CN106147581A - 一种环保水性聚酯涂料及其制备方法 - Google Patents
一种环保水性聚酯涂料及其制备方法 Download PDFInfo
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- CN106147581A CN106147581A CN201610550332.6A CN201610550332A CN106147581A CN 106147581 A CN106147581 A CN 106147581A CN 201610550332 A CN201610550332 A CN 201610550332A CN 106147581 A CN106147581 A CN 106147581A
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Abstract
本发明公开了一种环保水性聚酯涂料，它是由下述重量份的原料组成的：氧化聚乙烯蜡2‑3、铝酸钙2‑4、聚丙烯酸丁酯0.7‑1、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、失水山梨醇单油酸酯0.1‑0.3、四丁基溴化铵1‑2、烷基醇酰胺2‑3、蓖麻油酸锌0.6‑1。本发明的涂料无毒无污染，安全环保性好，综合性能优越。
Description
技术领域
本发明涉及聚酯涂料技术领域，尤其涉及一种环保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，提供一种环保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：
一种环保水性聚酯涂料，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2-3、铝酸钙2-4、聚丙烯酸丁酯0.7-1、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、失水山梨醇单油酸酯0.1-0.3、四丁基溴化铵1-2、烷基醇酰胺2-3、蓖麻油酸锌0.6-1。
一种所述的环保水性聚酯涂料的制备方法，包括以下步骤；
（1）将上述氧化聚乙烯蜡加入到其重量10-12倍的无水乙醇中，送入120-130℃的油浴中，保温搅拌6-9分钟，出料，加入松香、蓖麻油酸锌，搅拌至常温，蒸馏除去乙醇，得改性松香；
（2）将上述改性松香、富马酸混合，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，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）取上述四丁基溴化铵，加入到其重量10-17倍的去离子水中，搅拌均匀，加入失水山梨醇单油酸酯，升高温度为57-60℃，保温搅拌7-8分钟，加入铝酸钙，搅拌至常温，得水乳液；
（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，降温出料，得改性聚酯多元醇；
（5）将上述烷基醇酰胺加入到其重量6-8倍的无水乙醇中，搅拌均匀，加入聚丙烯酸丁酯，在80-90℃下保温搅拌4-7分钟，得醇酯溶液；
（6）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；
（7）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，加入上述醇酯溶液，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、蓖麻油酸锌，搅拌均匀，得松香酸改性聚酯；
（8）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、水乳液，超声20-30分钟，与剩余各原料混合，搅拌均匀，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，本发明的涂料无毒无污染，安全环保性好，综合性能优越。
具体实施方式
一种环保水性聚酯涂料，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2、铝酸钙2、聚丙烯酸丁酯0.7、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、失水山梨醇单油酸酯0.1、四丁基溴化铵1、烷基醇酰胺2、蓖麻油酸锌0.6。
一种所述的环保水性聚酯涂料的制备方法，包括以下步骤；
（1）将上述氧化聚乙烯蜡加入到其重量10倍的无水乙醇中，送入120℃的油浴中，保温搅拌6分钟，出料，加入松香、蓖麻油酸锌，搅拌至常温，蒸馏除去乙醇，得改性松香；
（2）将上述改性松香、富马酸混合，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，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）取上述四丁基溴化铵，加入到其重量10倍的去离子水中，搅拌均匀，加入失水山梨醇单油酸酯，升高温度为57℃，保温搅拌7分钟，加入铝酸钙，搅拌至常温，得水乳液；
（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，降温出料，得改性聚酯多元醇；
（5）将上述烷基醇酰胺加入到其重量6倍的无水乙醇中，搅拌均匀，加入聚丙烯酸丁酯，在80℃下保温搅拌4分钟，得醇酯溶液；
（6）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；
（7）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，加入上述醇酯溶液，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、蓖麻油酸锌，搅拌均匀，得松香酸改性聚酯；
（8）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、水乳液，超声20分钟，与剩余各原料混合，搅拌均匀，即得。
用本发明的涂料所得漆膜的性能测试：
耐冲击强度：116kg•cm;
附着力：1；
拉伸强度：26.4MPa；
断裂伸长率：560.7%；
吸水率：12.7%；
黏度：43.5 mPa•s。
Claims (2)
1.一种环保水性聚酯涂料，其特征在于，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2-3、铝酸钙2-4、聚丙烯酸丁酯0.7-1、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、失水山梨醇单油酸酯0.1-0.3、四丁基溴化铵1-2、烷基醇酰胺2-3、蓖麻油酸锌0.6-1。
2.一种如权利要求1所述的环保水性聚酯涂料的制备方法，其特征在于，包括以下步骤；
（1）将上述氧化聚乙烯蜡加入到其重量10-12倍的无水乙醇中，送入120-130℃的油浴中，保温搅拌6-9分钟，出料，加入松香、蓖麻油酸锌，搅拌至常温，蒸馏除去乙醇，得改性松香；
（2）将上述改性松香、富马酸混合，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，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）取上述四丁基溴化铵，加入到其重量10-17倍的去离子水中，搅拌均匀，加入失水山梨醇单油酸酯，升高温度为57-60℃，保温搅拌7-8分钟，加入铝酸钙，搅拌至常温，得水乳液；
（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，降温出料，得改性聚酯多元醇；
（5）将上述烷基醇酰胺加入到其重量6-8倍的无水乙醇中，搅拌均匀，加入聚丙烯酸丁酯，在80-90℃下保温搅拌4-7分钟，得醇酯溶液；
（6）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；
（7）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，加入上述醇酯溶液，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、蓖麻油酸锌，搅拌均匀，得松香酸改性聚酯；
（8）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、水乳液，超声20-30分钟，与剩余各原料混合，搅拌均匀，即得。
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|---|---|---|---|---|
| CN112760021A (zh) * | 2020-12-31 | 2021-05-07 | 湖州白洋装饰材料有限公司 | 一种水性装饰涂料及其制备方法 |
| CN113801286A (zh) * | 2021-09-03 | 2021-12-17 | 华南农业大学 | 一种改性阴离子型植物油基水性聚氨酯乳液及其制备方法和应用 |
| CN114590045A (zh) * | 2021-12-31 | 2022-06-07 | 南通威斯派尔半导体技术有限公司 | 一种高精度焊料图形的印刷方法 |
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2016
- 2016-07-13 CN CN201610550332.6A patent/CN106147581A/zh active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112760021A (zh) * | 2020-12-31 | 2021-05-07 | 湖州白洋装饰材料有限公司 | 一种水性装饰涂料及其制备方法 |
| CN113801286A (zh) * | 2021-09-03 | 2021-12-17 | 华南农业大学 | 一种改性阴离子型植物油基水性聚氨酯乳液及其制备方法和应用 |
| CN114590045A (zh) * | 2021-12-31 | 2022-06-07 | 南通威斯派尔半导体技术有限公司 | 一种高精度焊料图形的印刷方法 |
| CN114590045B (zh) * | 2021-12-31 | 2023-01-06 | 南通威斯派尔半导体技术有限公司 | 一种高精度焊料图形的印刷方法 |
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