CN107652875B - 一种uv防火涂料及其制备方法 - Google Patents
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Abstract
本发明属于涂料领域，尤其涉及一种UV防火涂料及其制备方法。其原料按重量份数配比如下：1,6‑乙二醇二丙烯酸酯30‑40份，阻燃改性超支化丙烯酸树脂30‑40份，聚酯丙烯酸酯15‑20份，光引发剂0.5‑2份，附着力促进剂1‑3份，流平剂0.5‑1份。该涂料阻燃性能优越，耐候性较强，并且属于环境友好型涂料。
Description
技术领域
本发明属于涂料领域，尤其涉及一种UV防火涂料及其制备方法。
背景技术
传统防火涂料易挥发、固化速度慢，不利于环境保护；而UV防火涂料对环境污染小，固化速度快，节省能源，固化产物性能好，适合于高速自动化生产等优点；因此，UV防火涂料是传统防火涂料的主要替代品。
传统UV防火涂料一般由单体、活性稀释剂、阻燃剂、光引发剂以及各种助剂组成，以采用辐射固化技术为特征的环保节能型防火涂料。UV防火涂料存在阻燃性能不好，成膜性差，耐水、耐油、耐候性差等缺点，且经过紫外线的长期照射，涂膜表面会发生明显的变色趋向，致使其机械性能下降。即便使用环境是室内，涂层也受到日光漫散射或荧光辐射的破坏以及化学物质的侵蚀，而导致涂料的涂膜变黄和老化降解，进而导致涂层的机械性能下降。
发明内容
针对现有技术存在的问题，本发明提供一种UV防火涂料及其制备方法。该涂料阻燃性能优越，耐候性较强，并且属于环境友好型涂料。
为了实现上述目的，本发明提供的UV防火涂料，其原料按重量份数配比如下：1,6-乙二醇二丙烯酸酯30-40份，阻燃改性超支化丙烯酸树脂30-40份，聚酯丙烯酸酯15-20份，光引发剂0.5-2份，附着力促进剂1-3份，流平剂0.5-1份。
所述的光引发剂为2,4,6-三甲基苯甲酰基-二苯基氧化膦（TPO）、2-甲基-2-(4-吗啉基)-1-[4-(甲硫基)苯基]-1-丙酮（907）、异丙基硫杂蒽酮（ITX）中的一种或两种的混合。
所述的附着力促进剂为CJ-1280、CD9051或PM-2中的一种。
所述的流平剂为1073或SC-333。
所述阻燃改性超支化丙烯酸树脂为阻燃改性含氟超支化聚氨酯-环氧丙烯酸树脂共聚体，其制备方法如下。
步骤1、在四口瓶中加入20-30g 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和100-200 mL二氧六环（AR），通入氮气并搅拌升温至90-100℃，DOPO全部溶解后，开始滴加13-20g全氟聚醚二元醇（ZDOL）并搅拌，ZDOL滴加速度为0.5-0.8mL/min，搅拌速度为200-400r/min；滴加完毕后，升温至70-85℃，反应0.5-1h，将反应物旋转蒸发回收二氧六环，反应结束后得到黏稠产品，然后用无水乙醇洗涤3-5次，50-70℃条件下真空干燥5-10h后，得到改性阻燃剂DOPO-ZDOL。
步骤2、在三口烧瓶中，加入200-300mLH302端羟基超支化聚酯的丙酮溶液（丙酮脱水后使用），其重量比为1:3-5（m聚酯:m丙酮=1:3-5），在25-35℃及氮气保护的条件下，边搅拌（400-500r/min）边滴加（滴加速度3-5mL/min）30-45mL的异佛尔酮二异氰酸酯（IPDI），滴加完毕后，于35-50℃条件下恒温反应5-7 h，得到端异氰酸酯基超支化聚氨酯低聚物。
步骤3、取20-30g环氧丙烯酸酯树脂，5-8g端异氰酸酯基超支化聚氨酯低聚物、10-20g改性阻燃剂DOPO-ZDOL和0.1-0.5g正丁基锡二月桂酸酯(DBTDL)加入到配有搅拌装置、恒压滴液漏斗、回流冷凝管和氮气保护的三口瓶中，待三口瓶中氮气达到饱和状态时,将烧瓶温度提升至50-85℃，搅拌速度为500-800r/min，搅拌持续6-8h，即可制得阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体。
所述的全氟聚醚二元醇分子式为HOCH2CF2O(CF2CF2O)p(CF2O)qCF2CH2OH，其中p:q=0.7-1.5，其中Mn=1000-3000。
为了实现上述目的，本发明提供的UV防火涂料的制备方法，具体包括以下步骤：按重量份数称取各原料后，先将1,6-乙二醇二丙烯酸酯和聚酯丙烯酸酯混合均匀；再向其中加入阻燃改性超支化丙烯酸树脂共聚体混合均匀，再依次分别加入光引发剂、附着力促进剂和流平剂；混合后用搅拌机搅拌，直至搅拌均匀。
本发明的有益效果。
本发明所用的单体为超支化单体，其固化速度较快，使用方便，节约能源，减少了浪费；并且所用单体和光引发剂在施工和固化过程中皆无含苯等有害气体的挥发，避免了空气的污染，属于环境友好型原料；本发明所用超支化单体的高度支化结构使得聚合物分子之间较少链缠结，不易结晶，使涂料具有良好的成膜性能，而且涂料的粘度更易于调节，生产制备工艺简易方便；本发明将阻燃剂DOPO接枝到含氟超支化单体上，得到的涂料不但具备了优良的防火性能，而且阻燃剂在涂层涂料表面不迁移，阻燃性能更持久；此外，DOPO属于无卤、无烟、无毒的阻燃剂，利于环境保护；本发明采用含氟超支化单体，涂层中含有大量的F-C键，使其具有超强的稳定性，不粉化、不褪色，而且贮存期长、施工方便、优良的抗菌性和自清洁性能。
附图说明
图1 DOPO-ZDOL的合成机理图。
图2端异氰酸酯基超支化聚氨酯低聚物的合成机理图。
图3阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体。
具体实施方案
现结合附图和实施例对本发明作进一步说明。
实施例1。
1.阻燃改性含氟超支化聚氨酯-环氧丙烯酸树脂共聚体的制备。
步骤1、在250mL四口瓶中加入30g 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和150mL二氧六环（AR），通入氮气并搅拌升温至90℃，DOPO全部溶解后开始滴加15g分子式为HOCH2CF2O(CF2CF2O)15(CF2O)15 CF2CH2OH的全氟聚醚二元醇（ZDOL）并伴随搅拌，ZDOL滴加速度为0.8mL/min,搅拌速度为300r/min滴加完毕后升温至80℃，反应1h将反应物旋转蒸发回收二氧六环，反应结束后得到黏稠产品，然后用无水乙醇洗涤5次，70℃下真空干燥7h后，得到改性阻燃剂DOPO-ZDOL；DOPO-ZDOL的合成机理图，见图1。
步骤2、在500mL三口烧瓶中，加入200mL H302端羟基超支化聚酯（购于武汉超支化树脂科技有限公司）的丙酮溶液（丙酮脱水后使用且m聚酯:m丙酮=1:3），在30℃及氮气保护下，边搅拌（500r/min）边滴加（5ml/min）45mL的异佛尔酮二异氰酸酯（IPDI），滴加完毕后，于40℃恒温反应5h，即可得端异氰酸酯基超支化聚氨酯低聚物；端异氰酸酯基超支化聚氨酯低聚物的合成机理图，见图2。
步骤3、取20g环氧丙烯酸酯树脂，8g端异氰酸酯基超支化聚氨酯低聚物、20g改性阻燃剂DOPO-ZDOL和0.5g正丁基锡二月桂酸酯(DBTDL)加入到配有搅拌装置、恒压滴液漏斗、回流冷凝管和氮气保护的500mL的三口瓶中，待三口瓶中氮气达到饱和状态时,将烧瓶温度提升至75℃，搅拌速度为700r/min，此过程持续8h，即可制得阻燃改性含氟超支化聚氨酯-环氧丙烯酸树脂共聚体；阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体，见图3。
UV防火涂料的制备方法如下。
先将40份1,6-乙二醇二丙烯酸酯和15份聚酯丙烯酸酯混合均匀,再向其中加入40份阻燃改性含氟超支化聚氨酯-环氧丙烯酸树脂共聚体混合均匀，再依次分别加入2份光引发剂907、3份附着力促进剂CJ-1280和1份流平剂SC-333，混合后用搅拌机搅拌，直至搅拌均匀。
实施例2。
1.阻燃改性含氟超支化聚氨酯-环氧丙烯酸树脂共聚体的制备：
步骤1、在250ml四口瓶中加入20g 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和100 mL二氧六环（AR），通入氮气并搅拌升温至90℃，DOPO全部溶解后开始滴加13g分子式为HOCH2CF2O(CF2CF2O)13(CF2O)10 CF2CH2OH的全氟聚醚二元醇（ZDOL）并伴随搅拌，ZDOL滴加速度为0.5mL/min,搅拌速度为300r/min滴加完毕后升温至80℃，反应1h将反应物旋转蒸发回收二氧六环，反应结束后得到黏稠产品，然后用无水乙醇洗涤5次，70℃下真空干燥10h后，得到改性阻燃剂DOPO-ZDOL。
步骤2、在500ml三口烧瓶中，加入250mL H302端羟基超支化聚酯（购于武汉超支化树脂科技有限公司）的丙酮溶液（丙酮脱水后使用且m聚酯:m丙酮=1:4），在30℃及氮气保护下，边搅拌（500r/min）边滴加（3mL/min）30ml的异佛尔酮二异氰酸酯（IPDI），滴加完毕后，于40℃恒温反应5h，即可得端异氰酸酯基超支化聚氨酯低聚物。
步骤3、取20g环氧丙烯酸酯树脂，5g端异氰酸酯基超支化聚氨酯低聚物、10g改性阻燃剂DOPO-ZDOL和0.3g正丁基锡二月桂酸酯(DBTDL)加入到配有搅拌装置、恒压滴液漏斗、回流冷凝管和氮气保护的500mL的三口瓶中，待三口瓶中氮气达到饱和状态时,将烧瓶温度提升至70℃，搅拌速度为500r/min，此过程持续8h，即可制得阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体
UV防火涂料的制备方法如下。
先将35份1,6-乙二醇二丙烯酸酯和20份聚酯丙烯酸酯混合均匀,再向其中加入40份阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体混合均匀，再依次分别加入2份光引发剂TPO、2.5份附着力促进剂CJ-1280和0.5份流平剂SC-333，混合后用搅拌机搅拌，直至搅拌均匀。
实施例3。
1.阻燃改性含氟超支化聚氨酯-环氧丙烯酯酸树脂共聚体的制备：
步骤1、在250mL四口瓶中加入25g H302端羟基超支化聚酯（购于武汉超支化树脂科技有限公司） (DOPO)和150 mL二氧六环（AR），通入氮气并搅拌升温至90℃，DOPO全部溶解后开始滴加20g分子式为HOCH2CF2O(CF2CF2O)10(CF2O)12 CF2CH2OH的全氟聚醚二元醇（ZDOL）并伴随搅拌，ZDOL滴加速度为0.8mL/min,搅拌速度为400r/min滴加完毕后升温至85℃，反应1h将反应物旋转蒸发回收二氧六环，反应结束后得到黏稠产品，然后用无水乙醇洗涤5次，60℃下真空干燥10h后，得到改性阻燃剂DOPO-ZDOL。
步骤2、在500mL三口烧瓶中，加入250mL H302端羟基超支化聚酯（购于武汉超支化树脂科技有限公司）的丙酮溶液（丙酮脱水后使用且m聚酯:m丙酮=1:5），在35℃及氮气保护下，边搅拌（500r/min）边滴加（4mL/min）45ml的异佛尔酮二异氰酸酯（IPDI），滴加完毕后，于40℃恒温反应5h，即可得端异氰酸酯基超支化聚氨酯低聚物。
步骤3、取25g环氧丙烯酸酯树脂，5g端异氰酸酯基超支化聚氨酯低聚物、15g改性阻燃剂DOPO-ZDOL和0.5g正丁基锡二月桂酸酯(DBTDL)加入到配有搅拌装置、恒压滴液漏斗、回流冷凝管和氮气保护的500mL的三口瓶中，待三口瓶中氮气达到饱和状态时,将烧瓶温度提升至80℃，搅拌速度为700r/min，此过程持续8h，即可制得阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体
UV防火涂料的制备方法如下。
先将40份1,6-乙二醇二丙烯酸酯和15份聚酯丙烯酸酯混合均匀,再向其中加入35份阻燃改性含氟超支化聚氨酯-环氧丙烯酸酯树脂共聚体混合均匀，再依次分别加入1.5份光引发剂ITX、2.5份附着力促进剂CJ-1280和1份流平剂SC-333，混合后用搅拌机搅拌，直至搅拌均匀。
对三个实施例制备得到的UV涂料的性能测试，测试结果如表1。
表1 UV涂料的性能测试。
由此可见，本发明相较于目前市售UV防火涂料（品牌：希贵型号：ZR-DG-A），其基本性能（附着力、固化时间、粘度、铅笔硬度、凝胶率）和耐候耐老化性能（耐酸性、耐碱性、耐水性、耐油性、耐紫外性能）均有较为明显的提升。其中耐火性能和防水性能提升最为明显。相对于对比例1（直接添加DOPO），其各方面性能的提升幅度虽不如市售UV防火涂料，但也都一定幅度的性能提升，因此在树脂单体上接枝DOPO是必要的。
Claims (6)
1.一种UV防火涂料，其特征在于，其原料按重量份数配比如下：1,6-乙二醇二丙烯酸酯30-40份，阻燃改性超支化丙烯酸树脂30-40份，聚酯丙烯酸酯15-20份，光引发剂0.5-2份，附着力促进剂1-3份，流平剂0.5-1份；
所述阻燃改性超支化丙烯酸树脂的制备方法，包括以下步骤：
步骤1、在四口瓶中加入20-30g 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和100-200mL二氧六环，通入氮气并搅拌升温至90-100℃，DOPO全部溶解后，开始滴加13-20g全氟聚醚二元醇并搅拌，ZDOL滴加速度为0.5-0.8mL/min，搅拌速度为200-400r/min；滴加完毕后，升温至70-85℃，反应0.5-1h，将反应物旋转蒸发回收二氧六环，反应结束后得到黏稠产品，然后用无水乙醇洗涤3-5次，50-70℃条件下真空干燥5-10h后，得到改性阻燃剂DOPO-ZDOL；
步骤2、在三口烧瓶中，加入200-300mLH302端羟基超支化聚酯的丙酮溶液，丙酮脱水后使用，其重量比m聚酯:m丙酮=1:3-5，在25-35℃及氮气保护的条件下，400-500r/min下边搅拌边滴加30-45mL的异佛尔酮二异氰酸酯，滴加速度为3-5mL/min，滴加完毕后，于35-50℃条件下恒温反应5-7 h，得到端异氰酸酯基超支化聚氨酯低聚物；
步骤3、取20-30g环氧丙烯酸酯树脂，5-8g端异氰酸酯基超支化聚氨酯低聚物、10-20g改性阻燃剂DOPO-ZDOL和0.1-0.5g正丁基锡二月桂酸酯(DBTDL)加入到配有搅拌装置、恒压滴液漏斗、回流冷凝管和氮气保护的三口瓶中，待三口瓶中氮气达到饱和状态时,将烧瓶温度提升至50-85℃，搅拌速度为500-800r/min，搅拌持续6-8h，即可制得阻燃改性超支化丙烯酸树脂。
2.如权利要求1所述的UV防火涂料，其特征在于，所述的光引发剂为2,4,6-三甲基苯甲酰基-二苯基氧化膦、2-甲基-2-(4-吗啉基)-1-[4-(甲硫基)苯基]-1-丙酮、异丙基硫杂蒽酮中的一种或两种的混合。
3.如权利要求1所述的UV防火涂料，其特征在于，所述的附着力促进剂为CJ-1280、CD9051或PM-2中的一种。
4.如权利要求1所述的UV防火涂料，其特征在于，所述的流平剂为1073或SC-333。
5.如权利要求1所述的UV防火涂料，其特征在于，所述的全氟聚醚二元醇分子式为HOCH2CF2O(CF2CF2O)p(CF2O)qCF2CH2OH，其中p:q=0.7-1.5，其中Mn=1000-3000。
6.如权利要求1-5任一所述的UV防火涂料的制备方法，其特征在于，具体包括以下步骤：按重量份数称取各原料后，先将1,6-乙二醇二丙烯酸酯和聚酯丙烯酸酯混合均匀；再向其中加入阻燃改性超支化丙烯酸树脂混合均匀，再依次分别加入光引发剂、附着力促进剂和流平剂；混合后用搅拌机搅拌，直至搅拌均匀。
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