CN112778817A - 一种海工混凝土用钢筋耐腐蚀涂层及其制备方法 - Google Patents

一种海工混凝土用钢筋耐腐蚀涂层及其制备方法 Download PDF

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CN112778817A
CN112778817A CN202011638599.3A CN202011638599A CN112778817A CN 112778817 A CN112778817 A CN 112778817A CN 202011638599 A CN202011638599 A CN 202011638599A CN 112778817 A CN112778817 A CN 112778817A
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corrosion
steel bar
stirring
coating
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CN112778817B (zh
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陈平
明阳
李玲
胡成
李青
陈宣东
刘荣进
李顺凯
赵艳荣
韦家崭
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Guilin University of Technology
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Abstract

本发明提供一种海工混凝土用钢筋耐腐蚀涂层的制备方法，包括以下步骤：（1）对钢筋表面进行预处理；（2）制备自修复腐蚀微胶囊；（3）制备阴极电泳涂料；（4）阴极电泳；（5）固化。本发明通过在电泳涂料中添加自修复腐蚀微胶囊以及金属粉末、氧化石墨烯粉末，通过自修复微胶囊的自修复性以及阴极保护的共同作用能够显著提高涂层的耐腐蚀性能，该耐腐蚀涂层具有优异的粘结性和防腐蚀性，可以延长了钢筋的使用寿命。可以广泛应用于海工混凝土用钢筋的防护，也可以应用一般环境下的金属结构的保护。

Description

一种海工混凝土用钢筋耐腐蚀涂层及其制备方法
技术领域
本发明涉及钢筋防护领域，具体涉及一种海工混凝土用钢筋耐腐蚀涂层及其制备方法。
背景技术
混凝土结构广泛应用于建筑、基建领域，通常使用钢筋骨架来改善混凝土的强度，成为钢筋混凝土，是海工基础设施的主要材料。然而其面临着海水介质的侵蚀容易引起混凝土结构破坏，造成了巨大的经济损失，而且再进行修复就非常困难。海水中氯离子侵蚀是引起钢筋锈蚀的重要原因，通过局部酸化和阳极去极化作用不断使钢筋表面的钝化膜溶解破坏；形成腐蚀电池对钢筋表面钝化膜的破坏发生在局部，使这些部位露出了钢筋基体，与尚完好的钝化膜区域之间构成电位差，钢筋作为阳极而易于发生腐蚀。现有技术对钢筋防腐蚀做了大量的研究，且也取得了不错的效果。
中国专利CN 111378350 A公开了一种预应力防腐蚀涂层钢棒，按照质量比，所述涂层包括5％-30％填料，和70％-95％改性水性环氧树脂，其特征在于，按照质量比，所述改性水性环氧树脂由以下比例的原料制备而成：10％-50％的高弹性水溶性聚合物、10％-60％的水性环氧树脂和10％-40％的固化剂。
中国专利CN106380111A公开了一种内含阻锈剂的缓释微胶囊及其制备方法，虽然该方法利用了微胶囊能够对混凝土中的钢筋产生持久的保护。但是其毕竟是分散于整个混凝土结构中，钢筋表面仍然属于暴露于腐蚀介质中。在一定程度上还是存在氯离子以及其他腐蚀介质对钢筋表面的腐蚀。
中国专利CN 105177679 A一种成本低和操作简单的在碳钢基体上电泳沉积石墨烯涂层的方法，用该方法沉积的石墨烯涂层能提高碳钢基体的耐蚀性、表面的耐磨性和基体的导电导热性。
鉴于海工混凝土用钢筋的广泛应用，如何提高其使用寿命仍然是现有技术研究的方向和重点。
发明内容
针对现有技术的需求，本发目的在于提供一种海工混凝土用钢筋耐腐蚀涂层及其制备方法，该耐腐蚀涂层具有优异的粘结性和防腐蚀性，能够有效的对钢筋结构进行防护，大大延长了海工混凝土用钢筋的使用寿命。
为了实现上述技术目的，本发明提供了一种海工混凝土用钢筋耐腐蚀涂层的制备方法，包括以下步骤：
(1)对钢筋表面进行预处理：钢筋经除油、酸洗、水洗、喷砂后备用；
(2)制备自修复腐蚀微胶囊：
(a1)将10～12份尿素、18～20份甲醛、1～3份氯化铵倒入反应器中，加入pH调节剂调节pH至为8～10，搅拌均匀后升温至60～80℃下进行回流反应2～3h形成脲醛树脂预聚体；
(b1)将5～10份间苯二酚、3～7份聚乙烯醇、10～20份亚麻籽油、1～3份2-苯基苯并咪唑，在50～60℃下搅拌10～15min，加入1～5份去离子水和0.1～0.5份十二烷基苯磺酸钠，乳化20～30min形成油乳状液；
(c1)将步骤(a1)得到的脲醛树脂预聚体加入至步骤(b1)油乳状液中，用盐酸调节pH为3～4，在70～90℃下回流反应2～3h，将所得产物真空抽滤，用去离子水和丙酮洗涤，放至烘干箱中干燥，即得自修复腐蚀微胶囊；
(3)制备阴极电泳涂料：
(a2)在反应釜中加入5～10份2,4-甲苯二异氰酸酯和20～30份丙二醇甲醚，在保护气氛下搅拌升温至50～60℃后，在2～3h内滴加完3～5份甲基异丁基酮，完成后再次升温至110～120℃反应2～3h，测量NCO基含量，即得到半封闭异氰酸酯；
(b2)在装有温度计、搅拌器和回流冷凝管的反应瓶中，依次加入50～60份水性羟基丙烯酸树脂、10～30份半封闭异氰酸酯，搅拌并升温至40～60℃，加入2～5份乙酸、1～5份金属粉末、1～5份氧化石墨烯粉末、5～10份异丙醇和10～30份去离子水，然后继续搅拌10～20min，制得色浆；
(c2)将30～50份有机胺改性环氧树脂、2～10份二乙二醇丁醚、5～15份双酚A聚氧乙烯醚、1～5份甲基异丁基酮、10～20份半封闭异氰酸酯以及20～30份去离子搅拌混合均匀，即得乳液，固含量为30～50％；
(d2)按色浆：乳液＝(1:2)～(1:4)的比例混合，再加入1～5份去离子水搅拌均匀熟化24-48h；然后加入5～10份自修复腐蚀微胶囊并继续搅拌10～30min，即得阴极电泳涂料，然后将阴极电泳涂料放入阴极电泳槽中；
(4)阴极电泳：将钢筋置于阴极电泳槽，设置电泳工艺参数为：阴极电泳槽液固含量10％～15％、pH值5.5～6.5、电导率200～500us/cm、槽液温度30～50℃、电泳电压50～100V、电泳时间3～10min；
(5)固化：将电泳后的钢筋放入烘干箱中，设置温度为150～200℃，时间为20～40min，自然冷却即可。
进一步地，所述pH调节剂为氢氧化钠或三乙醇胺。
进一步地，所述除油步骤为将钢筋放入含碳酸钠20～30g/L、磷酸钠30～50g/L、硅酸钠10～20g/L的水的溶液中超声清洗10～20min；除油温度为30～50℃。
进一步地，所述酸洗步骤为将钢筋放入0.5～1mol/L的稀盐酸溶液中浸泡5～10min。
进一步地，所述金属粉末粒径为50～80μm；氧化石墨烯粉末粒径为10～30μm。
更进一步地，所述金属粉末为锌粉或镁粉。
本发明提还供了一种海工混凝土用钢筋耐腐蚀涂层，所述耐腐蚀涂层由上述方法制备。
半封闭型异氰酸酯固化剂提供电泳涂料良好的成膜效果，保证漆膜足够的交联密度，使电泳涂层具备良好物理及化学性能。
本发明通过制备自修复微胶囊添加至电泳涂层中，包覆在涂层里面的微胶囊在外力作用下破裂，微胶囊内的修复剂流出，修复剂在毛细管作用下充满裂纹并发生聚合反应完成自修复过程，通过抑制裂纹的产生从而确保涂层的致密性，有效的提高了涂层的耐腐蚀性能。而且自修复微胶囊中添加了具有缓蚀作用的物质2-苯基苯并咪唑，在微胶囊破裂的情况下该物质也以在钢筋表面吸附抑制腐蚀的发生。
本发明一方面通过在钢筋表面电泳制备致密的防护性涂层来提高耐腐蚀性能，另一方面则是与阴极保护原理相结合，在电泳涂层中添加锌或镁等低电位金属粉末，涂层在海洋环境中容易形成阴极保护电路，进一步提高涂层的耐腐蚀性能。
氧化石墨烯硬度高，层间具有润滑作用，可以提高电泳涂层的机械强度、耐冲击性、柔韧性等机械性能。而且氧化石墨烯本身就具有一定的耐腐蚀性，可进一步提高电泳涂层的耐腐蚀性能。
与现有技术相比，本发明具有如下有益效果：
1、虽然现有技术中也有不少利用自修复腐蚀微胶囊来提高涂层耐腐蚀性的研究，但是很少利用阴极保护和自修复腐蚀微胶囊相结合的技术方案。本发明首先将两者相结合实现了对海工混凝土用钢筋耐腐蚀涂层的制备。
2、申请人经过检索，现有技术很少对电泳涂料中添加自修复腐蚀微胶囊的研究，本申请通过在电泳涂料中添加自修复腐蚀微胶囊、并相应的制备了对应的电泳涂料与其配合，实现了电泳法在钢筋表面制备形成了结合力优异、耐腐蚀性高的防护涂层。
3、本申请耐腐蚀涂层可以广泛应用于海工混凝土用钢筋的防护，也可以应用一般环境下的金属结构的保护。
附图说明
图1为实施例1-3制备的耐腐蚀涂层的Tafel极化曲线。
具体实施方式
下面结合具体实施例，对本发明的具体实施方式作进一步详细描述。
实施例1
一种海工混凝土用钢筋耐腐蚀涂层的制备方法，包括以下步骤：
(1)对钢筋表面进行预处理：钢筋经除油、酸洗、水洗、喷砂后备用；所述除油步骤为将钢筋放入含碳酸钠20g/L、磷酸钠30g/L、硅酸钠10g/L的水的溶液中超声清洗10min；除油温度为30℃；所述酸洗步骤为将钢筋放入0.5mol/L的稀盐酸溶液中浸泡5min；
(2)制备自修复腐蚀微胶囊：
(a1)将10份尿素、18份甲醛、1份氯化铵倒入反应器中，加入氢氧化钠pH调节剂调节pH至为8，搅拌均匀后升温至60℃下进行回流反应2h形成脲醛树脂预聚体；
(b1)将5份间苯二酚、3份聚乙烯醇、10份亚麻籽油、1份2-苯基苯并咪唑，在50℃下搅拌10min，加入1份去离子水和0.1份十二烷基苯磺酸钠，乳化20min形成油乳状液；
(c1)将步骤(a1)得到的脲醛树脂预聚体加入至步骤(b1)油乳状液中，用盐酸调节pH为3，在70℃下回流反应2h，将所得产物真空抽滤，用去离子水和丙酮洗涤，放至烘干箱中干燥，即得自修复腐蚀微胶囊；
(3)制备阴极电泳涂料：
(a2)在反应釜中加入5份2,4-甲苯二异氰酸酯和20份丙二醇甲醚，在保护气氛下搅拌升温至50℃后，在3h内滴加完3份甲基异丁基酮，完成后再次升温至110℃反应2h，测量NCO基含量，即得到半封闭异氰酸酯；
(b2)在装有温度计、搅拌器和回流冷凝管的反应瓶中，依次加入50份水性羟基丙烯酸树脂、10份半封闭异氰酸酯，搅拌并升温至40℃，加入2份乙酸、1份金属粉末、1份氧化石墨烯粉末、5份异丙醇和10份去离子水，然后继续搅拌10min，制得色浆；
(c2)将30份有机胺改性环氧树脂、2份二乙二醇丁醚、5份双酚A聚氧乙烯醚、1份甲基异丁基酮、10份半封闭异氰酸酯以及20份去离子搅拌混合均匀，即得乳液，固含量为30％；所述金属粉末粒径为50μm；氧化石墨烯粉末粒径为10μm、所述金属粉末为锌粉；
(d2)按色浆：乳液＝1:2的比例混合，再加入1份去离子水搅拌均匀熟化24h；然后加入5份自修复腐蚀微胶囊并继续搅拌10min，即得阴极电泳涂料，然后将阴极电泳涂料放入阴极电泳槽中；
(4)阴极电泳：将钢筋置于阴极电泳槽，设置电泳工艺参数为：阴极电泳槽液固含量10％、pH值5.5、电导率200us/cm、槽液温度30℃、电泳电压50V、电泳时间3min；
(5)固化：将电泳后的钢筋放入烘干箱中，设置温度为150℃，时间为20min，自然冷却即可。
实施例2
一种海工混凝土用钢筋耐腐蚀涂层的制备方法，包括以下步骤：
(1)对钢筋表面进行预处理：钢筋经除油、酸洗、水洗、喷砂后备用；所述除油步骤为将钢筋放入含碳酸钠25g/L、磷酸钠40g/L、硅酸钠15g/L的水的溶液中超声清洗15min；除油温度为40℃；所述酸洗步骤为将钢筋放入0.8mol/L的稀盐酸溶液中浸泡7min；
(2)制备自修复腐蚀微胶囊：
(a1)将11份尿素、19份甲醛、2份氯化铵倒入反应器中，加入氢氧化钠pH调节剂调节pH至为9，搅拌均匀后升温至70℃下进行回流反应2.5h形成脲醛树脂预聚体；
(b1)将7份间苯二酚、5份聚乙烯醇、15份亚麻籽油、2份2-苯基苯并咪唑，在55℃下搅拌12min，加入3份去离子水和03份十二烷基苯磺酸钠，乳化25min形成油乳状液；
(c1)将步骤(a1)得到的脲醛树脂预聚体加入至步骤(b1)油乳状液中，用盐酸调节pH为3.5，在80℃下回流反应2.5h，将所得产物真空抽滤，用去离子水和丙酮洗涤，放至烘干箱中干燥，即得自修复腐蚀微胶囊；
(3)制备阴极电泳涂料：
(a2)在反应釜中加入7份2,4-甲苯二异氰酸酯和25份丙二醇甲醚，在保护气氛下搅拌升温至55℃后，在2.5h内滴加完4份甲基异丁基酮，完成后再次升温至115℃反应2.5h，测量NCO基含量，即得到半封闭异氰酸酯；
(b2)在装有温度计、搅拌器和回流冷凝管的反应瓶中，依次加入55份水性羟基丙烯酸树脂、20份半封闭异氰酸酯，搅拌并升温至50℃，加入4份乙酸、3份金属粉末、3份氧化石墨烯粉末、8份异丙醇和20份去离子水，然后继续搅拌15min，制得色浆；
(c2)将40份有机胺改性环氧树脂、5份二乙二醇丁醚、10份双酚A聚氧乙烯醚、3份甲基异丁基酮、15份半封闭异氰酸酯以及25份去离子搅拌混合均匀，即得乳液，固含量为40％；所述金属粉末粒径为60μm；氧化石墨烯粉末粒径为20μm、所述金属粉末为锌粉；
(d2)按色浆：乳液＝1:3的比例混合，再加入3份去离子水搅拌均匀熟化36h；然后加入7份自修复腐蚀微胶囊并继续搅拌20min，即得阴极电泳涂料，然后将阴极电泳涂料放入阴极电泳槽中；
(4)阴极电泳：将钢筋置于阴极电泳槽，设置电泳工艺参数为：阴极电泳槽液固含量12％、pH值6、电导率300us/cm、槽液温度40℃、电泳电压70V、电泳时间5min；
(5)固化：将电泳后的钢筋放入烘干箱中，设置温度为180℃，时间为30min，自然冷却即可。
实施例3
一种海工混凝土用钢筋耐腐蚀涂层的制备方法，包括以下步骤：
(1)对钢筋表面进行预处理：钢筋经除油、酸洗、水洗、喷砂后备用；所述除油步骤为将钢筋放入含碳酸钠30g/L、磷酸钠50g/L、硅酸钠20g/L的水的溶液中超声清洗20min；除油温度为50℃；所述酸洗步骤为将钢筋放入1mol/L的稀盐酸溶液中浸泡10min；
(2)制备自修复腐蚀微胶囊：
(a1)将12份尿素、20份甲醛、3份氯化铵倒入反应器中，加入三乙醇胺pH调节剂调节pH至为10，搅拌均匀后升温至80℃下进行回流反应3h形成脲醛树脂预聚体；
(b1)将10份间苯二酚、7份聚乙烯醇、20份亚麻籽油、3份2-苯基苯并咪唑，在60℃下搅拌15min，加入5份去离子水和0.5份十二烷基苯磺酸钠，乳化30min形成油乳状液；
(c1)将步骤(a1)得到的脲醛树脂预聚体加入至步骤(b1)油乳状液中，用盐酸调节pH为4，在90℃下回流反应3h，将所得产物真空抽滤，用去离子水和丙酮洗涤，放至烘干箱中干燥，即得自修复腐蚀微胶囊；
(3)制备阴极电泳涂料：
(a2)在反应釜中加入10份2,4-甲苯二异氰酸酯和30份丙二醇甲醚，在保护气氛下搅拌升温至60℃后，在3h内滴加完5份甲基异丁基酮，完成后再次升温至120℃反应3h，测量NCO基含量，即得到半封闭异氰酸酯；
(b2)在装有温度计、搅拌器和回流冷凝管的反应瓶中，依次加入60份水性羟基丙烯酸树脂、30份半封闭异氰酸酯，搅拌并升温至60℃，加入6份乙酸、5份金属粉末、5份氧化石墨烯粉末、10份异丙醇和30份去离子水，然后继续搅拌20min，制得色浆；
(c2)将50份有机胺改性环氧树脂、10份二乙二醇丁醚、15份双酚A聚氧乙烯醚、5份甲基异丁基酮、20份半封闭异氰酸酯以及30份去离子搅拌混合均匀，即得乳液，固含量为50％；所述金属粉末粒径为80μm；氧化石墨烯粉末粒径为30μm、所述金属粉末为锌粉；
(d2)按色浆：乳液＝1:4的比例混合，再加入5份去离子水搅拌均匀熟化48h；然后加入10份自修复腐蚀微胶囊并继续搅拌30min，即得阴极电泳涂料，然后将阴极电泳涂料放入阴极电泳槽中；
(4)阴极电泳：将钢筋置于阴极电泳槽，设置电泳工艺参数为：阴极电泳槽液固含量15％、pH值6.5、电导率500us/cm、槽液温度50℃、电泳电压100V、电泳时间10min；
(5)固化：将电泳后的钢筋放入烘干箱中，设置温度为150℃，时间为20min，自然冷却即可。
1、对上述制备的混凝土结构涂层进行粘结性测试，根据《色漆和清漆拉开法附着力试验》规范要求，测试耐腐蚀涂层附着力效果，通过拉脱试验得出涂层与混凝土的附着力。结果如表1。
表1
Figure BDA0002879302840000081
从粘结强度数据可知，本发明制备的耐腐蚀涂层具有高粘结强度，可以保证涂层不容易在环境外力下导致脱落。
2、对实施例1-3的耐腐蚀涂层以及裸钢筋进行腐蚀性能测试，测试采用PARSTAT电化学工作站，以参比电极为饱和甘汞电极、辅助电极为高纯石墨棒、工作电极为待测试样构成的标准三电极系统，腐蚀电解质为质量分数3.5wt％的NaCl溶液，测试样品的极化曲线，其中曲线a-d分别对应裸钢筋、实施例1-3的极化曲线。通过Tafel曲线外推法得到腐蚀电位、腐蚀电流密度，记录于表2。
表2
裸露钢筋 实施例1 实施例2 实施例3
腐蚀电位(V) -0.51 -0.32 -0.31 -0.28
腐蚀电流密度(A) 5.2×10<sup>-7</sup> 4.1×10<sup>-7</sup> 2.5×10<sup>-8</sup> 1.3×10<sup>-9</sup>
从Tafle极化曲线及其拟合数据可知，本发明制备的耐腐蚀涂层具有更正的腐蚀电位，低于裸露钢筋的-0.51V、且腐蚀电流密度低至10-9数量级，由此说明，涂层具有优异的耐腐蚀性能。
以上实施方式仅用于说明本发明，而并非对本发明的限制，有关技术领域的普通技术人员，在不脱离本发明的精神和范围的情况下，还可以做出各种变化和变型，因此所有等同的技术方案也属于本发明的范畴，本发明的专利保护范围应由权利要求限定。

Claims (7)

1.一种海工混凝土用钢筋耐腐蚀涂层的制备方法，其特征在于，包括以下步骤：
（1）对钢筋表面进行预处理：钢筋经除油、酸洗、水洗、喷砂后备用；
（2）制备自修复腐蚀微胶囊：
（a1）将10～12份尿素、18～20份甲醛、1～3份氯化铵倒入反应器中，加入pH调节剂调节pH至为8～10，搅拌均匀后升温至60～80℃下进行回流反应2～3h形成脲醛树脂预聚体；
（b1）将5～10份间苯二酚、3～7份聚乙烯醇、10～20份亚麻籽油、1～3份2-苯基苯并咪唑，在50～60℃下搅拌10～15min，加入1～5份去离子水和0.1～0.5份十二烷基苯磺酸钠，乳化20～30min形成油乳状液；
（c1）将步骤（a1）得到的脲醛树脂预聚体加入至步骤（b1）油乳状液中，用盐酸调节pH为3～4，在70～90℃下回流反应2～3 h，将所得产物真空抽滤，用去离子水和丙酮洗涤，放至烘干箱中干燥，即得自修复腐蚀微胶囊；
（3）制备阴极电泳涂料：
（a2）在反应釜中加入5～10份2,4-甲苯二异氰酸酯和20～30份丙二醇甲醚，在保护气氛下搅拌升温至50～60℃后，在2～3h内滴加完3～5份甲基异丁基酮，完成后再次升温至110～120℃反应2～3h，测量NCO基含量，即得到半封闭异氰酸酯；（b2）在装有温度计、搅拌器和回流冷凝管的反应瓶中，依次加入50～60份水性羟基丙烯酸树脂、10～30份半封闭异氰酸酯，搅拌并升温至40～60℃，加入2～5份乙酸、1～5份金属粉末、1～5份氧化石墨烯粉末、5～10份异丙醇和10～30份去离子水，然后继续搅拌10～20min，制得色浆；
（c2）将30～50份有机胺改性环氧树脂、2～10份二乙二醇丁醚、5～15份双酚A聚氧乙烯醚、1～5份甲基异丁基酮、10～20份半封闭异氰酸酯以及20～30份去离子搅拌混合均匀，即得乳液，固含量为30～50%；
（d2）按色浆：乳液＝（1:2）～（1:4）的比例混合，再加入1～5份去离子水搅拌均匀熟化24-48h；然后加入5～10份自修复腐蚀微胶囊并继续搅拌10～30min，即得阴极电泳涂料，然后将阴极电泳涂料放入阴极电泳槽中；
（4）阴极电泳：将钢筋置于阴极电泳槽，设置电泳工艺参数为：阴极电泳槽液固含量10％～15％、pH值5.5～6.5、电导率200～500us/cm、槽液温度30～50℃、电泳电压50～100V、电泳时间3～10min；
（5）固化：将电泳后的钢筋放入烘干箱中，设置温度为150～200℃，时间为20～40min，自然冷却即可。
2.根据权利要求1所述的制备方法，其特征在于，所述pH调节剂为氢氧化钠或三乙醇胺。
3.根据权利要求1所述的制备方法，其特征在于，所述除油步骤为将钢筋放入含碳酸钠20～30g/L、磷酸钠30～50g/L、硅酸钠10～20g/L的水的溶液中超声清洗10～20min；除油温度为30～50℃。
4.根据权利要求1所述的制备方法，其特征在于，所述酸洗步骤为将钢筋放入0.5～1mol/L的稀盐酸溶液中浸泡5～10min。
5.根据权利要求1所述的制备方法，其特征在于，所述金属粉末粒径为50～80μm；氧化石墨烯粉末粒径为10～30μm。
6.根据权利要求1所述的制备方法，其特征在于，所述金属粉末为锌粉或镁粉。
7.一种海工混凝土用钢筋耐腐蚀涂层，其特征在于，所述耐腐蚀涂层由权利要求1-6任一项所述制备方法制备。
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