CN106085197A - 一种纤维增韧水性聚酯涂料及其制备方法 - Google Patents

一种纤维增韧水性聚酯涂料及其制备方法 Download PDF

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CN106085197A
CN106085197A CN201610550750.5A CN201610550750A CN106085197A CN 106085197 A CN106085197 A CN 106085197A CN 201610550750 A CN201610550750 A CN 201610550750A CN 106085197 A CN106085197 A CN 106085197A
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夏云
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ANHUI HEHAN OPTOELECTRONICS TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种纤维增韧水性聚酯涂料，它是由下述重量份的原料组成的：四氢糠醇2‑3、松香35‑40、富马酸8‑10、20‑30%氢氧化钠溶液6‑7、乙二醇20‑34、三氧化二锑0.1‑0.2、聚丙烯酸钠2‑3、氯化锌13‑20、聚醚二元醇80‑90、甲苯二异氰酸酯100‑130、2，2‑二羟甲基丙酸2‑3、二甘醇4‑5、三乙胺1‑2、2‑巯基苯并咪唑0.2‑0.4、全氟磺酸树脂3‑5、聚环氧琥珀酸0.6‑1、偏钒酸铵1‑2、氰乙基纤维素3‑4、苯甲酸单乙醇胺0.8‑1、海藻酸钙2‑3、十二碳醇酯0.7‑2、N，N‑二甲基甲酰胺17‑20。本发明加入的氰乙基纤维素等，可以有效的提高成品涂料的柔韧性。

Description

一种纤维增韧水性聚酯涂料及其制备方法
技术领域
本发明涉及聚酯涂料技术领域，尤其涉及一种纤维增韧水性聚酯涂料及其制备方法。
背景技术
目前，常用的水性聚氨酯材料虽然由于其环境友好而广泛应用于涂料、胶黏剂等行业，但是常规的水性聚氨酯材料仍然存在耐热性和耐候性不佳、抗静电性较差等不足，影响了其更广泛的应用为了更好的提高水性聚氨酯涂料的综合性能，克服其自身存在的耐水性差、固含量低等缺点，扩大其应用范围，近年来对水性聚氨酯的改性研究已成为一大热点，探讨的深度和广度也更为扩大。水性聚氨酯的改性主要分为两大部分，一是将水性聚氨酯与其他材料复合改性，根据改性剂不同，水性聚氨酯乳液的改性主要有环氧树脂改性、丙烯酸酯改性、添加纳米材料改性等。二是对水性聚氨酯的原料进行改性，引入淀粉、纤维素、油脂等生物质资源，利用其特性以提高水性聚氨酯的某一性能；
水性聚氨酯与无机纳米粒子的复合主要分为两种方式，一种将蒙脱土、云母、滑石粉等填料添加到水性聚氨酯中，制备成层状硅酸盐纳米改性水性聚氨酯复合材料；另一种是将二氧化硅、氧化锌、氢氧化镁、纳米纤维素等纳米粒子添加到水性聚氨酯材料中，制备成无机刚性纳米粒子复合水性聚氨酯材料。纳米氧化锌与普通 ZnO 相比，具有高的化学稳定性、较低的介电常数、较强的紫外和红外吸收以及催化活性等优异性能，将纳米 ZnO 添加到聚氨酯中，可制备出力学性能优异、抗紫外线、抗静电和抗菌等新型功能复合材料；
目前，石油价格的居高不下，造成聚酯及聚醚多元醇的生产成本也是日益增加。人们开始重视研发以可再生资源为原料生产聚氨酯的中间体。松香作为我国重要的林业生物质资源之一，已有学者研究将其加入到聚氨酯的合成中，以提高聚氨酯产品的光泽、黏结性等性能，但是他们均是直接将松香添加到聚氨酯中，而松香是多种树脂酸的混合物同时官能度不高，不能加入到聚氨酯的主链上，未能显著提高使得产品的性能，不能充分发挥松香的特性；松香具有硬度高、耐热性好以及绝缘、防腐等优良特性，如果把它引入到聚氨酯中，可以克服常规水性聚氨酯硬度低、耐热耐水性差等缺点。但是前人大多直接应用松香这一混合物，松香的结构只能作为封端剂连接在分子链的末端，使松香的性能不能得到充分的体现；。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种纤维增韧水性聚酯涂料及其制备方法。
本发明是通过以下技术方案实现的：
一种纤维增韧水性聚酯涂料，它是由下述重量份的原料组成的：
四氢糠醇2-3、松香35-40、富马酸8-10、20-30%氢氧化钠溶液6-7、乙二醇20-34、三氧化二锑0.1-0.2、聚丙烯酸钠2-3、氯化锌13-20、聚醚二元醇80-90、甲苯二异氰酸酯100-130、2，2-二羟甲基丙酸2-3、二甘醇4-5、三乙胺1-2、2-巯基苯并咪唑0.2-0.4、全氟磺酸树脂3-5、聚环氧琥珀酸0.6-1、偏钒酸铵1-2、氰乙基纤维素3-4、苯甲酸单乙醇胺0.8-1、海藻酸钙2-3、十二碳醇酯0.7-2、N，N-二甲基甲酰胺17-20。
一种所述的纤维增韧水性聚酯涂料的制备方法，包括以下步骤；
（1）取上述氰乙基纤维素、海藻酸钙混合，加入到N，N-二甲基甲酰胺中，升高温度为50-60℃，保温搅拌10-15分钟，加入上述松香重量的5-7%，升高温度为87-90℃，继续保温搅拌20-30分钟，冷却至常温，得纤维改性松香；
（2）将剩余的松香、富马酸、聚环氧琥珀酸混合，在氮气保护下200-230℃保温反应2.7-3小时，降温至157-160℃出料，加入到其重量10-15倍的无水乙醇中，加入上述纤维改性松香，搅拌均匀，滴加上述20-30%氢氧化钠溶液，搅拌至常温，抽滤，真空干燥，再加入到其重量6-8倍的无水乙醇中，滴加浓度为5-7%的盐酸溶液，调节pH为3-4，搅拌均匀，得改性富马海松酸；
（3）将上述苯甲酸单乙醇胺加入到四氢糠醇中，在50-60℃下保温搅拌3-4分钟，得胺醇溶液；
（4）将上述2-巯基苯并咪唑加入到改性富马海松酸中，在46-50℃下超声2-3分钟，抽滤，将沉淀真空干燥，与乙二醇、三氧化二锑混合，通入氮气，在150-160℃下搅拌反应3-4小时，升高温度为210-220℃，继续保温1.7-2小时，加入上述胺醇溶液，搅拌均匀，降温出料，得改性聚酯多元醇；
（5）将上述聚丙烯酸钠加入到其重量80-100倍的去离子水中，滴加醋酸，调节pH为2-3，加入氯化锌，搅拌均匀，滴加3-5mol/l的氢氧化钠，调节pH为10-11，在87-90℃下保温反应3-5小时，离心分离，将沉淀水洗2-3次，60-65℃下真空干燥10-11小时，得水分散型氧化锌；
（6）将上述聚醚二元醇、改性聚酯多元醇混合，在118-130℃下真空脱水2-3小时，冷却至常温，与甲苯二异氰酸酯混合，在76-80℃下保温反应100-120分钟，加入2，2-二羟甲基丙酸，继续保温反应50-60分钟，加入上述二甘醇，在57-60℃下保温反应4-5小时，冷却至室温，加入上述三乙胺、十二碳醇酯，搅拌均匀，得松香酸改性聚酯；
（7）将上述松香酸改性聚酯加入到其重量4-6倍的去离子水中，加入上述水分散型氧化锌与剩余各原料，超声20-30分钟，即得。
本发明的优点是：本发明通过松香制备富马海松酸，其是具有稠合多脂环刚性结构和多官能度的松香衍生物，以此为原料制备富马海松酸聚酯多元醇，引入到水性聚氨酯高分子主链中，会使聚氨酯产生交联，分子链运动受阻形成的亲水区域变小而被交联区域封闭，降低了水分子的渗入与扩散，使得漆膜具有较低的吸水率。同时富马海松酸的稠合多脂环结构的引入，增加了漆膜的拉伸强度和硬度，合成富马海松酸改性水性聚氨酯，可以克服常规水性聚氨酯硬度低、耐热耐水性差等缺点，得到的硬度高、光泽度好、耐热性及耐水性等性能优良的改性水性聚氨酯材料；本发明还加入了水分散型氧化锌，一方面提高了聚氨酯涂膜的结晶度，使得聚氨酯分子间的相互作用力增强，耐热性能升高：另一方面，分散在聚氨酯涂膜中的纳米氧化锌起到了类似交联剂的作用，使得聚氨酯的自由体积减少，分子链的活动受到约束的程度增加，相邻“交联点”之间的平均链长变小，所以聚氨酯的失重温度提高，耐热性能提高；同时纳米氧化锌在阳光，特别是在紫外光照射下，在水和空气中，能自行分解出自由移动的带负电的电子，同时留下带正电的空穴，空穴可以激活氧和氢氧根，使吸附于其上的水和空气变成活性的氧和氢氧根，它们具有很强的氧化还原作用，使细胞膜损伤而导致细菌的死灭，从而提高聚酯涂料的抗菌性能，本发明加入的氰乙基纤维素等，可以有效的提高成品涂料的柔韧性。
具体实施方式
一种纤维增韧水性聚酯涂料，它是由下述重量份的原料组成的：
四氢糠醇2、松香35、富马酸8、20%氢氧化钠溶液6、乙二醇20、三氧化二锑0.1、聚丙烯酸钠2、氯化锌13、聚醚二元醇80、甲苯二异氰酸酯100、2，2二羟甲基丙酸2、二甘醇4、三乙胺1、2巯基苯并咪唑0.2、全氟磺酸树脂3、聚环氧琥珀酸0.6、偏钒酸铵1、氰乙基纤维素3、苯甲酸单乙醇胺0.8、海藻酸钙2、十二碳醇酯0.7、N，N二甲基甲酰胺17。
一种所述的纤维增韧水性聚酯涂料的制备方法，包括以下步骤；
（1）取上述氰乙基纤维素、海藻酸钙混合，加入到N，N二甲基甲酰胺中，升高温度为50℃，保温搅拌10分钟，加入上述松香重量的5%，升高温度为87℃，继续保温搅拌20分钟，冷却至常温，得纤维改性松香；
（2）将剩余的松香、富马酸、聚环氧琥珀酸混合，在氮气保护下200℃保温反应2.7小时，降温至157℃出料，加入到其重量10倍的无水乙醇中，加入上述纤维改性松香，搅拌均匀，滴加上述20%氢氧化钠溶液，搅拌至常温，抽滤，真空干燥，再加入到其重量6倍的无水乙醇中，滴加浓度为5%的盐酸溶液，调节pH为3，搅拌均匀，得改性富马海松酸；
（3）将上述苯甲酸单乙醇胺加入到四氢糠醇中，在50℃下保温搅拌3分钟，得胺醇溶液；
（4）将上述2巯基苯并咪唑加入到改性富马海松酸中，在46℃下超声2分钟，抽滤，将沉淀真空干燥，与乙二醇、三氧化二锑混合，通入氮气，在150℃下搅拌反应3小时，升高温度为210℃，继续保温1.7小时，加入上述胺醇溶液，搅拌均匀，降温出料，得改性聚酯多元醇；
（5）将上述聚丙烯酸钠加入到其重量80倍的去离子水中，滴加醋酸，调节pH为2，加入氯化锌，搅拌均匀，滴加3mol/l的氢氧化钠，调节pH为10，在87℃下保温反应3小时，离心分离，将沉淀水洗2次，60℃下真空干燥10小时，得水分散型氧化锌；
（6）将上述聚醚二元醇、改性聚酯多元醇混合，在118℃下真空脱水2小时，冷却至常温，与甲苯二异氰酸酯混合，在76℃下保温反应100分钟，加入2，2二羟甲基丙酸，继续保温反应50分钟，加入上述二甘醇，在57℃下保温反应4小时，冷却至室温，加入上述三乙胺、十二碳醇酯，搅拌均匀，得松香酸改性聚酯；
（7）将上述松香酸改性聚酯加入到其重量4倍的去离子水中，加入上述水分散型氧化锌与剩余各原料，超声20分钟，即得。
用本发明的涂料所得漆膜的性能测试：
耐冲击强度：119kg•cm;
附着力：1；
拉伸强度：26.3MPa；
断裂伸长率：561.2%；
吸水率：12.4%；
黏度：43.5 mPa•s。

Claims (2)

1.一种纤维增韧水性聚酯涂料，其特征在于，它是由下述重量份的原料组成的：
四氢糠醇2-3、松香35-40、富马酸8-10、20-30%氢氧化钠溶液6-7、乙二醇20-34、三氧化二锑0.1-0.2、聚丙烯酸钠2-3、氯化锌13-20、聚醚二元醇80-90、甲苯二异氰酸酯100-130、2，2-二羟甲基丙酸2-3、二甘醇4-5、三乙胺1-2、2-巯基苯并咪唑0.2-0.4、全氟磺酸树脂3-5、聚环氧琥珀酸0.6-1、偏钒酸铵1-2、氰乙基纤维素3-4、苯甲酸单乙醇胺0.8-1、海藻酸钙2-3、十二碳醇酯0.7-2、N，N-二甲基甲酰胺17-20。
2.一种如权利要求1所述的纤维增韧水性聚酯涂料的制备方法，其特征在于，包括以下步骤；
（1）取上述氰乙基纤维素、海藻酸钙混合，加入到N，N-二甲基甲酰胺中，升高温度为50-60℃，保温搅拌10-15分钟，加入上述松香重量的5-7%，升高温度为87-90℃，继续保温搅拌20-30分钟，冷却至常温，得纤维改性松香；
（2）将剩余的松香、富马酸、聚环氧琥珀酸混合，在氮气保护下200-230℃保温反应2.7-3小时，降温至157-160℃出料，加入到其重量10-15倍的无水乙醇中，加入上述纤维改性松香，搅拌均匀，滴加上述20-30%氢氧化钠溶液，搅拌至常温，抽滤，真空干燥，再加入到其重量6-8倍的无水乙醇中，滴加浓度为5-7%的盐酸溶液，调节pH为3-4，搅拌均匀，得改性富马海松酸；
（3）将上述苯甲酸单乙醇胺加入到四氢糠醇中，在50-60℃下保温搅拌3-4分钟，得胺醇溶液；
（4）将上述2-巯基苯并咪唑加入到改性富马海松酸中，在46-50℃下超声2-3分钟，抽滤，将沉淀真空干燥，与乙二醇、三氧化二锑混合，通入氮气，在150-160℃下搅拌反应3-4小时，升高温度为210-220℃，继续保温1.7-2小时，加入上述胺醇溶液，搅拌均匀，降温出料，得改性聚酯多元醇；
（5）将上述聚丙烯酸钠加入到其重量80-100倍的去离子水中，滴加醋酸，调节pH为2-3，加入氯化锌，搅拌均匀，滴加3-5mol/l的氢氧化钠，调节pH为10-11，在87-90℃下保温反应3-5小时，离心分离，将沉淀水洗2-3次，60-65℃下真空干燥10-11小时，得水分散型氧化锌；
（6）将上述聚醚二元醇、改性聚酯多元醇混合，在118-130℃下真空脱水2-3小时，冷却至常温，与甲苯二异氰酸酯混合，在76-80℃下保温反应100-120分钟，加入2，2-二羟甲基丙酸，继续保温反应50-60分钟，加入上述二甘醇，在57-60℃下保温反应4-5小时，冷却至室温，加入上述三乙胺、十二碳醇酯，搅拌均匀，得松香酸改性聚酯；
（7）将上述松香酸改性聚酯加入到其重量4-6倍的去离子水中，加入上述水分散型氧化锌与剩余各原料，超声20-30分钟，即得。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109457500A (zh) * 2018-12-06 2019-03-12 福建禾欣中裕新材料有限公司 一种高物性固体无溶剂革
CN109457500B (zh) * 2018-12-06 2021-09-07 福建中裕新材料技术有限公司 一种高物性固体无溶剂革

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