CN112625209A - 一种自吸附型抗菌水性固化剂及其制备方法 - Google Patents
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Abstract
本发明涉及一种自吸附型抗菌水性固化剂,按重量份计,其组分为:三聚体100.0~200.0份、二羟甲基丙酸3.0~8.0份、醇酸树脂6.0~18.0份、三碟烯衍生物3.0~6.0份、2‑羟基查尔酮1.5~2.5份、多元醇2.0~5.0份、二月桂酸二丁基锡0.01~0.1份、中和剂2.5~10.0份、惰性溶剂15.0~30.0份;其中,所述的三碟烯衍生物由2,6,14‑三氨基三蝶烯与羟基香茅醛通过反应制得;本发明提供一种自吸附型抗菌水性固化剂,具有优异的抗划伤性、抗菌性能好、耐水性好、耐老化性优、耐盐雾性良好、吸附能力强等特点,与水性羟基组分配制的聚氨酯漆时,无需外加抗菌剂与吸附剂,其具备良好的抗菌性与吸附性能。
Description
技术领域
本发明涉及一种水性固化剂,尤其涉及到一种自吸附型抗菌水性固化剂及其制备方法,属于合成特种功能水性固化剂技术领域。
背景技术
固化剂是一类增进或控制固化反应的物质或混合物,在现有的油性和水性涂料中,为了加快涂料的固化速度、提高漆膜的各项性能,也需要在涂料中添加固化剂。水性涂料中最具代表性的双组分水性聚氨酯涂料,它不含或含很少量的有机溶剂,具有较好的分散稳定性,其保留了传统的溶剂型聚氨酯涂料的一些优良性能,但也具有一定的局限性。
目前,无论是家庭装修还是木器的涂饰或其他涂装等,或多或少都会产生挥发性有机物,挥发性有机物(VOCs)的无组织排放不仅会造成资源的大量浪费,还会引发环境污染,严重危害人体健康。而三蝶烯及其衍生物是一类具有独特的三维刚性结构的化合物,它们在过去的20多年内受到了人们很大的关注,并已在包括分子机器、材料化学以及超分子化学等许多领域内得到了广泛的应用。三蝶烯具有的无定形结构、高稳定性及有机微孔等特性,因而在气体吸附、氢气储存、气体分离等领域具有广泛的应用。
中国专利CN102050935A公开了一种水性聚氨酯固化剂及其制备方法,其包括甲苯二异氰酸酯、三羟甲基丙烷、聚乙二醇、聚碳酸酯二醇、醋酸乙酯和催化剂;制备方法的步骤为:加入18~25%甲苯二异氰酸酯、20.01~80%醋酸乙醋和0.01~40%聚碳酸酯二醇,然后,把1~5%三轻甲基丙烷分三批投入反应,然后,将0.01~40%聚乙二醇分两批投入反应,然后在58~63℃保温3h,加入0.1~0.5%的催化剂,在50℃~60℃之间保温反应2.5~4h,冷却至20~30℃,即可出料;其所制备的水性固化剂具有很大局限性,难以适应复杂的应用环境,其不具备抗菌性与吸附性能。
发明内容
本发明的目的旨在提供一种自吸附型抗菌水性固化剂。
本发明的另一目的提供一种自吸附型抗菌水性固化剂的制备方法。
三蝶烯具有独特的三维刚性结构,该化合物具有3个开放式富电子空腔,具有很强的配位能力和有机吸附能力。三蝶烯结构的引入也可以提高材料分子排列的有序性和空间上的延伸性.基于三蝶烯的多孔聚合材料,它具有良好的吸附能力,可用作潜在的吸附材料。
为解决上述问题本发明引入三碟烯,首先将三碟烯制备成三碟烯衍生物,三碟烯衍生物具有席夫碱结构,其具有良好的抗菌与杀菌性能,同时三碟烯具有良好的吸附性能。
本发明所述的一种自吸附型抗菌水性固化剂,采取以下技术方案:按重量份计,其组分为:三聚体100.0~200.0份、二羟甲基丙酸3.0~8.0份、醇酸树脂6.0~18.0份、三碟烯衍生物3.0~6.0份、2-羟基查尔酮1.5~2.5份、多元醇2.0~5.0份、二月桂酸二丁基锡0.01~0.1份、中和剂2.5~10.0份、惰性溶剂15.0~30.0份。
其中,所述的三碟烯衍生物由2,6,14-三氨基三蝶烯与羟基香茅醛通过反应制得。
所述的三聚体为异佛尔酮二异氰酸酯三聚体、六亚甲基二异氰酸酯三聚体中的一种或两种的组合。
所述的多元醇为1,4-环己烷二甲醇、1,4-丁二醇、乙二醇、新戊二醇、丙二醇、三羟甲基丙烷中的一种或几种的组合。
所述的惰性溶剂为二乙二醇乙醚醋酸酯、N-甲基吡咯烷酮、丙二醇甲醚醋酸酯、丙二醇乙醚醋酸酯中的一种或几种的组合。
所述的中和剂为三乙胺、碳酸氢钠中的一种或两种的组合。
本发明提供一种自吸附型抗菌水性固化剂的制备方法,包括以下步骤:
a)、预先对惰性溶剂、多元醇进行除水处理,得到预处理混合液;
b)、在反应器中通入氮气,按配方量加入上述预处理混合液、三碟烯衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解;
c)、加入三聚体,在82~84℃保温搅拌反应2.0~2.5h,检测NCO值,滴加二月桂酸二丁基锡,升温至86~88℃保温反应1.5~2.0h,检测NCO值,当NCO值与设计值一致为止;
d)、降温,加入中和剂,分散均匀,过滤,出料,即得自吸附型抗菌水性固化剂。
本发明所述的三碟烯衍生物,其制备步骤如下:
按配方量(2,6,14-三氨基三蝶烯与羟基香茅醛的摩尔比为1:3),在反应釜中,加入2,6,14-三氨基三蝶烯和适量乙醇,升温至82~84℃搅拌均匀;另外按配方量称取羟基香茅醛缓慢加入反应釜中,加入少量冰醋酸,继续回流反应12.0~14.0h,冷却,真空干燥,即得三碟烯衍生物。
本发明提供一种自吸附型抗菌水性固化剂,具有优异的抗划伤性、抗菌性能好、耐水性好、耐老化性优、耐盐雾性良好、吸附能力强等特点,与水性羟基组分配制的聚氨酯漆时,无需外加抗菌剂与吸附剂,其具备良好的抗菌性与吸附性能。
具体实施方式
下面结合实施例对本发明的一种自吸附型抗菌水性固化剂做进一步的描述。可以理解的是,此处所描述的具体实施例仅仅用于解释相关发明,而非对该发明的限定。
实施例1
一种自吸附型抗菌水性固化剂,按重量份计,其组分为:异佛尔酮二异氰酸酯三聚体180.0份、二羟甲基丙酸6.0份、醇酸树脂14.0份、三碟烯衍生物4.5份、2-羟基查尔酮2.0份、1,4-丁二醇3.0份、二月桂酸二丁基锡0.05份、三乙胺6.0份、二乙二醇乙醚醋酸酯25.0份。
本实施例中一种自吸附型抗菌水性固化剂的制备方法,包括以下步骤:
a)、预先对二乙二醇乙醚醋酸酯、1,4-丁二醇进行除水处理,得到预处理混合液;
b)、在反应器中通入氮气,按配方量加入上述预处理混合液、三碟烯衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解;
c)、加入异佛尔酮二异氰酸酯三聚体,在82~84℃保温搅拌反应2.5h,检测NCO值,滴加二月桂酸二丁基锡,升温至86~88℃保温反应2.0h,检测NCO值,当NCO值与设计值一致为止;
d)、降温,加入三乙胺,分散均匀,过滤,出料,即得自吸附型抗菌水性固化剂。
实施例2
一种自吸附型抗菌水性固化剂,按重量份计,其组分为:六亚甲基二异氰酸酯三聚体150.0份、二羟甲基丙酸5.5份、醇酸树脂13.0份、三碟烯衍生物4.0份、2-羟基查尔酮1.5份、新戊二醇4.0份、二月桂酸二丁基锡0.05份、碳酸氢钠6.5份、丙二醇甲醚醋酸酯22.0份。
本实施例中一种自吸附型抗菌水性固化剂的制备方法,包括以下步骤:
a)、预先对丙二醇甲醚醋酸酯、新戊二醇进行除水处理,得到预处理混合液;
b)、在反应器中通入氮气,按配方量加入上述预处理混合液、三碟烯衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解;
c)、加入六亚甲基二异氰酸酯三聚体,在82~84℃保温搅拌反应2.5h,检测NCO值,滴加二月桂酸二丁基锡,升温至86~88℃保温反应1.5h,检测NCO值,当NCO值与设计值一致为止;
d)、降温,加入碳酸氢钠,分散均匀,过滤,出料,即得自吸附型抗菌水性固化剂。
实施例3
一种自吸附型抗菌水性固化剂,按重量份计,其组分为:六亚甲基二异氰酸酯三聚体130.0份、二羟甲基丙酸5.0份、醇酸树脂10.0份、三碟烯衍生物4.0份、2-羟基查尔酮2.5份、丙二醇1.5份、三羟甲基丙烷1.0份、二月桂酸二丁基锡0.05份、三乙胺5.0份、丙二醇乙醚醋酸酯20.0份。
本实施例中一种自吸附型抗菌水性固化剂的制备方法,包括以下步骤:
a)、预先对丙二醇乙醚醋酸酯、丙二醇、三羟甲基丙烷进行除水处理,得到预处理混合液;
b)、在反应器中通入氮气,按配方量加入上述预处理混合液、三碟烯衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解;
c)、加入六亚甲基二异氰酸酯三聚体,在82~84℃保温搅拌反应2.0h,检测NCO值,滴加二月桂酸二丁基锡,升温至86~88℃保温反应2.0h,检测NCO值,当NCO值与设计值一致为止;
d)、降温,加入三乙胺,分散均匀,过滤,出料,即得自吸附型抗菌水性固化剂。
对本发明的实施例与对比例(市售水性固化剂)与水性羟基丙烯酸树脂配制成水性罩光涂料后,实施例对应的涂料分别为涂料1、涂料2、涂料3、对比例对应的为涂料4,按照相关标准,对漆膜性能进行对比检测,检测的性能指标如表1所示。
表1:水性罩光涂料性能技术指标
检测项目 | 涂料1 | 涂料2 | 涂料3 | 涂料4 |
耐水性/480h | 漆膜正常 | 漆膜正常 | 漆膜正常 | 漆膜发白 |
附着力 | 0级 | 0级 | 0级 | 1级 |
硬度 | 2H | 2H | 2H | H |
耐盐雾性 | 900h | 860h | 840h | 600h |
耐沸水/煮1h | 漆膜正常 | 漆膜正常 | 漆膜正常 | 漆膜发白 |
耐碱性(50g/L NaOH)/480h | 漆膜正常 | 漆膜正常 | 漆膜正常 | 漆膜发白 |
耐酸性(50g/L H2SO4)/480h | 漆膜正常 | 漆膜正常 | 漆膜正常 | 漆膜发白 |
耐油性(92<sup>#</sup>汽油)/120h | 漆膜正常 | 漆膜正常 | 漆膜正常 | 漆膜起泡 |
抗菌性(枯草杆菌) | 99.78% | 99.71% | 99.65% | 45.62% |
吸附性能测试:
对同样新装修的2个实验房子,每个房子均为50m2,初始测得甲醛的浓度为2.68mg/m3、苯的浓度为1.98mg/m3、一氧化碳的浓度为45.6mg/m3、氨的浓度为1.32mg/m3,分别涂覆本发明的涂料1(为例)与对比例涂料4,密封48h后进行空气质量检测:
涂覆本发明样品涂料1(为例)的实验房子:
甲醛的浓度为0.03mg/m3、苯的浓度为0.04mg/m3、一氧化碳的浓度为5.32mg/m3、氨的浓度为0.03mg/m3。
涂覆对比例涂料4的实验房子:
甲醛的浓度为1.79mg/m3、苯的浓度为1.63mg/m3、一氧化碳的浓度为38.2mg/m3、氨的浓度为0.95mg/m3。
尽管本发明已作了详细说明并引证了实施例,但对于本领域的普通技术人员,显然可以按照上述说明而做出的各种方案、修改和改动,都应该包括在权利要求的范围之内。
Claims (7)
1.一种自吸附型抗菌水性固化剂,其特征在于,所述的自吸附型抗菌水性固化剂,按重量份计,其组分为:三聚体100.0~200.0份、二羟甲基丙酸3.0~8.0份、醇酸树脂6.0~18.0份、三碟烯衍生物3.0~6.0份、2-羟基查尔酮1.5~2.5份、多元醇2.0~5.0份、二月桂酸二丁基锡0.01~0.1份、中和剂2.5~10.0份、惰性溶剂15.0~30.0份;
其中,所述的三碟烯衍生物由2,6,14-三氨基三蝶烯与羟基香茅醛通过反应制得。
2.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的三聚体为异佛尔酮二异氰酸酯三聚体、六亚甲基二异氰酸酯三聚体中的一种或两种的组合。
3.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的多元醇为1,4-环己烷二甲醇、1,4-丁二醇、乙二醇、新戊二醇、丙二醇、三羟甲基丙烷中的一种或几种的组合。
4.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的惰性溶剂为二乙二醇乙醚醋酸酯、N-甲基吡咯烷酮、丙二醇甲醚醋酸酯、丙二醇乙醚醋酸酯中的一种或几种的组合。
5.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的中和剂为三乙胺、碳酸氢钠中的一种或两种的组合。
6.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的自吸附型抗菌水性固化剂,其制备方法,包括以下步骤:
a)、预先对惰性溶剂、多元醇进行除水处理,得到预处理混合液;
b)、在反应器中通入氮气,按配方量加入上述预处理混合液、三碟烯衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解;
c)、加入三聚体,在82~84℃保温搅拌反应2.0~2.5h,检测NCO值,滴加二月桂酸二丁基锡,升温至86~88℃保温反应1.5~2.0h,检测NCO值,当NCO值与设计值一致为止;
d)、降温,加入中和剂,分散均匀,过滤,出料,即得自吸附型抗菌水性固化剂。
7.根据权利要求1所述的自吸附型抗菌水性固化剂,其特征在于:所述的三碟烯衍生物,其制备方法,包括以下步骤:
按配方量(2,6,14-三氨基三蝶烯与羟基香茅醛的摩尔比为1:3),在反应釜中,加入2,6,14-三氨基三蝶烯和适量乙醇,升温至82~84℃搅拌均匀;另外按配方量称取羟基香茅醛缓慢加入反应釜中,加入少量冰醋酸,继续回流反应12.0~14.0h,冷却,真空干燥,即得三碟烯衍生物。
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