CN114045059B - 一种防液体、细菌粘附的电泳漆及其应用方法 - Google Patents
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Abstract
本发明提供一种防液体、细菌粘附的电泳漆,所述电泳漆由高羟值水溶性阳离子树脂、硅改性交联组分和稀释溶剂组成;所述高羟值水溶性阳离子树脂由乙烯基单体在第一反应溶剂中聚合得到,所述乙烯基单体包括共聚单体、阳离子单体和交联单体;所述硅改性交联组分由硅油类液态低表面能化合物与水分散或水溶性氨基树脂在第二反应溶剂中反应得到;本发明所述电泳漆对液体及细菌具有优良的低粘附性。
Description
技术领域
本发明涉及功能涂层及其制备技术领域,具体涉及一种防液体、细菌粘附的电泳漆及其应用方法。
背景技术
人类活动中,液体粘附表面的现象无处不在,但在不少的领域,如防污(水、油性液体和腐蚀性液体)、自清洁、减阻、防堵等,液体粘附带来的影响是消极的;同时,在日常生活环境中,细菌广泛粘附在日用品、家电、医疗器械、建筑墙体及航海船舶等表面,且随细菌的生长,会对表面造成不可逆转的破坏;进一步的,细菌还通过接触而传递至人类皮肤表面并大量繁殖,对人类生活就人体健康造成极大的危害。因此,制备防液体及细菌粘附的表面在实际场景中有着巨大的应用潜力,在学术界和工业界都受到了相当大的关注。
目前主要有微纳级粗糙结构超疏液表面、液体灌注光滑多孔表面、共价接枝防污单分子层和防液体粘附聚合物涂层等防液体及细菌粘附材料。对于微纳级粗糙结构表面,其精细结构固有的刚性及低表面能限制了其与基材的强附着力,同时材料制备过程的复杂也为其在各个领域的工业化应用增加难度。对于液体灌注光滑多孔表面,其在液体聚合物选择方面有明显的复杂性,同时灌注在涂层中的液体聚合物容易通过蒸发等方式流失,且对压力敏感。对于在光滑表面共价接枝柔性单分子层,其制备方法具有复杂性,且所制备表面不耐磨也不耐刮。对于防液体粘附聚合物涂层,能克服上述防液体粘附平滑表面存在的不足,同时具有耐磨性好、附着力强、耐用且厚度可调等特点。然而,目前防液体粘附聚合物涂层通常需要特制的氟化化合物并使用有机溶剂,对环境不友好,同时不利于可持续发展。此外,对于实现复杂器件的防液体及细菌粘附,其涂覆工艺也存在挑战。
发明内容
针对上述现有技术存在的不足之处中的至少一个,本发明提供一种防液体及细菌粘附性能佳、附着性和耐磨性优良的电泳漆。
本发明的目的采用以下技术方案来实现:
一种防液体、细菌粘附的电泳漆,所述电泳漆由高羟值水溶性阳离子树脂、硅改性交联组分和稀释溶剂组成;
所述高羟值水溶性阳离子树脂由乙烯基单体在第一反应溶剂中聚合得到,所述乙烯基单体包括共聚单体、阳离子单体和交联单体,其质量比例为(65-70):(10-15):(20-25);
所述硅改性交联组分由质量比例为(90-95):(5-10)的硅油类液态低表面能化合物与水分散或水溶性氨基树脂在第二反应溶剂中反应得到。
优选的,所述电泳漆中所述高羟值水溶性阳离子树脂、所述硅改性交联组分和所述稀释溶剂的质量百分比分别为(5-10):(10-15):(60-65)。
优选的,所述共聚单体包括丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸丁酯、丙烯酸十八酯、甲基丙烯酸十八酯、丙烯酸异冰片酯、苯乙烯中的一种或几种。
优选的,所述阳离子单体包括丙烯酸二甲氨基乙酯和/或甲基丙烯酸二甲氨基乙酯。
优选的,所述交联单体包括丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯中的一种或几种。
优选的,所述第一反应溶剂为聚合物涂层体系常使用的分散相,包括乙醇、异丙醇、丙酮、丁酮、乙酸乙酯、乙酸丁酯、丙二醇甲醚醋酸酯、丙二醇丁醚醋酸酯、丙二醇甲醚、丙二醇丁醚一种或几种。
优选的,所述硅油类液态低表面能化合物包括分子量50-5000的末端单羟基硅油、支链单羟基硅油、聚醚改性硅油以及羧基改性硅油中的一种或几种。
优选的,所述水分散或水溶性氨基树脂包括CYMEL 325、CQ-8727、MF 921、MF 900一种或几种。
优选的,所述第二反应溶剂为乙醇、异丙醇、丙酮、丁酮、丙二醇甲醚醋酸酯、丙二醇丁醚醋酸酯中的一种或几种。
本发明的另一目的在于提供一种前述的一种防液体、细菌粘附的电泳漆的应用方法,具体包括以下步骤:
(1)按照成分比例配制电泳漆;
(2)设置电压10~30V,电泳时间10~60s;
(3)将导电基底置于所述电泳漆中,开始电泳;
(4)电泳结束后用清水冲洗去掉多余的电泳漆;
(5)对涂层进行温度120℃~180℃,时长为0.5~4h的烘干,使交联成膜。
本发明的有益效果为:
(1)得到了对液体及细菌具有优良低粘附性的涂层材料。
(2)电泳漆的为水分散体系,环保安全。
(3)电泳沉积工艺简单易行,适用于涂层的大规模制备。
(4)电泳漆的制备原料来源广泛,且均为工业化市场化的化工原料。
(5)涂层的防液体粘附原理不依赖于任何微/纳米尺度的粗糙度,而是基于平滑聚合物的交联网络所形成,所制备的涂层具有良好的耐磨性及柔性。
(6)通过将水溶性固化剂进行低表面能改性,固化过程低表面能的聚二甲基硅氧烷自发快速在表面富集,实现使用极少量的聚二甲基硅氧烷便实现了表面防液体及抗菌粘附。
附图说明
利用附图对本发明作进一步说明,但附图中的实施例不构成对本发明的任何限制,对于本领域的普通技术人员,在不付出创造性劳动的前提下,还可以根据以下附图获得其它的附图。
图1是实施例1-4所述涂层对水的接触角结果对比图;
图2是实施例1-4所述涂层对水的滑动角结果对比图;
图3是实施例1所述涂层对不同液体的滑动角结果对比图;
图4是实施例1-4所述涂层对防细菌粘附性能测试结果图;
图5是实施例1所述涂层的柔韧性能测试结果图;
图6是实施例1所述涂层的抗冲击性能测试结果图;
图7是实施例1所述涂层的耐摩擦性能测试结果图。
具体实施方式
结合以下实施例对本发明作进一步描述。
本发明的实施例涉及一种防液体、细菌粘附的电泳漆,其制备方法包括以下步骤:
S1、分别制备高羟值水溶性阳离子树脂和硅改性交联组分,其中:
所述高羟值水溶性阳离子树脂的制备方法为:
按重量份数,将0.2份偶氮二异丁腈作为引发剂,50份丙二醇甲醚醋酸酯作为溶剂混合搅拌,升温至100℃并保温,接着,按表1的配比将共聚单体、阳离子单体和交联单体混合后匀速滴加0.5h,随后,升温至110℃后加入0.2份的偶氮二异丁腈,保温继续反应15h,降温至室温,加入乳酸中和至pH值为7.6,即得到所述高羟值水溶性阳离子树脂,树脂的固含量为44%;
所述共聚单体优选为质量比3:2的甲基丙烯酸甲酯和丙烯酸丁酯;阳离子单体优选为甲基丙烯酸二甲基氨基乙酯;交联单体优选为甲基丙烯酸羟丙酯;
所述硅改性交联组分的制备方法为:
按重量份数,按表1的配比将硅油类液态低表面能化合物和氨基树脂加入到3份对甲苯磺酸催化剂和83份丁酮溶剂的混合溶液中,随后在搅拌下75℃保温反应3h,即得到硅所述改性交联组分,固含量为14%;
所述氨基树脂优选为MF 900,硅油类液态低表面能化合物优选分子量为5000的末端单羟基硅油;
S2、将步骤S1制备得到的高羟值水溶性阳离子树脂和硅改性交联组分分散于水中,制得所述电泳漆;
制备原料明细如表1所示,各实施例用蒸馏水稀释至固含为15%。
所述电泳漆的涂装方法是:
将导电基底置于所述电泳漆中,设置电泳参数电压15V,电泳时间20s,电泳后移出涂覆的导电基底,用清水冲洗去多余电泳漆,并在温度160℃下烘干2h,使其交联成膜。
表1所述防液体、抗菌粘附的电泳漆的制备原料比例表
实验例
对实施例1-4所制备涂层的防液体、细菌粘附性能进行了测试,具体的:
1、防液体性能
参见附图1-2,附图1-2为实施例1~4的水接触角和滑动角测试,接触角所需测试液体为2μL,滑动角所需测试液体为50μL。通过对比实施例1和4可以看出,添加PDMS后滑动角明显降低。随着PDMS添加量的增加(1~5%),涂层的水接触角和滑动角增大。PDMS用量为0.015g(1%)时,具有良好的防液体粘附性能,继续增加PDMS用量,反而会因PDMS链在聚合物体系中的相容性差出现宏观分相,导致性能下降。通过对比实施例4和实施例1可以看出,添加PDMS后,涂层的水接触角增加,滑动角降低。这可以归因于PDMS在涂层表面的覆盖,从而提高其防液体粘附性能,实施例1的防液体粘附效果最佳。
参见附图3,附图3为实施例1涂层分别对水、正十六烷、二碘甲烷和泵油的滑动角测试结果对比,其对水、正十六烷、二碘甲烷、泵油的滑动角分别为14°、3°、5°、10°,表明该涂层可在防污、减阻领域中应用。
2、防细菌粘附性能
用0.05ml大肠杆菌菌液(菌液浓度:108个/ml)滴入装有4.95ml PBS溶液的试管中稀释100倍后,将1cm×1cm的样品分别放入,接种培养24h后,用2ml PBS溶液冲洗已接种样品残余菌液,然后将样品放置装有2ml无菌PBS溶液的试管中,在40kHz下超声3min取0.05ml溶液,滴在培养基进行涂布,在培养基中恒温37℃培养16h,以探究样品的抗细菌粘附能力。实验结果参见附图4。
通过统计培养基表面大肠杆菌数,对比可知,涂层具有良好的抗菌性能。这是归因于基材表面具有低表面能,细菌表面难以和表面发生相互作用,从而降低细菌粘附。通过实施例4和空白对照对比,可知,原料中的阳离子单体甲基丙烯酸二甲基氨基乙酯具有一定的杀菌效果。
3、柔韧性、抗冲击和耐摩擦性能
柔韧性方面,参照GB/T 1731-93《漆膜柔韧性测定法》对涂层进行柔韧性测试,测试结果参见附图5;从图可知,涂层达到了小于1mm的最小弯曲半径。
耐冲击测试方面,采用QCJ-50漆膜冲击器,设置1kg的冲击锤上升至50cm,使其自由落体落下,对实施例1的涂层的耐冲击性能进行测试,参见附图6,结果显示实施例1涂层无破裂现象,滑动角没有变化,漆膜具有理想的耐冲击性。
附图7为实施例1的耐磨擦性能测试结果,由于这种涂层的防液体粘附原理不依赖于任何微/纳米尺度的粗糙度,而是基于平滑聚合物的交联网络所形成,因此表现出了出色的耐磨性。从附图7可看出,即使在18KPa载荷下,在棉布上进行400次磨损循环后,水在涂层表面仍然有出色的防液体黏附效果,表明涂层具有出色的耐磨擦性。
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (1)
1.一种防液体、细菌粘附的电泳漆,其特征在于,制备方法包括以下步骤:
S1、分别制备高羟值水溶性阳离子树脂和硅改性交联组分,所述高羟值水溶性阳离子树脂的制备方法为:
按重量份数,将0.2份偶氮二异丁腈作为引发剂,50份丙二醇甲醚醋酸酯作为溶剂混合搅拌,升温至100℃并保温,将共聚单体9.9份、阳离子单体1.5份和交联单体3份混合后匀速滴加0.5h,随后,升温至110℃后加入0.2份的偶氮二异丁腈,保温继续反应15h,降温至室温,加入乳酸中和至pH值为7.6,即得到所述高羟值水溶性阳离子树脂,树脂的固含量为44%;
所述共聚单体为质量比3:2的甲基丙烯酸甲酯和丙烯酸丁酯;所述阳离子单体为甲基丙烯酸二甲基氨基乙酯;所述交联单体为甲基丙烯酸羟丙酯;
所述硅改性交联组分的制备方法为:
按重量份数,将0.015份、0.04份或0.07份的硅油类液态低表面能化合物和氨基树脂0.45份加入到3份对甲苯磺酸催化剂和83份丁酮溶剂的混合溶液中,随后在搅拌下75℃保温反应3h,即得到硅所述改性交联组分,固含量为14%;
所述氨基树脂为MF 900,所述硅油类液态低表面能化合物为分子量5000的末端单羟基硅油;
S2、将步骤S1制备得到的高羟值水溶性阳离子树脂和硅改性交联组分分散于水中,稀释至固含为15%,制得所述电泳漆。
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