CN113444221A - 一种环氧树脂改性水性聚氨酯的制备方法 - Google Patents
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Abstract
本发明属于有机合成和高分子材料技术领域,公开了一种环氧树脂改性水性聚氨酯的制备方法,即将聚己二酸丁二醇酯二醇脱水后,与二苯基甲烷二异氰酸酯和催化剂在70~80℃搅拌反应2h,加入二羟甲基丙酸的N‑甲基吡咯烷酮溶液,于70℃搅拌反应1.5h,加入1,4‑丁二醇于70℃搅拌反应1h,过程中加入适量丙酮调节粘度。加入环氧树脂E‑44于65~75℃搅拌反应1.5h。降温至30℃后加入三乙胺中和搅拌0.5h,再加入去离子水高速剪切乳化0.5h。真空除去丙酮后,得环氧树脂改性水性聚氨酯乳液,具有优异的耐水性、耐溶剂性,良好的力学性能及硬度等性质,可用于涂料和胶粘剂等领域。
Description
技术领域
本发明属于有机合成和高分子材料技术领域,具体涉及一种环氧树脂改性水性聚氨酯的制备方法。
背景技术
水性聚氨酯是在高速剪切下将聚氨酯预聚体分散于水中制备的,它作为热门材料除了拥有传统溶剂型聚氨酯的部分优良性能,还具有产品安全、对环境友好、成本低等优点,被广泛应用于涂料、纺织、胶粘剂等领域。但由于其耐水性差、力学性能弱等不足之处,限制了水性聚氨酯的应用范围及进一步发展。所以通过对其改性,来增强水性聚氨酯的综合性能就非常关键。
环氧树脂具有力学性能好,硬度高,耐热性能强,耐溶剂、耐腐蚀性能优良等性能。通过环氧树脂改性的水性聚氨酯兼具环氧树脂和聚氨酯的优异性能,具有广泛的应用前景。
发明内容
本发明的目的是针对现有工艺的不足,提供一种环氧树脂改性水性聚氨酯的制备方法,改善水性聚氨酯的耐水性、力学性能、硬度和耐腐蚀性能。
为实现以上目的,本发明采用的技术方案是:
一种环氧树脂改性水性聚氨酯的制备,它包括下列的原料:聚己二酸丁二醇酯二醇(PBA),环氧树脂(E-44),二苯基甲烷二异氰酸酯(MDI),二羟甲基丙酸(DMPA),1,4-丁二醇(BDO),三乙胺,二月桂酸二丁基锡,N-甲基吡咯烷酮,丙酮和去离子水。
一种环氧树脂改性水性聚氨酯的制备方法,它包括以下步骤:
(1)将聚己二酸丁二醇酯二醇加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至70~80℃;
(2)将一定量二苯基甲烷二异氰酸酯和二月桂酸二丁基锡加入上述三口烧瓶中,在温度70~80℃下搅拌反应2.0 h;
(3)将一定量的二羟甲基丙酸的N-甲基吡咯烷酮溶液加入上述三口烧瓶中,于70℃搅拌反应1.5 h得反应产物-I,再加入适量1,4-丁二醇并于70℃搅拌反应1.0 h,得反应产物-II,过程中加入适量丙酮调节粘度;
(4)加入一定量的环氧树脂E-44,控制物料温度65~75℃,搅拌反应1.5 h得反应产物-III;
(5)降温至30℃后,加入适量三乙胺中和搅拌0.5 h,再加入适量去离子水并高速剪切乳化0.5 h;
(6)真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液。
步骤(1)中的聚己二酸丁二醇酯二醇分子量为1000-2000。
步骤(2)中二苯基甲烷二异氰酸酯与聚己二酸丁二醇酯二醇的摩尔比为1.8~2.4。
步骤(3)中N-甲基吡咯烷酮溶液中二羟甲基丙酸的质量百分比为20%,二羟甲基丙酸的质量为反应产物-I的3%~5%,1,4-丁二醇的质量为反应产物-II的2%。
步骤(4)中环氧树脂E-44的质量为反应产物-III的2%~6%。
步骤(5)中三乙胺的物质的量与二羟甲基丙酸的物质的量相同,去离子水的质量为反应产物-III的100%~150%。
本发明的创新之处,在于将一定量的环氧树脂E-44引入聚氨酯预聚体中,采用共聚法制备得到具有优异的耐水性、耐溶剂性、良好的力学性能及硬度等性质的水性聚氨酯乳液。
具体实施方式
下面结合具体实施例对本发明进一步详细说明。
实施例1
将20g(0.02mol)聚己二酸丁二醇酯二醇(PBA1000)加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至70℃。将9g(0.036mol)二苯基甲烷二异氰酸酯(MDI)和二月桂酸二丁基锡加入上述三口烧瓶中,在温度70℃下搅拌反应2.0 h。将1.21 g二羟甲基丙酸(DMPA)用4.84 gN-甲基吡咯烷酮溶解后加入上述三口烧瓶中,于70℃搅拌反应1.5 h后,再加入0.62 g1,4-丁二醇(BDO)于70℃搅拌反应1.0 h,过程中加入适量丙酮调节粘度。加入0.65 g环氧树脂E-44,控制物料温度70℃,搅拌反应1.5 h。降温至30℃后,加入0.91 g三乙胺中和搅拌0.5 h,再加入39.33 g去离子水并高速剪切乳化0.5 h。真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液EWPU-1。
实施例2
将20g(0.02mol)聚己二酸丁二醇酯二醇(PBA1000)加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至80℃。将12g(0.048mol)二苯基甲烷二异氰酸酯(MDI)和二月桂酸二丁基锡加入上述三口烧瓶中,在温度80℃下搅拌反应2.0 h。将1.33 g二羟甲基丙酸(DMPA)用5.32 gN-甲基吡咯烷酮溶解后加入上述三口烧瓶中,于70℃搅拌反应1.5 h后,再加入0.68 g1,4-丁二醇(BDO)于70℃搅拌反应1.0 h,过程中加入适量丙酮调节粘度。加入2.1 g环氧树脂E-44,控制物料温度70℃,搅拌反应1.5 h。降温至30℃后,加入1 g三乙胺中和搅拌0.5 h,再加入45.23 g去离子水并高速剪切乳化0.5 h。真空除去丙酮,得目标产物环氧树脂改性水性聚氨酯乳液EWPU-2。
实施例3
将20 g(0.02mol)聚己二酸丁二醇酯二醇(PBA1000)加入带有搅拌的三口烧瓶中,加热至110 ℃后真空脱水3.0 h,然后降温至75℃。将10.5 g (0.042mol)二苯基甲烷二异氰酸酯(MDI)和二月桂酸二丁基锡加入上述三口烧瓶中,在温度75℃下搅拌反应2.0 h。将0.98 g二羟甲基丙酸(DMPA)用3.92 g N-甲基吡咯烷酮溶解后加入上述三口烧瓶中,于70℃搅拌反应1.5 h后,再加入0.64 g 1,4-丁二醇(BDO)于70℃搅拌反应1.0 h,过程中加入适量丙酮调节粘度。加入1.34 g环氧树脂E-44,控制物料温度65℃,搅拌反应1.5 h。降温至30℃后,加入0.74 g三乙胺中和搅拌0.5 h,再加入35.13 g去离子水并高速剪切乳化0.5h。真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液EWPU-3。
实施例4
将20g(0.02mol)聚己二酸丁二醇酯二醇(PBA1000)加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至75℃。将10.5g(0.042mol)二苯基甲烷二异氰酸酯(MDI)和二月桂酸二丁基锡加入上述三口烧瓶中,在温度75℃下搅拌反应2.0 h。将1.55g二羟甲基丙酸(DMPA)用6.2 gN-甲基吡咯烷酮溶解后加入上述三口烧瓶中,于70℃搅拌反应1.5 h后,再加入0.65 g1,4-丁二醇(BDO)于70℃搅拌反应1.0 h,过程中加入适量丙酮调节粘度。加入1.37 g环氧树脂E-44,控制物料温度75℃,搅拌反应1.5 h。降温至30℃后,加入1.17 g三乙胺中和搅拌0.5 h,再加入49.41 g去离子水并高速剪切乳化0.5 h。真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液EWPU-4。
实施例5
将20g(0.01mol)聚己二酸丁二醇酯二醇(PBA2000)加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至75℃。将5.25g(0.021mol)二苯基甲烷二异氰酸酯(MDI)和二月桂酸二丁基锡加入上述三口烧瓶中,在温度75℃下搅拌反应2.0 h。将1.05g二羟甲基丙酸(DMPA)用4.2 gN-甲基吡咯烷酮溶解后加入上述三口烧瓶中,于70℃搅拌反应1.5 h后,再加入0.54 g1,4-丁二醇(BDO)于70℃搅拌反应1.0 h,过程中加入适量丙酮调节粘度。加入1.12 g环氧树脂E-44,控制物料温度70℃,搅拌反应1.5 h。降温至30℃后,加入0.79 g三乙胺中和搅拌0.5 h,再加入34.95 g去离子水并高速剪切乳化0.5 h。真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液EWPU-5。
五个实施例的性能测试结果如表1所示
表1.环氧树脂改性水性聚氨酯乳液及薄膜的性能测试结果
EWPU-1 | EWPU-2 | EWPU-3 | EWPU-4 | EWPU-5 | |
硬度 | HB | H | HB | H | H |
拉伸强度/MPA | 12.46 | 18.06 | 13.38 | 14.97 | 15.32 |
断裂伸长率/% | 620.18 | 384.29 | 573.55 | 503.26 | 514.87 |
吸水率/% | 12.47 | 6.49 | 8.02 | 11.03 | 10.37 |
吸碱率/% | 18.26 | 8.45 | 11.33 | 14.48 | 12.92 |
贮存稳定性/月 | 6月以上 | 6月以上 | 6月以上 | 6月以上 | 6月以上 |
Claims (5)
1.一种环氧树脂改性水性聚氨酯的制备方法,其特征在于包括以下步骤:
(1)将聚己二酸丁二醇酯二醇加入带有搅拌的三口烧瓶中,加热至110℃后真空脱水3.0 h,然后降温至70~80℃;
(2)将一定量二苯基甲烷二异氰酸酯和二月桂酸二丁基锡加入上述三口烧瓶中,在温度70~80℃下搅拌反应2.0 h;
(3)将一定量的二羟甲基丙酸的N-甲基吡咯烷酮溶液加入上述三口烧瓶中,于70℃搅拌反应1.5 h得反应产物-I,再加入适量1,4-丁二醇并于70℃搅拌反应1.0 h,得反应产物-II,过程中加入适量丙酮调节粘度;
(4)将一定量的环氧树脂E-44加入上述三口烧瓶中,控制物料温度65~75℃,搅拌反应1.5 h得反应产物-III;
(5)将上述反应产物降温至30℃后,加入适量三乙胺中和搅拌0.5 h,再加入适量去离子水并高速剪切乳化0.5 h;
(6)真空除去丙酮, 得目标产物环氧树脂改性水性聚氨酯乳液。
2.如权利要求1所述的一种环氧树脂改性水性聚氨酯的制备方法, 其特征在于所述步骤(1)中的聚己二酸丁二醇酯二醇分子量为1000-2000;所述步骤(2)中二苯基甲烷二异氰酸酯与聚己二酸丁二醇酯二醇的摩尔比为1.8~2.4。
3.如权利要求1所述的一种环氧树脂改性水性聚氨酯的制备方法, 其特征在于所述步骤(3)中N-甲基吡咯烷酮溶液中二羟甲基丙酸的质量百分比为20%。
4.如权利要求1所述的一种环氧树脂改性水性聚氨酯的制备方法, 其特征在于所述步骤(3)中二羟甲基丙酸的质量为反应产物-I的3%~5%,1,4-丁二醇的质量为反应产物-II的2%;所述步骤(4)中环氧树脂E-44的质量为反应产物-III的2%~6%。
5.如权利要求1所述的一种环氧树脂改性水性聚氨酯的制备方法,其特征在于所述步骤(5)中三乙胺的物质的量与二羟甲基丙酸的物质的量相同,去离子水的质量为反应产物-III的100%~150%。
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CN113912814A (zh) * | 2021-10-29 | 2022-01-11 | 山东圳谷新材料科技有限公司 | 一种有机氟与环氧树脂协同改性水性聚氨酯的制备方法 |
CN114806480A (zh) * | 2022-05-06 | 2022-07-29 | 湖南松井新材料股份有限公司 | 一种有机硅改性聚氨酯丙烯酸密封胶及其制备方法 |
CN115572556A (zh) * | 2022-11-07 | 2023-01-06 | 南宝树脂(佛山)有限公司 | 一种抗撞击的环保水性球类胶黏剂 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113912814A (zh) * | 2021-10-29 | 2022-01-11 | 山东圳谷新材料科技有限公司 | 一种有机氟与环氧树脂协同改性水性聚氨酯的制备方法 |
CN114806480A (zh) * | 2022-05-06 | 2022-07-29 | 湖南松井新材料股份有限公司 | 一种有机硅改性聚氨酯丙烯酸密封胶及其制备方法 |
CN114806480B (zh) * | 2022-05-06 | 2024-02-20 | 湖南松井新材料股份有限公司 | 一种有机硅改性聚氨酯丙烯酸密封胶及其制备方法 |
CN115572556A (zh) * | 2022-11-07 | 2023-01-06 | 南宝树脂(佛山)有限公司 | 一种抗撞击的环保水性球类胶黏剂 |
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