CN112745738A - 用于水利工程的劣化免疫仿生防护涂层及其制备方法 - Google Patents
用于水利工程的劣化免疫仿生防护涂层及其制备方法 Download PDFInfo
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- CN112745738A CN112745738A CN202011577851.4A CN202011577851A CN112745738A CN 112745738 A CN112745738 A CN 112745738A CN 202011577851 A CN202011577851 A CN 202011577851A CN 112745738 A CN112745738 A CN 112745738A
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Abstract
本发明公开了用于水利工程的劣化免疫仿生防护涂层及制备方法。所述劣化免疫仿生防护涂层为混凝土基体上的防护涂层，所述劣化免疫仿生防护涂层由底漆和面漆两层组成；且两层间互相扩散并发生化学交联，形成分子交联互穿网络。所述的底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧粉末或者自修复环氧溶液，所述底漆成膜的厚度为250‑1000μm；所述的面漆为二维材料复合聚氨酯/聚脲溶液，所述面漆成膜的厚度为100‑2000μm。所述用于水利工程的劣化免疫仿生防护涂层，从物理裂纹修复和耐化学侵蚀两方面对混凝土进行防护，实现了对混凝土结构劣化的免疫，克服了现有技术中防护涂层容易破损、不能修复的缺陷，具有重要的经济价值和社会效益。
Description
技术领域
本发明属于材料领域，涉及一种防护涂层及其制备方法，具体地说，涉及一种水利工程结构劣化免疫仿生防护涂层及其制备方法。
背景技术
随着城市规模的扩大和工业的发展，生活污水和工业废水的排放量显著增加，使地表水受到了不同程度的污染，污水中的酸、碱、盐及有机物等强腐蚀性物质的含量明显升高。由于水利工程结构构件长期浸水，尤其经常处于阴暗潮湿、干湿交替、水流冲刷等恶劣的服役条件，水工钢筋混凝土构件普遍会发生不同程度的破坏，污水中的硫酸盐、碳酸盐、镁盐和氯化物等腐蚀介质不仅会影响混凝土本身的耐久性，还会破坏钢筋表面钝化膜，导致的钢筋腐蚀破坏。据美国(FHWA)的统计结果，美国近60万座桥梁中50％以上出现钢筋腐蚀病害，每年需750亿美元的维修费。日本目前用于钢筋混凝土设施的修复费用，也远远超过了其建造费用。因此，污水环境下的钢筋混凝土的多重防腐技术，对增强建筑物的耐久性、维护工程安全运行具有重要意义。
为提高水工结构钢筋混凝土材料的服役寿命，对混凝土和钢筋的协同防护是实现水工混凝土结构全寿命防护的关键。随着钢筋混凝土腐蚀机理与防护技术的快速发展，钢筋混凝土的防护技术已经形成了混凝土外防护涂层、添加钢筋阻锈/缓蚀剂、阴极保护和钢筋涂层防护等多种防护技术。与其他防护技术相比，混凝土表面涂层防护技术可以很好的阻挡外界环境中的侵蚀性离子的渗透，通过完全隔离外界环境与钢筋混凝土基体而提供优异的防腐蚀保护。只要涂层粘附在混凝土基体上，没有失效破坏，就能一直对混凝土和钢筋提供良好的保护。然而在实际应用中，混凝土表面涂层防护技术却难以实现全寿命周期防护。这是因为：(1)涂层与混凝土界面粘结力较弱，在外部荷载作用下易发生脱粘；(2)现有钢筋混凝土涂层防护多为环氧涂层，其硬度高、脆性大；在施工现场加工时，涂层容易发生破坏；换言之，现有涂层防护技术无法兼顾力学性能与可加工性。对涂层防护技术来说，涂层一旦发生局部破坏，就会腐蚀介质发生从破坏处入侵，从而导致整套涂层防护系统就会失效；(3)现有涂层防护技术仅能通过隔离钢筋混凝土基体而提供防腐蚀保护，但无法兼顾对裂纹和侵蚀因子的修复和免疫。
发明内容
针对现有混凝土涂层防护技术所存在的问题，本发明公开了用于水利工程的劣化免疫仿生防护涂层。所述劣化免疫仿生防护涂层模拟人体免疫系统，通过混凝土涂层结构的的优化设计，实现了对混凝土的仿生化免疫防腐处理。
本发明的技术方案：用于水利工程的劣化免疫仿生防护涂层的制备方法，包括以下步骤：
(1)混凝土表面预处理：
(1a)对混凝土表面进行处理，使混凝土表面干净、平整，并达到一定的表面粗糙度。具体方法为：除去表面浮尘、碎屑和表面污渍；除去损坏及薄弱的混凝土表层，对混凝土表面的不平整处采用修复剂或砂浆进行修复；对混凝土表面进行处理以提高混凝土表面粗糙度，从而确保涂层与混凝土之间的附着力。
(1b)采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为5-40℃，混凝土浸渍的深度为1-4mm。所述的硅烷乳液通过硅烷单体水解得到；所述硅烷单体为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、甲基三乙氧基硅烷、辛基三乙氧基硅烷、异丁基三乙氧基硅烷中的一种或几种。通过对混凝土的表面进行硅烷浸渍处理，使得硅烷偶联剂一端中的氨基、环氧基或不饱和双键可参与底漆的固化反应；同时偶联剂另一端的水解产物硅醇基与混凝土表面发生脱水反应，形成化学键，使混凝土与底漆间通过偶联剂化学相连，进一步提高界面的粘聚力。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至25-60℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆成膜的厚度为250-1000μm。所述底漆为环氧树脂，制备方法如下：
(2a)制备GO改性的聚脲基双壁微胶囊；采用GO-modified double-walledpolyurea microcapsules/epoxy composites for marine anticorrosive self-healingcoating.(Materials&Design,Ma Y,Zhang Y,Liu J,et al.2020,189:108547)公开的制备方法制备氧化石墨烯改性聚脲基双壁微胶囊。
(2b)制备聚多巴胺微球；采用水相氧化法制备聚多巴胺，将一定浓度的乙醇溶液和氨水在40-50℃下搅拌，加入一定量的多巴胺盐酸盐溶液，搅拌反应8～10h；反应完成后离心、洗涤，得到聚多巴胺微球。
(2c)制备自修复环氧粉末或者环氧溶液：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球和环氧树脂固化剂I加入粉末状的环氧树脂中并分散均匀，得到自修复环氧粉末；或者将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球加入到环氧树脂溶液中，高速分散使体系混合均匀；分散完成后加入环氧树脂固化剂II，搅拌均匀，得到自修复环氧溶液。制备自修复环氧粉末或者自修复环氧溶液中，所述聚多巴胺微球、GO改性的聚脲基双壁微胶囊的添加量均为环氧树脂的0.5-10wt％。所述自修复环氧粉末或者环氧溶液将外援型的自修复双壁微胶囊与本征型的自修复手段相结合，不但损伤处的微胶囊能够释放修复剂修复损伤，而且聚多巴胺分子间形成氢键能够对微胶囊释放后留下的空洞和未触发微胶囊的损伤部位进行修复，进一步提高了底漆的自修复效率。
其中，所述环氧树脂的型号为E-44、E51或E-54。所述环氧树脂固化剂I为双氰胺、双氰胺衍生物、酸酐、咪唑、环醚和酚醛树脂中的一种或几种。所述环氧树脂固化剂II为聚酰胺树脂、乙二胺、二乙烯三胺、四乙烯五胺、顺丁烯二酸酐和邻苯二甲酸酐中的一种或几种。
所述喷涂底漆的具体方法为：(1)采用热熔喷涂方式：将自修复环氧粉末加入热熔喷涂机中，加热到140-200℃，用喷枪均匀喷涂于混凝土的表面；或者(2)采用溶液喷涂或涂刷方式：向自修复环氧溶液中加入一定量的溶剂，使底漆达到喷涂标准；然后将其均匀喷涂或涂刷于混凝土表面上；所述溶剂为二甲苯、正丁醇或两者的混合溶液。
(3)制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备。所述面漆成膜的厚度为100-2000μm；所述面漆为二维材料复合聚氨酯/聚脲溶液，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在100-120℃下真空脱水1-3h，然后冷却至20-65℃，缓慢加入异氰酸酯单体，预聚5-60min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应0.5-3h，得到二维材料复合聚氨酯/聚脲溶液。所述面漆的涂层基体是纯聚氨酯、半聚氨酯半聚脲或纯聚脲。当所述涂层基体以聚氨酯为主体时，所用的聚醚为聚醚多元醇；以聚脲为主体时，所用的聚醚为聚醚胺。面漆中的二维材料层状分布，能够阻断或延长腐蚀介质的入侵路径，提高被保护混凝土材料的耐久性；面漆中的光稳定剂和热稳定剂则能够提高涂层的耐老化性能。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为(0-0.37):1和(0.48-1):1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为(1.05-1.2):1，所述二维材料的用量为异氰酸酯单体的0.5～15wt％，所述紫外光稳定剂的用量为异氰酸酯单体的0.01-1wt％，所述热稳定剂的用量为异氰酸酯单体的0.05-5wt％。
其中，所述的聚醚多元醇是聚氧化丙烯二醇、三羟甲基丙烷聚醚、聚四氢呋喃二醇、四氢呋喃-氧化丙烯共聚二醇和聚氧化乙烯二醇中的一种或几种；所述的聚醚胺是D230、D400、D2000、T403、T5000中的一种或几种；所述二维材料为石墨烯、云母、蒙脱石、石墨和氮化硼中的一种或几种；所述的异氰酸酯单体是六亚甲基二异氰酸酯(HDI)、二环己基甲烷二异氰酸酯(HMDI)、二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)和异佛尔酮二异氰酸酯(IPDI)中的一种或几种；所述聚酯多元醇是乙二醇、一缩二乙二醇、1,2-丙二醇、一缩二丙二醇、1,4-丁二醇、新戊二醇、1,6-己二醇、己二酸、三羟甲基丙烷和间苯二甲酸中的一种或几种；所述的胺基扩链剂为二乙基甲苯二胺、二甲硫基甲苯二胺、N,N'-二烷基甲基二苯胺、环己烷二胺、氯化MDH、乙二胺、1,3-二氨基丙烷、1,4-二氨基丁烷、二亚乙基三胺、五亚乙基六胺、六亚乙基二胺、四亚乙基五胺、1,6-己二胺和3,3'-4,4'-二氨基-二苯甲烷中的一种或几种；所述的紫外光稳定剂为水杨酸苯酯、水杨酸-4-辛基苯酯、单苯甲酸间苯二酚酯、2-羟基-4-甲氧基二苯酮、2，4-二羟基二苯酮和2-羟基-4-正辛氧基二苯酮中的一种或几种；所述热稳定剂为三盐基硫酸铅、二盐基亚磷酸铅、二盐基硬脂酸铅、硬脂酸镉、硬脂酸钡、硬脂酸钙、硬脂酸铅、硬脂酸锌、脂肪酸盐和马来酸盐中的一种或几种。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯/聚脲溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
采用前述方法制备得到的用于水利工程的劣化免疫仿生防护涂层，所述劣化免疫仿生防护涂层为混凝土基体上的防护涂层，所述劣化免疫仿生防护涂层由底漆和面漆两层组成；且两层间互相扩散并发生化学交联，形成分子交联互穿网络；所述的底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧粉末或者自修复环氧溶液，所述底漆成膜的厚度为250-1000μm；所述的面漆为二维材料复合聚氨酯/聚脲溶液，所述面漆成膜的厚度为100-2000μm。
制备原理：底漆和面漆在未完全固化时顺序涂装，使得界面处两层漆随溶剂相互扩散，聚合物分子的长链短相互渗透、扩散并缠绕形成互穿网络。其中，底漆互相扩散的链段中未反应完全的环氧基和固化剂会继续与对方扩链剂中的氨基和—NCO继续反应，从而使两层漆面发生化学交联，最终固化得到分子交联互穿网络。因此，从本质上说，劣化免疫仿生防护涂层的两层结构实质上已经密不可分，形成了一层。此外，混凝土表面采用硅烷浸渍处理，偶联剂一端的水解产物硅醇基与混凝土表面发生脱水反应，形成化学键；同时偶联剂另一端中的氨基、环氧基或不饱和双键可参与底漆的固化反应，使混凝土与底漆间通过偶联剂化学相连，进一步提高界面的粘聚力。
本发明的有益效果：
(1)本发明所述的用于水利工程的劣化免疫仿生防护涂层，从物理裂纹修复和耐化学侵蚀两方面对混凝土进行防护，实现了对混凝土结构劣化的免疫，克服了现有技术中防护涂层容易破损、不能修复的缺陷，具有重要的经济价值和社会效益。
(2)本发明所述的用于水利工程的劣化免疫仿生防护涂层，由底漆和面漆两层组成，两层在界面处相互渗透，形成分子交联互穿网络界面，融为一体，消除了界面薄弱的技术问题。
(3)本发明所述的用于水利工程的劣化免疫仿生防护涂层，混凝土表面采用硅烷浸渍处理使混凝土与底漆间通过偶联剂化学相连，进一步提高界面的粘聚力。
附图说明
附图1为本发明所述的劣化免疫仿生防护涂层的结构示意图之一。
附图2为本发明所述劣化免疫仿生防护涂层中的底漆的结构示意图。
附图3为本发明所述劣化免疫仿生防护涂层中的面漆的结构示意图。
其中：1：混凝土；2：底漆；3：面漆；4：外界水环境；5：自修复微胶囊；6：涂层基体；7：自修复聚合物；8：腐蚀介质；9：二维材料；10：涂层基体。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1:
用于水利工程的劣化免疫仿生防护涂层，所述劣化免疫仿生防护涂层为混凝土基体上的防护涂层。所述劣化免疫仿生防护涂层由底漆和面漆两层组成；且两层间互相扩散并发生化学交联，形成分子交联互穿网络。所述的底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧粉末，所述底漆成膜的厚度为500μm；所述的面漆为二维材料复合聚氨酯/聚脲溶液，所述面漆成膜的厚度为1000μm。制备方法如下：
(1)混凝土表面预处理：
(1a)对混凝土表面进行处理，使混凝土表面干净、平整，并达到一定的表面粗糙度。具体方法为：除去表面浮尘、碎屑和表面污渍；除去损坏及薄弱的混凝土表层，对混凝土表面的不平整处采用修复剂或砂浆进行修复；对混凝土表面进行处理以提高混凝土表面粗糙度，从而确保涂层与混凝土之间的附着力。
(1b)采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为25℃，混凝土浸渍的深度为2mm。所述的硅烷乳液通过硅烷单体水解得到；所述硅烷单体为异丁基三乙氧基硅烷。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至55℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆为环氧树脂，制备方法如下：
(2a)制备GO改性的聚脲基双壁微胶囊；采用GO-modified double-walledpolyurea microcapsules/epoxy composites for marine anticorrosive self-healingcoating.(Materials&Design,Ma Y,Zhang Y,Liu J,et al.2020,189:108547)公开的制备方法制备氧化石墨烯改性聚脲基双壁微胶囊。
(2b)制备聚多巴胺微球：采用水相氧化法制备聚多巴胺，将一定浓度的乙醇溶液和氨水在45℃下搅拌，加入一定量的多巴胺盐酸盐溶液，搅拌反应10h；反应完成后离心、洗涤，得到聚多巴胺微球。
(2c)制备自修复环氧粉末：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球和环氧树脂固化剂I加入粉末状的环氧树脂中并分散均匀，得到自修复环氧粉末；所述聚多巴胺微球的添加量为环氧树脂的2wt％，所述GO改性的聚脲基双壁微胶囊的添加量均为环氧树脂的3wt％。其中，所述环氧树脂的型号为E-44。所述环氧树脂固化剂I为双氰胺。
所述喷涂底漆的具体方法为热熔喷涂方式：将自修复环氧粉末加入热熔喷涂机中，加热到140℃，用喷枪均匀喷涂于混凝土的表面。
(3)制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备。所述面漆为二维材料复合聚氨酯，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在105℃下真空脱水2h，然后冷却至55℃，缓慢加入异氰酸酯单体，预聚5min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应2h，得到二维材料复合聚氨酯/聚脲溶液。所述面漆的涂层基体是纯聚氨酯。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为1:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为1.05:1，所述二维材料的用量为异氰酸酯单体的1wt％，所述紫外光稳定剂的用量为异氰酸酯单体的0.1wt％，所述热稳定剂的用量为异氰酸酯单体的0.5wt％。
其中，所述的聚醚多元醇是聚氧化丙烯二醇；所述二维材料为石墨烯；所述的异氰酸酯单体是六亚甲基二异氰酸酯(HDI)；所述聚酯多元醇是乙二醇；所述的紫外光稳定剂为水杨酸苯酯；所述的胺基扩链剂为1,6-己二胺；所述热稳定剂为三盐基硫酸铅。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
实施例2：与实施例1不同的是，
所述劣化免疫仿生防护涂层中，所述底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧溶液，所述底漆成膜的厚度为250μm；所述面漆成膜的厚度为1200μm。制备方法如下：
(1)混凝土表面预处理：
(1a)同实施例1。
(1b)采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为40℃，混凝土浸渍的深度为1mm。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至60℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆为环氧树脂，制备方法如下：
(2a)同实施例1。
(2b)同实施例1。
(2c)制备自修复环氧溶液：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球加入到环氧树脂溶液中，高速分散使体系混合均匀；分散完成后加入环氧树脂固化剂II，搅拌均匀，得到自修复环氧溶液。所述聚多巴胺微球的添加量为环氧树脂的10wt％，所述GO改性的聚脲基双壁微胶囊的添加量为环氧树脂的6％。其中，所述环氧树脂的型号为E-44。所述环氧树脂固化剂II为聚酰胺树脂。
所述喷涂底漆的具体方法为溶液喷涂方式：向自修复环氧溶液中加入一定量的溶剂，使底漆达到喷涂标准；然后将其均匀喷涂于混凝土表面上；所述溶剂为二甲苯。
(3)制备非特异性损伤自分化免疫层：所述面漆为二维材料复合聚氨酯/聚脲，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在120℃下真空脱水1h，然后冷却至65℃，缓慢加入异氰酸酯单体，预聚30min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应0.5h，得到二维材料复合聚氨酯/聚脲溶液。所述面漆的涂层基体是半聚氨酯半聚脲。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为0.48:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为1.1:1，所述二维材料的用量为异氰酸酯单体的10wt％，所述紫外光稳定剂的用量为异氰酸酯单体的1wt％，所述热稳定剂的用量为异氰酸酯单体的5wt％。
其中，所述的聚醚是聚氧化丙烯二醇；所述二维材料为石墨烯；所述的异氰酸酯单体是六亚甲基二异氰酸酯(HDI)；所述聚酯多元醇是乙二醇；所述的紫外光稳定剂为水杨酸苯酯；所述的胺基扩链剂为五亚乙基六胺，所述热稳定剂为三盐基硫酸铅。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
实施例3：与实施例1不同的是，
所述劣化免疫仿生防护涂层中，所述底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧溶液，所述底漆成膜的厚度为1000μm；所述面漆成膜的厚度为2000μm。制备方法如下：
(1)混凝土表面预处理：
(1a)同实施例1。
(1b)采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为5℃，混凝土浸渍的深度为4mm。所述的硅烷乳液通过硅烷单体水解得到；所述硅烷单体为乙烯基三甲氧基硅烷。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至35℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆为环氧树脂，制备方法如下：
(2a)同实施例1。
(2b)制备聚多巴胺微球；采用水相氧化法制备聚多巴胺，将一定浓度的乙醇溶液和氨水在50℃下搅拌，加入一定量的多巴胺盐酸盐溶液，搅拌反应9h；反应完成后离心、洗涤，得到聚多巴胺微球。
(2c)制备自修复环氧溶液：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球加入到环氧树脂溶液中，高速分散使体系混合均匀；分散完成后加入环氧树脂固化剂II，搅拌均匀，得到自修复环氧溶液。所述聚多巴胺微球的添加量为环氧树脂的5％，所述GO改性的聚脲基双壁微胶囊的添加量为环氧树脂的10wt％。其中，所述环氧树脂的型号为E51。所述环氧树脂固化剂II为四乙烯五胺。
所述喷涂底漆的具体方法为溶液涂刷方式：向自修复环氧溶液中加入一定量的溶剂，使底漆达到喷涂标准；然后将其均匀涂刷于混凝土表面上；所述溶剂正丁醇。
(3)制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备。所述面漆为二维材料复合聚氨酯/聚脲溶液，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在110℃下真空脱水1h，然后冷却至20℃，缓慢加入异氰酸酯单体，预聚60min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应3h，得到二维材料复合聚氨酯/聚脲溶液。所述面漆的涂层基体是半聚氨酯半聚脲。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为0.37:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为1.2:1，所述二维材料的用量为异氰酸酯单体的5wt％，所述紫外光稳定剂的用量为异氰酸酯单体的0.01wt％，所述热稳定剂的用量为异氰酸酯单体的1wt％。
其中，所述的聚醚是D2000；所述二维材料为云母；所述的异氰酸酯单体是甲苯二异氰酸酯(TDI)；所述聚酯多元醇是1,2-丙二醇；所述的胺基扩链剂为乙二胺；所述的紫外光稳定剂为单苯甲酸间苯二酚酯；所述热稳定剂为二盐基亚磷酸铅。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯/聚脲溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
实施例4：与实施例1不同的是，
所述劣化免疫仿生防护涂层中，所述底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧粉末，所述底漆成膜的厚度为800μm；所述面漆成膜的厚度为300μm。制备方法如下：
(1)混凝土表面预处理：
(1a)同实施例1。
(1b)同实施例1。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至60℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆为环氧树脂，制备方法如下：
(2a)同实施例1。
(2b)同实施例1。
(2c)制备自修复环氧粉末：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球和环氧树脂固化剂I加入粉末状的环氧树脂中并分散均匀，得到自修复环氧粉末。所述聚多巴胺微球的添加量为环氧树脂的0.5wt％，所述GO改性的聚脲基双壁微胶囊的添加量均为环氧树脂的6wt％。其中，所述环氧树脂的型号为E51。所述环氧树脂固化剂I为双氰胺。
所述喷涂底漆的具体方法为热熔喷涂方式：将自修复环氧粉末加入热熔喷涂机中，加热到200℃，用喷枪均匀喷涂于混凝土的表面。
(3)制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备。所述面漆为二维材料复合聚氨酯/聚脲溶液，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在100℃下真空脱水3h，然后冷却至35℃，缓慢加入异氰酸酯单体，预聚15min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应1h，得到二维材料复合聚氨酯/聚脲溶液。所述面漆的涂层基体是半聚氨酯半聚脲。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为0.75:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为1.1:1，所述二维材料的用量为异氰酸酯单体的0.5wt％，所述紫外光稳定剂的用量为异氰酸酯单体的0.05wt％，所述热稳定剂的用量为异氰酸酯单体的2wt％。
其中，所述的聚醚是聚氧化丙烯二醇；所述二维材料为蒙脱石；所述的异氰酸酯单体是异佛尔酮二异氰酸酯(IPDI)；所述聚酯多元醇是1,6-己二醇；所述的胺基扩链剂为1,6-己二胺；所述的紫外光稳定剂为2，4-二羟基二苯酮；所述热稳定剂为硬脂酸钙。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯/聚脲溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
实施例5：与实施例1不同的是，
所述劣化免疫仿生防护涂层中，所述底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧溶液，所述底漆成膜的厚度为250μm；所述面漆成膜的厚度为100μm。制备方法如下：
(1)混凝土表面预处理：
(1a)同实施例1。
(1b)采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为35℃，混凝土浸渍的深度为3mm。所述的硅烷乳液通过硅烷单体水解得到；所述硅烷单体为乙烯基三甲氧基硅烷。
(2)制备非特异性自修复应力免疫层：步骤(1)的混凝土预处理完成后，加热至35℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆为环氧树脂，制备方法如下：
(2a)同实施例1。
(2b)制备聚多巴胺微球；采用水相氧化法制备聚多巴胺，将一定浓度的乙醇溶液和氨水在40℃下搅拌，加入一定量的多巴胺盐酸盐溶液，搅拌反应10h；反应完成后离心、洗涤，得到聚多巴胺微球。
(2c)制备自修复环氧溶液：将步骤(2a)得到的GO改性的聚脲基双壁微胶囊、步骤(2b)得到的聚多巴胺微球加入到环氧树脂溶液中，高速分散使体系混合均匀；分散完成后加入环氧树脂固化剂II，搅拌均匀，得到自修复环氧溶液。所述聚多巴胺微球的添加量为环氧树脂的6wt％，所述GO改性的聚脲基双壁微胶囊的添加量为环氧树脂的0.5wt％。其中，所述环氧树脂的型号为E44。所述环氧树脂固化剂II为聚酰胺树脂。
所述喷涂底漆的具体方法为溶液喷涂方式：向自修复环氧溶液中加入一定量的溶剂，使底漆达到喷涂标准；然后将其均匀喷涂于混凝土表面上；所述溶剂为二甲苯、正丁醇的混合溶液。
(3)制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备。所述面漆为二维材料复合聚脲溶液，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在110℃下真空脱水1h，然后冷却至45℃，缓慢加入异氰酸酯单体，预聚5min得到预聚物。将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应3h，得到二维材料复合聚脲溶液。所述面漆的涂层基体是纯聚脲。
其中，所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为0:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为1.2:1，所述二维材料的用量为异氰酸酯单体的15wt％，所述紫外光稳定剂的用量为异氰酸酯单体的0.5wt％，所述热稳定剂的用量为异氰酸酯单体的0.05wt％。
所述的聚醚是D230；所述二维材料为氮化硼；所述的异氰酸酯单体是甲苯二异氰酸酯(TDI)；所述的胺基扩链剂为乙二胺；所述的紫外光稳定剂为单苯甲酸间苯二酚酯；所述热稳定剂为二盐基亚磷酸铅。所述的溶剂I为N，N—二甲基乙酰胺，所述的溶剂II为N，N—二甲基乙酰胺。
所述面漆喷涂的具体方法为：向二维材料复合聚氨酯/聚脲溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
实施例6：附着力试验和电化学试验检测实施例1-5制备的劣化免疫仿生防护涂层
电化学试验：分别以无涂层钢筋混凝土、涂装普通聚脲涂层的混凝土和实施例1-5所述的劣化免疫仿生防护涂层钢筋混凝土，制备电化学试验所需试件。钢筋混凝土试块尺寸为150×150×150mm，混凝土等级为C30，混凝土保护层厚度为68mm，钢筋锚固长度为70mm，试件养护28d后，涂装普通聚脲涂层和实施例1-5所述涂层，同时制备无涂层的空白组进行对照。将试件放置于3.5％NaCl溶液中浸泡3个月，以钢筋为工作电极，饱和甘汞电极为参比电极，钛网为辅助电极的三电极系统，进行动电位极化测量，扫描范围为开路电位附近±250mV，扫描速度为0.5mV/s。所得数据采用塔菲尔外推法处理，得到自腐蚀电位和腐蚀电流密度。
附着力试验：参照《色漆和清漆拉开法附着力试验》(GB/T5210-2006)和《附着力测定法》(ASTM-D-4541)中的规定，进行涂层的附着力测试。将养护完成的混凝土表面分别涂装普通聚脲涂层(对照)和实施例1-5所述涂层。试验前，选取光滑、无缺陷的表面为实验面，将实验面和试柱用无水乙醇擦拭干净，选用丙烯酸胶黏剂将试柱粘接在实验面，静置24h后进行测试。
上述试验结果如表1所示。
表1电化学试验和附着力试验的测试结果
根据表1中电化学试验的测试结果可知，无涂层钢筋混凝土在浸泡3个月后腐蚀电位为-0.579V，腐蚀电流密度最大，为2.8×10-6A·cm2；说明钢筋处于活性腐蚀状态，腐蚀速率最高。涂装普通聚脲涂层的钢筋混凝土的腐蚀电位正移-0.310V，腐蚀电流密度降低至3.3×10-9A·cm2。而本申请实施例1-5制备样品钢筋混凝土的腐蚀电位为-0.289～-0.187V，腐蚀电流密度为2.8×10-10～9.4×10-13A·cm2。由此可知，与无涂层钢筋相比，本申请实施例1-5制备样品钢筋混凝土的腐蚀电位正移0.3-0.4V，腐蚀电流密度则降低了4-7个数量级；这说明，普通聚脲涂层一定程度上免疫钢筋的腐蚀，但本申请所述的劣化免疫仿生防护涂层与之相比，能够在更大程度上阻隔海水，从而有效免疫钢筋的腐蚀，使其具有更小的腐蚀电流密度，延缓了腐蚀的发生，更好的实现了对钢筋混凝土的防护。
根据表1中附着力试验的测试结果可知，实施例1-5制备的混凝土涂层的粘结强度与普通聚脲涂层相比，均有所提高。其中，实施例2和实施例4中硅烷浸渍深度小，因此底漆与混凝土表面粘结强度较低，因此破坏发生在底漆与混凝土界面处，但其粘结强度仍高于普通聚脲涂层。而实施例5的成膜厚度最小，且面漆厚度最小，因此粘结强度最低，破坏发生在成膜厚度最小的面漆处。实施例3所采用的硅烷浸渍深度最大，且溶液型底漆能够向混凝土中进行渗透，因此底漆与混凝土界面粘结能力最强；并且实施例3采用了成膜厚度最大的面漆，抗拉能力强，因此在试验过程中底漆到达了强度极限而发生了破坏，说明混凝土与底 漆界面粘结强度、底漆与面漆粘结强度均高于了材料本身的强度，具有优秀的附着力。此外，实施例1-5均未发生底漆与面漆界面的破坏，说明采用了界面互穿网络的底漆与面漆的界面间的强度已经不低于整体材料的强度，也证实了两层结构已经形成为整体界面体系。
综上可知，本申请所述的用于水利工程的劣化免疫仿生防护涂层，虽然由底漆和面漆两层组成，但在界面处相互渗透，形成分子交联互穿网络界面，使二者融为一体，消除了界面薄弱的关键问题。而且，所述免疫界面的底漆与混凝土表面通过化学键相连，提高了界面系统与混凝土的界面粘结力。因此，本申请所述的劣化免疫仿生防护涂层，克服了现有技术中防护涂层容易破损的问题，从物理裂纹修复和耐化学侵蚀两方面实现了对混凝土的防护，具有重要的经济价值和社会效益。
Claims (10)
1.用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：包括以下步骤：
（1）混凝土表面预处理：（1a）对混凝土表面进行处理，使混凝土表面干净、平整，并达到一定的表面粗糙度；（1b）采用硅烷乳液对混凝土表面进行浸渍，浸渍期间混凝土表面的温度为5-40℃，混凝土浸渍的深度为1-4mm；
（2）制备非特异性自修复应力免疫层：步骤（1）的混凝土预处理完成后，加热至25-60℃后喷涂底漆，得到非特异性自修复应力免疫层；所述底漆成膜的厚度为250-1000μm；所述底漆为环氧树脂，制备方法如下：（2a）制备GO改性的聚脲基双壁微胶囊；（2b）制备聚多巴胺微球；（2c）制备自修复环氧粉末或者环氧溶液：将步骤（2a）得到的GO改性的聚脲基双壁微胶囊、步骤（2b）得到的聚多巴胺微球和环氧树脂固化剂I加入粉末状的环氧树脂中并分散均匀，得到自修复环氧粉末；或者将步骤（2a）得到的GO改性的聚脲基双壁微胶囊、步骤（2b）得到的聚多巴胺微球加入到环氧树脂溶液中，高速分散使体系混合均匀；分散完成后加入环氧树脂固化剂II，搅拌均匀，得到自修复环氧溶液；制备自修复环氧粉末或者自修复环氧溶液中，所述聚多巴胺微球、GO改性的聚脲基双壁微胶囊的添加量均为环氧树脂的0.5-10wt%；
（3）制备非特异性损伤自分化免疫层：底漆喷涂完成后，保持表面温度不低于30℃，立刻进行面漆的喷涂，得到非特异性损伤自分化免疫层，从而完成劣化免疫仿生防护涂层的制备；所述面漆成膜的厚度为100-2000μm；所述面漆为二维材料复合聚氨酯/聚脲溶液，制备方法如下：将聚醚、溶剂I和乳化剂混合均匀，在100-120℃下真空脱水1-3h，然后冷却至20-65℃，缓慢加入异氰酸酯单体，预聚5-60min得到预聚物；将二维材料、紫外光稳定剂、热稳定剂、聚酯多元醇和氨基扩链剂加入到溶剂II中混合均匀，再加入到前述预聚物中，保温反应0.5-3h，得到二维材料复合聚氨酯/聚脲溶液；所述面漆的涂层基体是纯聚氨酯、半聚氨酯半聚脲或纯聚脲。
2.根据权利要求1所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（3）中所述的聚酯多元醇-氨基扩链剂的羟基与“羟基+氨基”的官能团当量比为（0-0.37）:1和（0.48-1）:1，所述反应体系中—NCO与“羟基+氨基”的官能团当量比为（1.05-1.2）:1，所述二维材料的用量为异氰酸酯单体的0.5~15wt%，所述紫外光稳定剂的用量为异氰酸酯单体的0.01-1wt%，所述热稳定剂的用量为异氰酸酯单体的0.05-5wt%。
3.根据权利要求2所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（3）所述面漆的涂层基体中，以聚氨酯为主体时，所用的聚醚为聚醚多元醇；以聚脲为主体时，所用的聚醚为聚醚胺。
4.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（1b）所述的硅烷乳液通过硅烷单体水解得到；所述硅烷单体为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、甲基三乙氧基硅烷、辛基三乙氧基硅烷、异丁基三乙氧基硅烷中的一种或几种。
5.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（2b）所述聚多巴胺微球的制备方法具体为：采用水相氧化法制备聚多巴胺，将一定浓度的乙醇溶液和氨水在40-50℃下搅拌，加入一定量的多巴胺盐酸盐溶液，搅拌反应8~10h；反应完成后离心、洗涤，得到聚多巴胺微球。
6.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（2c）所述环氧树脂的型号为E-44、E51或E-54；所述环氧树脂固化剂I为双氰胺、双氰胺衍生物、酸酐、咪唑、环醚和酚醛树脂中的一种或几种；所述环氧树脂固化剂II为聚酰胺树脂、乙二胺、二乙烯三胺、四乙烯五胺、顺丁烯二酸酐和邻苯二甲酸酐中的一种或几种。
7.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（2）中所述喷涂底漆的具体方法为：（1）采用热熔喷涂方式：将自修复环氧粉末加入热熔喷涂机中，加热到140-200℃，用喷枪均匀喷涂于混凝土的表面；或者（2）采用溶液喷涂或涂刷方式：向自修复环氧溶液中加入一定量的溶剂，使底漆达到喷涂标准；然后将其均匀喷涂或涂刷于混凝土表面上；所述溶剂为二甲苯、正丁醇或两者的混合溶液。
8.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：步骤（3）所述的聚醚多元醇是聚氧化丙烯二醇、三羟甲基丙烷聚醚、聚四氢呋喃二醇、四氢呋喃-氧化丙烯共聚二醇和聚氧化乙烯二醇中的一种或几种；
所述的聚醚胺是D230、D400、D2000、T403、T5000中的一种或几种；
所述二维材料为石墨烯、云母、蒙脱石、石墨和氮化硼中的一种或几种；
所述的异氰酸酯单体是六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和异佛尔酮二异氰酸酯中的一种或几种；
所述聚酯多元醇是乙二醇、一缩二乙二醇、1,2-丙二醇、一缩二丙二醇、1,4-丁二醇、新戊二醇、1,6-己二醇、己二酸、三羟甲基丙烷和间苯二甲酸中的一种或几种；
所述的胺基扩链剂为二乙基甲苯二胺、二甲硫基甲苯二胺、N,N'-二烷基甲基二苯胺、环己烷二胺、氯化MDH、乙二胺、1,3-二氨基丙烷、1,4-二氨基丁烷、二亚乙基三胺、五亚乙基六胺、六亚乙基二胺、四亚乙基五胺、1,6-己二胺和3,3'-4,4'-二氨基-二苯甲烷中的一种或几种；
所述的紫外光稳定剂为水杨酸苯酯、水杨酸-4-辛基苯酯、单苯甲酸间苯二酚酯、2-羟基-4-甲氧基二苯酮、2，4-二羟基二苯酮和2-羟基-4-正辛氧基二苯酮中的一种或几种；
所述热稳定剂为三盐基硫酸铅、二盐基亚磷酸铅、二盐基硬脂酸铅、硬脂酸镉、硬脂酸钡、硬脂酸钙、硬脂酸铅、硬脂酸锌、脂肪酸盐和马来酸盐中的一种或几种。
9.根据权利要求3所述的用于水利工程的劣化免疫仿生防护涂层的制备方法，其特征在于：所述面漆喷涂的具体方法为：向步骤（3）得到的二维材料复合聚氨酯/聚脲溶液中加入一定量的溶剂N,N-二甲基乙酰胺，使底漆达到喷涂标准；然后采用喷枪将其均匀喷涂于底漆上。
10.采用如权利要求1-9所述的方法制备得到的用于水利工程的劣化免疫仿生防护涂层，所述劣化免疫仿生防护涂层为混凝土基体上的防护涂层，其特征在于：所述劣化免疫仿生防护涂层由底漆和面漆两层组成；且两层间互相扩散并发生化学交联，形成分子交联互穿网络；所述的底漆为GO改性的聚脲基双壁微胶囊和聚多巴胺在环氧树脂中分散均匀，得到的自修复环氧粉末或者自修复环氧溶液，所述底漆成膜的厚度为250-1000μm；所述的面漆为二维材料复合聚氨酯/聚脲溶液，所述面漆成膜的厚度为100-2000μm。
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| CN113698736B (zh) * | 2021-10-09 | 2023-09-12 | 深圳市永杰诚电子有限公司 | 一种无卤阻燃导热电线绝缘层及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20230019494A (ko) | 2023-02-08 |
| KR102551925B1 (ko) | 2023-07-07 |
| WO2022141949A1 (zh) | 2022-07-07 |
| CN112745738B (zh) | 2021-10-01 |
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