CN114133513A - 一种水性聚天门冬氨酸酯分散体、其制备方法以及水性聚脲涂料树脂 - Google Patents
一种水性聚天门冬氨酸酯分散体、其制备方法以及水性聚脲涂料树脂 Download PDFInfo
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Abstract
本发明属于涂料技术领域,具体涉及一种水性聚天门冬氨酸酯分散体、其制备方法以及水性聚脲涂料树脂。该方法包括步骤:1)将聚醚胺和聚天门冬氨酸酯树脂在100℃‑120℃、负压条件下脱水;2)步骤1)完成后,降温至20℃‑60℃,匀速滴加二异氰酸酯,滴加时间控制在0.5h‑1.5h,并加入溶剂,滴加完后升温至40℃‑80℃,恒温反应;3)在步骤2)完成后,缓慢滴加预热的去离子水,0.5h‑1.5h滴加完毕,然后继续搅拌约0.4h‑0.6h,降温出料,即得所述的水性聚天门冬氨酸酯分散体。本发明制备得到的水性聚天门冬氨酸酯分散体VOC含量低、安全无毒环保,与水性多异氰酸酯配伍形成的聚脲涂层综合性能优异。
Description
技术领域
本发明属于涂料技术领域,具体涉及一种水性聚天门冬氨酸酯分散体、其制备方法以及水性聚脲涂料树脂。
背景技术
鉴于当前有关环保的法律法规日趋严厉,传统涂料的水性化开发已经成为趋势,“油改水”的趋势已越来越成为涂料界的共识。在此背景下,聚脲涂料的水性化技术也已逐渐开始。聚天门冬氨酸酯是一种带仲胺基的脂肪族化合物。相比一般的羟基树脂和环氧树脂,具有更优异的干燥速度。聚天门冬氨酸酯本身分子量小,且自身的官能团结构使得用聚天门冬氨酸酯做出来的涂膜比一般树脂做出来的硬度高。除此之外,聚天门冬氨酸酯支链上高密度的酯键也为大分子链提供了强大的极性基团,从而使得聚合物制品具有很强的内聚力,表现在聚天冬氨酸酯涂膜具有突出的机械强度。
发明内容
为解决现有技术的不足,本发明提供了一种水性聚天门冬氨酸酯分散体及其制备方法以及水性聚脲涂料树脂。本发明制备得到的水性聚天门冬氨酸酯分散体VOC含量低、安全无毒环保、且机械性能和耐化学品性能优异。用该方法制得的水性聚天冬氨酸酯分散体与水性多水性多异氰酸酯固化剂互配使用,可以得到具有施工周期长、便于施工等特点的水性聚脲涂料树脂。
本发明所提供的技术方案如下:
一种水性聚天门冬氨酸酯分散体的制备方法,包括以下步骤:
1)将聚醚胺和聚天门冬氨酸酯树脂在100℃-120℃、负压为0.03MPa-0.06MPa的条件下脱水1h-2h;
2)步骤1)完成后,降温至20℃-60℃,匀速滴加二异氰酸酯,滴加时间控制在0.5h-1.5h,并加入溶剂,滴加完后升温至40℃-80℃,恒温反应1h-3h;
3)将步骤2)所得的产物在50℃-90℃、800-1200r/min条件下缓慢滴加预热的去离子水,0.5h-1.5h滴加完毕,然后在转速为800-1200r/min条件下继续搅拌约0.4h-0.6h,降温出料,即得所述的水性聚天门冬氨酸酯分散体。
上述技术方案中,二异氰酸酯可分别与聚醚胺的胺基或聚天门冬氨酸酯树脂的胺基反应,生成聚脲,构成水性聚天门冬氨酸酯分散体的主要成分。
具体的,步骤2)可为:利用恒压滴定漏斗匀速滴加二异氰酸酯,滴加时间控制在0.5h-1.5h;滴完用适量溶剂冲洗滴液漏斗并滴入烧瓶中,加入升温至40℃-80℃,恒温反应1h-3h。
具体的,步骤1)中:
聚醚胺的平均分子量为600-2000;
聚醚胺的用量与聚醚胺、聚天门冬氨酸酯树脂和二异氰酸酯的总用量的重量百分比为10%-25%。
具体的,聚醚胺选自聚醚胺M600、聚醚胺M1000或聚醚胺M2070中的任意一种或多种的混合。
具体的,步骤)中:
聚天门冬氨酸酯树脂选用F420聚天门冬氨酸酯树脂(例如深圳飞扬骏研新材料股份有限公司的)和F520聚天门冬氨酸酯树脂(例如深圳飞扬骏研新材料股份有限公司的)中的任意一种或两种的混合物;
聚天门冬氨酸酯树脂的用量与聚醚胺、聚天门冬氨酸酯树脂和二异氰酸酯的总用量的重量百分比为70%-82%。
具体的,步骤2)中:
二异氰酸酯选自芳香族二异氰酸酯、脂肪族二异氰酸酯或脂环族二异氰酸酯中的任意一种或多种的混合;
二异氰酸酯与聚醚胺的摩尔比为(1.0-1.05):1。
具体的,二异氰酸酯选自甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、二苯基甲烷二异氰酸酯(MDI)或二环己基甲烷二异氰酸酯(HMDI)中的任意一种或多种的混合。
具体的,步骤2)中:
所述溶剂选用二乙二醇二甲醚、二丙二醇二甲醚、N-甲基吡洛烷酮、二甲基甲酰胺、二甲基乙酰胺一种或两种的混合物;
所述溶剂与所述水性聚天门冬氨酸酯分散体的重量比为5%-20%。
具体的,水性聚天门冬氨酸酯分散体的固含为40%-60%。
本发明还提供了上述制备方法制备得到的水性聚天门冬氨酸酯分散体。
本发明还提供了一种水性聚脲涂料树脂,包括:
本发明所提供的水性聚天门冬氨酸酯分散体;
以及水性多异氰酸酯固化剂。
上述技术方案中,水性聚天门冬氨酸酯分散体中未反应掉的胺基可再与水性多异氰酸酯固化剂反应,生成聚脲。因此,本发明通过所制备的含酰胺基聚天冬氨酸酯作为双组份聚脲的B料树脂,与双组份聚脲的A料含多异氰酸酯固化剂互配使用,生成性能优异的聚脲涂层。
上述技术方案中,水性聚天门冬氨酸酯分散体与水性多异氰酸酯固化剂的重量比按n(NCO):n(活性H)=1.2:1计算。
进一步,还包括基材润湿剂、消泡剂、增稠剂或润湿分散剂中的任意一种或多种,各成分与所述水性聚脲涂料树脂的重量比分别为0.1%-1%。
本发明所提供的水性聚脲涂料的涂膜性能保持了溶剂型聚脲涂料的主要优点,包括室温下快速固化、高光泽度、高透明度以及优良的耐水性、耐腐蚀性和耐紫外光性、耐老化等性能。
附图说明
图1是本发明所合成的水性聚天门冬氨酸酯分散体的IR谱图。其中,3434.62cm-1为N-H键的吸收峰,1735.07cm-1为C=O键的吸收峰,1029.96cm-1为C-O-C键的吸收峰。
具体实施方式
以下对本发明的原理和特征进行描述,所举实施例只用于解释本发明,并非用于限定本发明的范围。
实施例1
在装有搅拌器、加热装置、加料漏斗和氮气入口的四口烧瓶中加入7.200g聚醚胺M1000和39.202gF420(深圳飞扬骏研新材料股份有限公司)聚天门冬氨酸酯,在110℃、负压为0.05MPa真空脱水1h;降温至40℃,利用恒压滴定漏斗匀速滴加1.598g异佛尔酮二异氰酸酯(IPDI),控制在0.5h内滴完;滴完后用12.00g二丙二醇二甲醚冲洗恒压滴定漏斗并滴入反应烧瓶中,升温至50℃,继续反应1h;提高转速到1000r/min,换恒压滴定漏斗缓慢滴加去离子水36.00g,控制在0.5h内滴完,降温出料,即可得到固含为50%的水性聚天门冬氨酸酯的分散体。
实施例2
在装有搅拌器、加热装置、加料漏斗和氮气入口的四口烧瓶中加入7.167g聚醚胺M2070、15.877gF420(深圳飞扬骏研新材料股份有限公司)聚天门冬氨酸酯和5.000F520(深圳飞扬骏研新材料股份有限公司)聚天门冬氨酸酯,在105℃、负压为0.05MPa真空脱水1h;降温至50℃,利用恒压滴定漏斗匀速滴加0.624g甲苯二异氰酸酯(TDI),控制在0.5h内滴完;滴完后用3.185g丙二醇甲醚冲洗恒压滴定漏斗并滴入反应烧瓶中,升温至60℃,继续反应1.5h;提高转速到1200r/min,换恒压滴定漏斗缓慢滴加去离子水39.817g,控制在0.5h内滴完,降温出料,即可得到固含为40%的水性聚天门冬氨酸酯的分散体。
实施例3
在装有搅拌器、加热装置、加料漏斗和氮气入口的四口烧瓶中加入6.857g聚醚胺M600、24.434gF420(深圳飞扬骏研新材料股份有限公司),在105℃、负压为0.05MPa真空脱水1h;降温至45℃,利用恒压滴定漏斗匀速滴加3.144g二环己基甲烷二异氰酸酯(HMDI),控制在1h内滴完;滴完后用6.077g N-甲基吡洛烷酮冲洗恒压滴定漏斗并滴入反应烧瓶中,升温至55℃,继续反应3h;提高转速到1200r/min,换恒压滴定漏斗缓慢滴加去离子水16.88g,控制在0.5h内滴完,降温出料,即可得到固含为60%的水性聚天门冬氨酸酯的分散体。
实施例4
将实施例1、实施例2、实施例3中水性聚天门冬氨酸酯分散体分别与科思创水性固化剂XP2655组成双组份涂料,并加入适量的涂料助剂,按相应比例混合均匀,涂覆于打磨的马口铁板上,可以形成性能优良的聚脲涂层,其表干时间均约30min,施工期约2h,光泽(60°)均大于100,拉伸强度均大于16MPa,断裂伸长率均可达420%以上。其中,水性固化剂XP2655是科思创基于六亚甲基二异氰酸酯(HDI)的亲水性脂肪族聚异氰酸酯,供应形式100%,NCO含量为21%。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种水性聚天门冬氨酸酯分散体的制备方法,其特征在于,包括以下步骤:
1)将聚醚胺和聚天门冬氨酸酯树脂在100℃-120℃、负压为0.03MPa-0.06MPa的条件下脱水1h-2h;
2)步骤1)完成后,降温至20℃-60℃,匀速滴加二异氰酸酯,滴加时间控制在0.5h-1.5h,并加入溶剂,滴加完后升温至40℃-80℃,恒温反应1h-3h;
3)将步骤2)所得的产物在50℃-90℃、800-1200r/min条件下缓慢滴加预热的去离子水,0.5h-1.5h滴加完毕,然后在转速为800-1200r/min条件下继续搅拌约0.4h-0.6h,降温出料,即得所述的水性聚天门冬氨酸酯分散体。
2.根据权利要求1所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于,步骤1)中:
聚醚胺的平均分子量为600-2000;
聚醚胺的用量与聚醚胺、聚天门冬氨酸酯树脂和二异氰酸酯的总用量的重量百分比为10%-25%。
3.根据权利要求2所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于:聚醚胺选自聚醚胺M600、聚醚胺M1000或聚醚胺M2070中的任意一种或多种的混合。
4.根据权利要求1所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于,步骤)中:
聚天门冬氨酸酯树脂选用F420聚天门冬氨酸酯树脂和F520聚天门冬氨酸酯树脂中的任意一种或两种的混合物;
聚天门冬氨酸酯树脂的用量与聚醚胺、聚天门冬氨酸酯树脂和二异氰酸酯的总用量的重量百分比为70%-82%。
5.根据权利要求1所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于,步骤2)中:
二异氰酸酯选自芳香族二异氰酸酯、脂肪族二异氰酸酯或脂环族二异氰酸酯中的任意一种或多种的混合;
二异氰酸酯与聚醚胺的摩尔比为(1.0-1.05):1。
6.根据权利要求5所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于:二异氰酸酯选自甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二苯基甲烷二异氰酸酯或二环己基甲烷二异氰酸酯中的任意一种或多种的混合。
7.根据权利要求1所述的水性聚天门冬氨酸酯分散体的制备方法,其特征在于,步骤2)中:
所述溶剂选用二乙二醇二甲醚、二丙二醇二甲醚、N-甲基吡洛烷酮、二甲基甲酰胺、二甲基乙酰胺一种或两种的混合物;
所述溶剂与所述水性聚天门冬氨酸酯分散体的重量比为5%-20%。
8.一种根据权利要求1至7任一所述的制备方法制备得到的水性聚天门冬氨酸酯分散体。
9.一种水性聚脲涂料树脂,其特征在于,包括:
权利要求8所述的水性聚天门冬氨酸酯分散体;
以及水性多异氰酸酯固化剂。
10.根据权利要求9所述的水性聚脲涂料树脂,其特征在于:还包括基材润湿剂、消泡剂、增稠剂或润湿分散剂中的任意一种或多种,各成分与所述水性聚脲涂料树脂的重量比分别为0.1%-1%。
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