CN105969167A - 一种水性晶须型聚酯涂料及其制备方法 - Google Patents
一种水性晶须型聚酯涂料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种水性晶须型聚酯涂料,它是由下述重量份的原料组成的:碱式硫酸镁晶须3‑4、脂肪醇聚氧乙烯醚硫酸铵0.8‑2、壬二酸二辛酯0.1‑0.2、甲酰胺1‑2、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、棕榈蜡3‑4、苯甲酸单乙醇胺0.7‑2、马来酸酐3‑4、石油磺酸钙1‑2。本发明加入的碱式硫酸镁晶须可以有效的改善粒子在聚合物间的分散性,提高成品涂膜的表面强度。
Description
技术领域
本发明涉及聚酯涂料技术领域,尤其涉及一种水性晶须型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,提供一种水性晶须型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:
一种水性晶须型聚酯涂料,它是由下述重量份的原料组成的:
碱式硫酸镁晶须3-4、脂肪醇聚氧乙烯醚硫酸铵0.8-2、壬二酸二辛酯0.1-0.2、甲酰胺1-2、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、棕榈蜡3-4、苯甲酸单乙醇胺0.7-2、马来酸酐3-4、石油磺酸钙1-2。
一种所述的水性晶须型聚酯涂料的制备方法,包括以下步骤;
(1)将上述石油磺酸钙加入到其重量7-9倍的无水乙醇中,搅拌均匀,加入上述松香重量的10-14%,升高温度为90-95℃,保温搅拌10-16分钟,加入上述甲酰胺,降低温度为68-70℃,保温搅拌20-30分钟,得酰胺松香醇液;
(2)将剩余的松香、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)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,加入上述酰胺松香醇液,搅拌均匀,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;
(4)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,得沉淀;
(5)将上述脂肪醇聚氧乙烯醚硫酸铵、马来酸酐混合,加入到混合料重量13-18倍的去离子水中,搅拌均匀,加入上述沉淀、碱式硫酸镁晶须,升高温度为80-90℃,保温搅拌至水干,再置于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、苯甲酸单乙醇胺,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,本发明加入的碱式硫酸镁晶须可以有效的改善粒子在聚合物间的分散性,提高成品涂膜的表面强度。
具体实施方式
一种水性晶须型聚酯涂料,它是由下述重量份的原料组成的:
碱式硫酸镁晶须3、脂肪醇聚氧乙烯醚硫酸铵0.8、壬二酸二辛酯0.1、甲酰胺1、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、棕榈蜡3、苯甲酸单乙醇胺0.7、马来酸酐3、石油磺酸钙1。
一种所述的水性晶须型聚酯涂料的制备方法,包括以下步骤;
(1)将上述石油磺酸钙加入到其重量7倍的无水乙醇中,搅拌均匀,加入上述松香重量的10%,升高温度为90℃,保温搅拌10分钟,加入上述甲酰胺,降低温度为68℃,保温搅拌20分钟,得酰胺松香醇液;
(2)将剩余的松香、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)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,加入上述酰胺松香醇液,搅拌均匀,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;
(4)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,得沉淀;
(5)将上述脂肪醇聚氧乙烯醚硫酸铵、马来酸酐混合,加入到混合料重量13倍的去离子水中,搅拌均匀,加入上述沉淀、碱式硫酸镁晶须,升高温度为80℃,保温搅拌至水干,再置于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、苯甲酸单乙醇胺,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:25.4MPa;
断裂伸长率:560.4%;
吸水率:12.4%;
黏度:43.5 mPa•s。
Claims (2)
1.一种水性晶须型聚酯涂料,其特征在于,它是由下述重量份的原料组成的:
碱式硫酸镁晶须3-4、脂肪醇聚氧乙烯醚硫酸铵0.8-2、壬二酸二辛酯0.1-0.2、甲酰胺1-2、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、棕榈蜡3-4、苯甲酸单乙醇胺0.7-2、马来酸酐3-4、石油磺酸钙1-2。
2.一种如权利要求1所述的水性晶须型聚酯涂料的制备方法,其特征在于,包括以下步骤;
(1)将上述石油磺酸钙加入到其重量7-9倍的无水乙醇中,搅拌均匀,加入上述松香重量的10-14%,升高温度为90-95℃,保温搅拌10-16分钟,加入上述甲酰胺,降低温度为68-70℃,保温搅拌20-30分钟,得酰胺松香醇液;
(2)将剩余的松香、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)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,加入上述酰胺松香醇液,搅拌均匀,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;
(4)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,得沉淀;
(5)将上述脂肪醇聚氧乙烯醚硫酸铵、马来酸酐混合,加入到混合料重量13-18倍的去离子水中,搅拌均匀,加入上述沉淀、碱式硫酸镁晶须,升高温度为80-90℃,保温搅拌至水干,再置于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、苯甲酸单乙醇胺,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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