CN114381194A - 一种竹炭改性水性聚氨酯涂料及其制备方法和应用 - Google Patents
一种竹炭改性水性聚氨酯涂料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及建筑涂料制备技术领域,具体来说是一种竹炭改性水性聚氨酯涂料及其制备方法和应用,竹炭改性水性聚氨酯涂料由如下重量份数的原料制成:竹炭80‑180份;多元醇30‑70份;二异氰酸酯20‑50份;改性聚丙烯腈纤维20‑50份,改性方式为水解改性。本发明对水性聚氨酯采用竹炭和改性聚丙烯腈纤维进行了改性,制得了一种环保、价格低廉的竹炭改性水性聚氨酯涂料。
Description
技术领域
本发明涉及建筑涂料制备技术领域,具体来说是一种竹炭改性水性聚氨酯涂料及其制备方法和应用。
背景技术
水性聚氨酯是以水为分散介质,聚氨酯树脂溶解或分散于水中而形成的二元胶态体系,以其制备的水性聚氨酯涂料中不含或含有极少量的有机溶剂。水性聚氨酯涂料不仅具有无毒无臭味、无污染、不易燃烧、成本低、不易损伤被涂饰表面、施工方便、易于清理等优点,还具有溶剂型聚氨酯涂料所固有的高硬度、耐磨损等优异性能,因而在木器涂料、汽车涂料、建筑涂料、塑料涂料、纸张涂层以及织物和皮革涂饰等许多领域得到了广泛的应用。
为了满足人们在生产和生活方面对具有新型功能水性聚氨酯的需求,近年来人们对水性聚氨酯进行了一系列改性,并赋予了水性聚氨酯不同的物理化学性能,继而提升了聚氨酯的功能性。
水性聚氨酯涂料含有高分子树脂、颜填料、助剂和水等多种物质,为微生物的生存提供了充足的营养条件,因此极易受到微生物的污染;受污染的水性聚氨酯涂料会发生霉变、变质,进而散发不愉快气味,产生色变,不仅丧失了对基材的保护作用,还对人体健康造成危害。现有技术的解决方法是在水性涂料中添加适量的防霉杀菌剂,来抑制微生物的生长与繁殖,保护涂料与涂层不受破坏;常用的防霉杀菌剂包括无机杀菌剂和有机杀菌剂,无机杀菌剂包括银、纳米二氧化钛和纳米氧化锌等;有机杀菌剂包括季铵盐类、酚类、吡啶类、哌三嗪类,虽然现有技术的杀菌剂杀菌效果较为明显,但是相对来说,无机杀菌剂价格较为昂贵,而有机杀菌剂对人体具有一定的副作用。
竹炭是竹材高温热解的主要产品,其显微构造类似并接近于洋葱状富勒烯碳和展开的碳纳米管的特殊结构,因此竹炭具有疏松多孔的结构,其分子细密多孔,比表面积大,若周围环境湿度大时,可吸收水分,若周围环境干燥,则可释放水分;同时具有很强的吸附能力,对硫化物、氢化物、甲醇、苯、酚等有害化学物质起到吸附、分解异味和消臭作用,能净化空气、消除异味、吸湿防霉、抑菌驱虫,已被广泛应用于日常生活中,同时竹炭无毒且价格低廉,若能够将竹炭与水性聚氨酯进行复合并制成涂料,则在一定程度上实现了环保的同时有效降低了成本。
发明内容
针对上述存在的技术不足,本发明的目的是提供了一种竹炭改性水性聚氨酯涂料及其制备方法和应用,本发明对水性聚氨酯采用竹炭和改性聚丙烯腈纤维进行了改性,制得了一种环保、价格低廉的竹炭改性水性聚氨酯涂料。
为解决上述技术问题,本发明采用如下技术方案:
一种竹炭改性水性聚氨酯涂料,由如下重量份数的原料制成:竹炭80-180份;多元醇30-70份;二异氰酸酯20-50份;改性聚丙烯腈纤维20-50份,所述改性方式为水解改性。
优选的,还包括10-15份相容剂,所述相容剂为马来酸酐接枝相容剂。
优选的,所述二异氰酸酯选自亚甲基双-4,4'-环己基二异氰酸酯、异佛尔酮二异氰酸酯、己二异氰酸酯的三异氰酸酯、四亚甲基-1,4-二异氰酸酯、1,6-己二异氰酸酯、环己基二异氰酸酯、甲基环已烯二异氰酸酯、环已烷-1,4-二异氰酸酯、二环己基甲烷二异氰酸酯中的一种或多种的混合物。
优选的,所述多元醇选自丙二醇、二乙二醇、1,4-丁二醇中的一种或几种的混合物。
优选的,所述改性聚丙烯腈纤维按照如下步骤制备:
将聚丙烯腈纤维加入至NaOH溶液中,于90-100℃下水解2-3h后,过滤、水洗至中性,干燥至恒重,得到改性聚丙烯腈纤维;
所述聚丙烯腈纤维的质量与NaOH溶液的体积比为1g:15-20mL,所述NaOH溶液的体积分数为30-40%。
本发明还保护了一种竹炭改性水性聚氨酯涂料的制备方法,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭80-180份,多元醇30-70份,二异氰酸酯20-50份,改性聚丙烯腈纤维20-50份,备用;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将多元醇和二异氰酸酯于催化条件下,80-90℃下反应1.5-2.5h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,多元醇和二异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为150-180:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维于醇溶液中混合,于70-120℃下反应6-10h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
优选的,所述步骤(1)称量的原料中还包括了10-15份相容剂,并于步骤(2)中同竹炭和改性聚丙烯腈纤维一起与聚氨酯预聚体混合,然后反应。
优选的,所述改性聚丙烯腈纤维在制备竹炭改性水性聚氨酯涂料前先粉碎至粒径400-800目。
本发明还保护了竹炭改性水性聚氨酯涂料在制备建筑内墙涂料中的应用。
与现有技术相比,本发明具有的有益效果是:
1、本发明先制得改性聚丙烯腈纤维,具体将聚丙烯腈纤维进行水解反应,使得聚丙烯腈表面的氰键发生部分水解,实现聚丙烯腈纤维上部分的-CN被水解成-COOH或-CONH2;而这两个基团均能够与聚氨酯预聚体结构中的异氰酸酯基发生反应,实现改性聚丙烯腈纤维与聚氨酯预聚体的稳定接枝。
2、竹炭改性水性聚氨酯涂料由竹炭、多元醇、二异氰酸酯、改性聚丙烯腈纤维制成,竹炭表面含有多种含氧官能团,如羟基、羧基等,因此在与聚氨酯预聚体高温共混后能够发生化学反应,并将竹炭接枝于聚氨酯预聚体上;本发明以聚氨酯预聚体为中心,将竹炭与聚氨酯预聚体进行自由基聚合反应,通过羟基和异氰酸酯基的反应实现接枝,同时将改性聚丙烯腈纤维与聚氨酯预聚体发生反应,实现了三者的稳定接枝,使得竹炭和改性聚丙烯腈纤维均稳定接枝在聚氨酯预聚体上,得到了竹炭改性水性聚氨酯材料,其稳定分散于醇溶剂中,得到了涂料。
3、本发明中通过采用竹炭来替代现有技术的杀菌剂,接枝在聚氨酯预聚体上,不仅提升了竹炭的稳定性,而且实现了制备环保、廉价涂料的目的;同时采用了改性聚丙烯腈纤维,通过聚丙烯腈纤维提升整个竹炭改性水性聚氨酯涂料的耐水性,继而避免由于竹炭吸水后,导致聚氨酯遇水发生溶胀或溶解,影响竹炭改性水性聚氨酯涂料的装饰性能,还使得涂料丧失了对基材的防水和保护性能。
4、本发明还包括了马来酸酐接枝相容剂,马来酸酐接枝相容剂促进了分子间的结合变成分子键的结合,提升三者的结合力,同时提升整个材料的力学性能。
具体实施方式
下面对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。本发明各实施例中所述实验方法,如无特殊说明,均为常规方法。
本发明实施例所使用的改性聚丙烯腈纤维均按照如下步骤制备:
将聚丙烯腈纤维加入至体积分数为35%的NaOH溶液中,于90℃下水解3h后,过滤、水洗至中性,干燥至恒重,得到改性聚丙烯腈纤维;
其中,所述聚丙烯腈纤维的质量与NaOH溶液的体积比为1g:20mL。
实施例1
一种竹炭改性水性聚氨酯涂料的制备方法,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭80份,二乙二醇30份,己二异氰酸酯的三异氰酸酯50份,改性聚丙烯腈纤维20份,备用;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将二乙二醇和二异氰酸酯的三异氰酸酯于催化条件下,80℃下反应2.5h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,二乙二醇和二异氰酸酯的三异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为150:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维于醇溶液中混合,于120℃下反应10h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
实施例2
一种竹炭改性水性聚氨酯涂料的制备方法,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭150份,丙二醇40份,异佛尔酮二异氰酸酯30份,改性聚丙烯腈纤维40份,备用;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将丙二醇和异佛尔酮二异氰酸酯于催化条件下,85℃下反应2h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,丙二醇和异佛尔酮二异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为170:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维于醇溶液中混合,于100℃下反应8h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
实施例3
一种竹炭改性水性聚氨酯涂料的制备方法,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭180份,1,4-丁二醇70份,四亚甲基-1,4-二异氰酸酯20份,改性聚丙烯腈纤维50份,备用;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将1,4-丁二醇和四亚甲基-1,4-二异氰酸酯于催化条件下,90℃下反应1.5h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,1,4-丁二醇和四亚甲基-1,4-二异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为180:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维于醇溶液中混合,于70℃下反应6h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
实施例4
一种竹炭改性水性聚氨酯涂料的制备方法,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭150份,丙二醇40份,异佛尔酮二异氰酸酯30份,改性聚丙烯腈纤维40份,马来酸酐接枝相容剂15份;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将丙二醇和异佛尔酮二异氰酸酯于催化条件下,85℃下反应2h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,丙二醇和异佛尔酮二异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为170:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维、马来酸酐接枝相容剂于醇溶液中混合,于100℃下反应8h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
本发明实施例1-实施例4均制得性能优异的建筑内墙涂料,下面以实施例1-实施例4的竹炭改性水性聚氨酯涂料为例,进行涂料自身性能和使用性能的研究,具体研究方法和结果如下所示:
(1)采用本领域常规检测方法获得实施例1-4竹炭改性水性聚氨酯涂料的理化性能,检测其应用性能,结果如表1所示:
表1本发明实施例1-4的竹炭改性水性聚氨酯涂料常规使用性能表
项目 | 指标 | 结果 |
容器中状态 | 无硬块,搅拌后呈均匀状态 | 合格 |
施工性能 | 刷涂二道无障碍 | 合格 |
低温稳定性 | 不变质 | 合格 |
干燥时间(表干)/h≤ | 2 | 合格 |
涂膜外观 | 正常 | 合格 |
耐碱性 | 24小时无异常 | 合格 |
耐洗刷性/次≥ | 1000 | 合格 |
对比率(白色)≥ | 0.95 | 0.97 |
结果表明,实施例1-4制得的竹炭改性水性聚氨酯涂料指标均达到国家标准GB/T9756-2009合成树脂乳液内墙涂料标准,能够被作为建筑内墙涂料进行推广应用。
(2)将本发明实施例1-4制得的竹炭改性水性聚氨酯涂料分别用于进行甲醛净化性能的研究,将甲醛净化效果持久性检验结果与国家建材行业标准JC/T1074-2008《室内空气净化功能涂覆材料净化性能》中I类规定进行对比,具体检测结果如表2所示:
表2本发明实施例1-4的竹炭改性水性聚氨酯涂料甲醛净化结果对照表
结果表明,由于竹炭的稳定复合接枝,使得涂料具备了优异的甲醛净化性能,且实现了长久有效地甲醛净化。
(3)本发明对实施例1-4的竹炭改性水性聚氨酯涂料抗菌性能也进行了研究和评价,具体研究方法和结果如下所示:
测试的细菌为分别为金黄色葡萄球菌和大肠杆菌,参照最小抑菌浓度(minimalinhibitory concentration,MIC)的测试方法;称取一定量的实施例1-4的涂料,将涂料用MH肉汤稀释到不同浓度,使最终菌液的浓度达到106个/mL,然后在37℃下震荡培养24h,观察并对照结果,如表3所示;不加抗菌样品作为对照,无菌生长的实验管液体透明,以不长菌管的抗菌剂计量为该抗菌剂的最低抑菌浓度(MIC);
表3实施例1-4及对照组抗菌性能的对照表
结果表明,本发明实施例1-4制得的竹炭改性水性聚氨酯涂料均具有优异的抑菌性能,这得益于竹炭。
(4)本发明实施例1-4制得的竹炭改性水性聚氨酯涂料力学性能基本平行,下面以实施例2制得的竹炭改性水性聚氨酯涂料为例,进行自身力学性能的评价,研究结果如表4所示:
表4实施例2竹炭改性水性聚氨酯涂料性能测试结果表
结果表明本发明实施例2制得的竹炭改性水性聚氨酯涂料具有优异的力学性能。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (9)
1.一种竹炭改性水性聚氨酯涂料,其特征在于,由如下重量份数的原料制成:竹炭80-180份;多元醇30-70份;二异氰酸酯20-50份;改性聚丙烯腈纤维20-50份,所述改性方式为水解改性。
2.根据权利要求1所述的一种竹炭改性水性聚氨酯涂料,其特征在于,还包括10-15份相容剂,所述相容剂为马来酸酐接枝相容剂。
3.根据权利要求1所述的一种竹炭改性水性聚氨酯涂料,其特征在于,所述二异氰酸酯选自亚甲基双-4,4'-环己基二异氰酸酯、异佛尔酮二异氰酸酯、己二异氰酸酯的三异氰酸酯、四亚甲基-1,4-二异氰酸酯、1,6-己二异氰酸酯、环己基二异氰酸酯、甲基环已烯二异氰酸酯、环已烷-1,4-二异氰酸酯、二环己基甲烷二异氰酸酯中的一种或多种的混合物。
4.根据权利要求1所述的一种竹炭改性水性聚氨酯涂料,其特征在于,所述多元醇选自丙二醇、二乙二醇、1,4-丁二醇中的一种或几种的混合物。
5.根据权利要求1所述的一种竹炭改性水性聚氨酯涂料,其特征在于,所述改性聚丙烯腈纤维按照如下步骤制备:
将聚丙烯腈纤维加入至NaOH溶液中,于90-100℃下水解2-3h后,过滤、水洗至中性,干燥至恒重,得到改性聚丙烯腈纤维;
所述聚丙烯腈纤维的质量与NaOH溶液的体积比为1g:15-20mL,所述NaOH溶液的体积分数为30-40%。
6.一种权利要求1-5任一项所述的一种竹炭改性水性聚氨酯涂料的制备方法,其特征在于,包括如下步骤:
(1)称量:按照如下重量份数称取原料:竹炭80-180份,多元醇30-70份,二异氰酸酯20-50份,改性聚丙烯腈纤维20-50份,备用;
(2)竹炭改性水性聚氨酯涂料的制备:
S1、于氮气气氛中,将多元醇和二异氰酸酯于催化条件下,80-90℃下反应1.5-2.5h,得到聚氨酯预聚体;
其中,所述催化条件的催化剂为二月桂酸二丁基锡,多元醇和二异氰酸酯总物质的量与二月桂酸二丁基锡物质的量之比为150-180:1;
S2、将S1制得的聚氨酯预聚体与竹炭、改性聚丙烯腈纤维于醇溶液中混合,于70-120℃下反应6-10h后,冷却至室温,得到竹炭改性水性聚氨酯涂料。
7.根据权利要求6所述的一种竹炭改性水性聚氨酯涂料的制备方法,其特征在于,所述步骤(1)称量的原料中还包括了10-15份相容剂,并于步骤(2)中同竹炭和改性聚丙烯腈纤维一起与聚氨酯预聚体混合,然后反应。
8.根据权利要求6所述的一种竹炭改性水性聚氨酯涂料的制备方法,其特征在于,所述改性聚丙烯腈纤维在制备竹炭改性水性聚氨酯涂料前先粉碎至粒径400-800目。
9.根据权利要求1所述的竹炭改性水性聚氨酯涂料在制备建筑内墙涂料中的应用。
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