二氧六环，氮气保护，80℃下反应5h。
进一步地，所述丙烯酸类单体选自甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸丁酯的一种以及甲基丙烯酸羟乙酯、甲基丙烯酸缩水甘油醚、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯腈中的一种。
进一步地，所述乳化剂优选为苯乙烯磺酸钠、聚氧丙烯甘油醚、壬基酚聚氧乙烯醚中的一种或多种。
进一步地，所述分散剂优选为Amp-95或Sufynol104BC。
进一步地，所述消泡剂优选为磷酸三丁酯或聚二甲基硅氧烷。
进一步地，所述填料优选为云母粉、氧化铝粉、硅藻土粉、高岭土中的一种。
本发明进一步提供了一种如上所述的紫外光固化丙烯酸树脂水性涂料的制备方法，包括如下步骤：将丙烯酸树脂预聚体、消泡剂、乳化剂、填料、分散剂和水加入到搅拌机中，800rpm-1200rpm的搅拌速度搅拌2h，即得到紫外光固化丙烯酸树脂水性涂料。
本发明中采用SCVP法和RAFT法相结合制备了超支化的聚丙烯酸树脂，同时，7-甲基丙烯酰氧基-4-甲基香豆素作为紫外光固化剂被接枝到支化结构中，在紫外光辐射下，可在分子内交联固化，形成紧密的交联网状结构。
本发明的有益效果是：本发明采用SCVP法和RAFT法相结合制备聚丙烯酸酯，产物具有反应活性，可在聚合过程中添加功能性丙烯基单体，制备不同功能的超支化聚合物，应用范围广泛；相比于传统的紫外光固化水性涂料需要在涂料配方中添加光引发剂，且光引发剂多为油溶性与水性体系相容性不好，导致固化速度低或固化效果不佳，本发明则是将紫外光固化剂直接接枝到超支化聚合物结构中，可在分子内交联固化，形成三维网状结构，固化效率高；且固化反应仅在紫外光照下才开始交联固化，因而最终固化膜的性能易于控制，显著降低涂料的施工难度；以水代替有机溶剂，具有明显的环保、无毒、高效、降低成本的优点，具有显著的经济和社会效益；本发明制得的水性涂料具有极强的附着力，涂布后能阻隔水和空气，表干速度快，漆膜光泽度高，可广泛应用于木制品表面的涂装。
具体实施方式
下面将结合实施例对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例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。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
实施工艺：
一种紫外光固化丙烯酸树脂水性涂料，按照重量份计由以下成分制成：丙烯酸树脂预聚体50-60份、消泡剂1-3份、乳化剂1-3份、填料20-30份、分散剂2-4份、水100份；其中所述丙烯酸树脂预聚体由丙烯酸类单体、乙烯基三硫代碳酸酯、AIBN和7-甲基丙烯酰氧基-4-甲基香豆素聚合而成，所述乙烯基三硫代碳酸酯由以下步骤制得：
在反应瓶中依次加入醋酸钯(0.04eq)、2-溴丙酸(10g)和醋酸乙烯酯60 ml，90℃搅拌反应24h，反应液过滤除去醋酸钯，有机相用饱和碳酸钾溶液洗涤、无水硫酸钠干燥，经柱层析提纯中间体产物；
反应瓶中加入氢氧化钠0.4g(10mmol)，丙酮/THF的混合溶剂(v/v 1:1) 10ml，搅拌下缓慢滴加3-巯基丙酸1.06g(10mmol)的混合溶剂(10ml)溶液，滴加二硫化碳2.52g(33mmol)的丙酮(2ml)溶液，滴毕，反应10min后再加入所述中间体产物，于室温反应30min，旋蒸除去溶剂，用二氯甲烷稀释后，水洗干燥，再在正己烷中重结晶，析出来的黄色晶体即乙烯基三硫代碳酸酯。
其中，所述丙烯酸树脂预聚体的制备方法，包括如下步骤：将乙烯基三硫代碳酸酯、AIBN、丙烯酸类单体和7-甲基丙烯酰氧基-4-甲基香豆素按照摩尔比为1:0.5:20～200:20～200投入到反应瓶中，加入1,4-二氧六环，氮气保护，80℃下反应5h，减压蒸馏除去有机溶剂得丙烯酸树脂预聚体。
其中，所述丙烯酸类单体选自甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸丁酯的一种以及甲基丙烯酸羟乙酯、甲基丙烯酸缩水甘油醚、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯腈中的一种。
其中，所述乳化剂优选为苯乙烯磺酸钠、聚氧丙烯甘油醚、壬基酚聚氧乙烯醚中的一种或多种。
其中，所述分散剂优选为Amp-95或Sufynol104BC。
其中，所述消泡剂优选为磷酸三丁酯或聚二甲基硅氧烷。
其中，所述填料优选为云母粉、氧化铝粉、硅藻土粉、高岭土中的一种。
一种如上所述的紫外光固化丙烯酸树脂水性涂料的制备方法，包括如下步骤：将丙烯酸树脂预聚体、消泡剂、乳化剂、分散剂2-4份、填料和水加入到搅拌机中，800rpm-1200rpm的搅拌速度搅拌2h，即得到紫外光固化丙烯酸树脂水性涂料。
实施例1：聚合单体为甲基丙烯酸甲酯和甲基丙烯酸羟乙酯，各组分的用量为丙烯酸树脂预聚体50份、磷酸三丁酯1份、苯乙烯磺酸钠1份、云母粉10、氧化铝粉10份、2份Amp-95水100份。
实施例2：聚合单体为丙烯酸甲酯和甲基丙烯酸羟乙酯，各组分的用量为丙烯酸树脂预聚体55份、磷酸三丁酯1份、苯乙烯磺酸钠1份、硅藻土粉 12、高岭土9份、2份Amp-95水100份。
实施例3：聚合单体为丙烯酸丁酯和甲基丙烯酸缩水甘油醚，各组分的用量为丙烯酸树脂预聚体60份、磷酸三丁酯1份、苯乙烯磺酸钠1份、硅藻土粉15、氧化铝粉10份、2份Amp-95水100份。
对比例：对比例工艺同上述实施例，区别在于丙烯酸树脂预聚体聚合过程中未添加7-甲基丙烯酰氧基-4-甲基香豆素，聚合单体具体为甲基丙烯酸甲酯和甲基丙烯酸羟乙酯，各组分的用量为丙烯酸树脂预聚体60份、磷酸三丁酯1份、苯乙烯磺酸钠1份、硅藻土粉15、氧化铝粉10份、2份Amp-95水 100份。
考察实施例1-3及对比例的涂料的各项技术指标，附着力按GB/T 9286-1998测试，大于2级则附着力较差；漆膜硬度按GB/T 6739-2006测试，耐水性按GB/T 5209-1985测定，96h漆膜外观无异常；光泽度按GB/T 9754-2007测试；VOC含量按照GB/T 23985-2009测定。
测试数据记录在表1中，从表1数据可知本发明实施例制得的水性涂料干燥速度快，具有较强的附着力和硬度，耐水性好，光泽度高，VOC含量低，环保型好，可用于室内木材的涂装。对比例的预聚体中未接枝有光固化剂，而是在制备涂料的过程中额外添加，此时的涂料性能相对减弱，附着力、硬度等指标均有不同程度的降低。
表1
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。
Claims (9)
1.一种紫外光固化丙烯酸树脂水性涂料，其特征在于，按照重量份计由以下成分制成：丙烯酸树脂预聚体50-60份、消泡剂1-3份、乳化剂1-3份、填料20-30份、分散剂2-4份、水100份；其中所述丙烯酸树脂预聚体由丙烯酸类单体、乙烯基三硫代碳酸酯、AIBN和7-甲基丙烯酰氧基-4-甲基香豆素聚合而成，所述乙烯基三硫代碳酸酯由以下步骤制得：
S1:在反应瓶中依次加入醋酸钯、2-溴丙酸和醋酸乙烯酯，90℃搅拌反应24h，反应液过滤除去醋酸钯，有机相用饱和碳酸钾溶液洗涤、无水硫酸钠干燥，经柱层析提纯中间体产物；
S2:反应瓶中加入氢氧化钠，丙酮/THF的混合溶剂，搅拌下缓慢滴加3-巯基丙酸，滴加二硫化碳的丙酮溶液，滴毕，反应10min后再加入所述中间体产物，于室温反应30min，提纯得乙烯基三硫代碳酸酯。
2.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，步骤S2中所述提纯步骤为，反应液经旋蒸除去溶剂，用二氯甲烷稀释后，水洗干燥，再在正己烷中重结晶，析出来的黄色晶体即乙烯基三硫代碳酸酯。
3.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述丙烯酸树脂预聚体的制备方法，包括如下步骤：将乙烯基三硫代碳酸酯、AIBN、丙烯酸类单体和7-甲基丙烯酰氧基-4-甲基香豆素按照摩尔比为1:0.5:20～200:20～200投入到反应瓶中，加入1,4-二氧六环，氮气保护，80℃下反应5h。
4.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述丙烯酸类单体选自甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸丁酯的一种以及甲基丙烯酸羟乙酯、甲基丙烯酸缩水甘油醚、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯腈中的一种。
5.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述乳化剂选自苯乙烯磺酸钠、聚氧丙烯甘油醚、壬基酚聚氧乙烯醚中的一种或多种。
6.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述分散剂为Amp-95或Sufynol104BC。
7.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述消泡剂为磷酸三丁酯或聚二甲基硅氧烷。
8.如权利要求1所述的一种紫外光固化丙烯酸树脂水性涂料，其特征在于，所述填料选自云母粉、氧化铝粉、硅藻土粉、高岭土中的一种。
9.一种如权利要求1-8所述的紫外光固化丙烯酸树脂水性涂料的制备方法，其特征在于，包括如下步骤：将丙烯酸树脂预聚体、消泡剂、乳化剂、填料、分散剂和水加入到搅拌机中，800rpm-1200rpm的搅拌速度搅拌2h，即得到紫外光固化丙烯酸树脂水性涂料。
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