CN112778874B - 一种海洋工程混凝土耐腐蚀涂层及其制备方法 - Google Patents

一种海洋工程混凝土耐腐蚀涂层及其制备方法 Download PDF

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CN112778874B
CN112778874B CN202011638575.8A CN202011638575A CN112778874B CN 112778874 B CN112778874 B CN 112778874B CN 202011638575 A CN202011638575 A CN 202011638575A CN 112778874 B CN112778874 B CN 112778874B
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明阳
陈平
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

本发明提供一种海洋工程混凝土耐腐蚀涂层及其制备方法，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，其中A组分按重量份计包括：水性非离子型环氧树脂、C10～C12烷基缩水甘油醚、笼型倍半硅氧烷、金属粉末、镁铝水滑石粉、分散剂、消泡剂；其中B组分按重量份计包括：改性芳香胺类固化剂、C10～C12烷基缩水甘油醚、自修复微胶囊、流平剂、抗氧化剂、附着力促进剂、其他助剂。本发明的耐腐蚀涂层具有优异的粘结性和防腐蚀性，同时能够实现耐腐蚀涂层的自修复性和阻止氯离子的迁移，进而延长了混凝土结构的使用寿命，可以广泛应用于海洋工程混凝土结构的防护。

Description

一种海洋工程混凝土耐腐蚀涂层及其制备方法
技术领域
本发明涉及混凝土防护领域，具体涉及一种海洋工程混凝土耐腐蚀涂层及其制备方法。
背景技术
混凝土广泛应用于海港工程、桥梁、地下工程、基础建设，然而混凝土结构仍然存在外部环境的影响而容易导致其失效，也可引发重大事故。而根据应用的环境存在复杂多样的原因。海洋工程是今年来发展的重点,海工混凝土结构的耐久性、安全性与使用年限一直是研究的重点。由于环境介质中的氯离子或原材料的氯离子侵入混凝土内部引起钢筋锈蚀膨胀造成混凝土胀裂破坏以及腐蚀，显著降低了混凝土结构的耐久性。
混凝土结构的破坏主要介质是水，由于混凝土并非严格意义上的实心，而是存在一定的孔隙，表面明显粗糙，水中的介质带入了CO2会使其发生碳化，而海水中的各种阴离子的侵蚀会严重腐蚀内部钢筋。而提高混凝土结构的措施一方面在于混凝土组成成分的改进，另一方面是在混凝土表面涂覆防腐蚀性质的涂层进而阻止有害介质的侵入。所以混凝土的使用寿命很大程度上取决于涂层的性能。如何寻求更有效的防护仍然是现有技术研究的方向和重点。
发明内容
针对现有技术的不足，本发目的之一在于提供一种海洋工程混凝土耐腐蚀涂层，该耐腐蚀涂层具有优异的粘结性和防腐蚀性，同时能够实现耐腐蚀涂层的自修复性和阻止氯离子的迁移，进而延长了混凝土结构的使用寿命。
为了实现上述技术目的，本发明提供了一种海洋工程混凝土耐腐蚀涂层，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，
其中A组分按重量份计包括：水性非离子型环氧树脂80～100份、C10～C12烷基缩水甘油醚5～10份、笼型倍半硅氧烷1～5份、金属粉末2～3份、镁铝水滑石粉1～2份、分散剂0.1～0.5份、消泡剂0.1～0.5份；
其中B组分按重量份计包括：改性芳香胺类固化剂50～70份、C10～C12烷基缩水甘油醚5～10份、自修复微胶囊5～10份、流平剂1～3份、抗氧化剂1～5份、附着力促进剂0.1～1份、其他助剂1～3份。
进一步地，所述进一步地选择十三氟辛基丙基笼型倍半硅氧烷或十二氟庚基丙基笼型倍半硅氧烷。
进一步地，所述金属粉末为锌粉或镁粉，所述金属粉末的粒径在10～20μm；所述镁铝水滑石粉的粒径在10～20μm。
进一步地，所述分散剂选自聚氧乙烯异癸基醚、聚氧乙烯苯乙烯基苯基醚中的一种或多种。
进一步地，所述消泡剂为有机硅类消泡剂；所述流平剂为有机硅聚醚类共聚物。
进一步地，所述自修复微胶囊通过如下步骤制备：将0.5～1g十二烷基苯磺酸分散于500mL去离子水中，搅拌的过程中缓慢加入30～50g桐油形成乳液，持续5～10min后加入15～20g尿素和5～10g六甲氧基三聚氰胺树脂；然后加入3～5g氯化铵和3～5g间苯二酚，继续搅拌10～20min后滴加稀盐酸调节乳液pH至为5.5～6.5，随后加入10～15g饱和甲醛溶液和3～5滴辛醇，升高温度至60～65℃进行反应60～120min；反应结束后停止搅拌、静置5～10min后进行过滤，对过滤后的物质进行冲洗后在30～50℃下干燥即得自修复微胶囊。
进一步地，所述抗氧化剂选自4-叔丁基邻苯二酚、2-叔丁基氢醌、2,6-二叔丁基-对甲酚、2,2-亚甲基-双(4-甲基-6-叔丁基苯酚)中的一种或多种。
进一步地，所述附着力促进剂为BYK-4511或AP-507。
进一步地，所述其他助剂包括增稠剂、紫外吸收剂中的一种或多种。
进一步地，所述增稠剂选自乙基纤维素、羟甲基纤维素、羟乙基纤维素、羧甲基纤维素中的一种或多种。
进一步地，所述紫外吸收剂选自2-羟基-4-正辛氧基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-(2-羟基3,5-二叔丁基苯基)-5-氯代苯并三唑中的一种或多种。
本发明的另一目的在于提供一种上述海洋工程混凝土耐腐蚀涂层的制备方法，包括以下步骤：
(1)对混凝土表面进行清理；
(2)将分散剂、金属粉末、镁铝水滑石粉依次加入反应器中，开启搅拌，加热至30～50℃后加入水性非离子型环氧树脂、C10～C12烷基缩水甘油醚，加入消泡剂，继续搅拌20～30min进行抽真空脱泡后，得到A组分；
(3)将改性芳香胺类固化剂、C10～C12烷基缩水甘油醚5～10份加入反应器中，开启搅拌，并升温至70～80℃，搅拌全溶后，缓慢加入自修复微胶囊，降温至室温，依次加入流平剂、抗氧化剂、附着力促进剂、其他助剂，继续搅拌20～30min，得到B组分；
(4)将A组分和B组分等体积混合搅拌均匀后备用；
(5)将步骤(4)的混合物喷涂或刷涂于混凝土表面，干燥后重复喷涂或刷涂2～3次，干燥后在25～30℃、空气相对湿度50～70％下养护2～3天。
以下对本申请各组分的作用以及原理做出解释：
十三氟辛基丙基笼型倍半硅氧烷或十二氟庚基丙基笼型倍半硅氧烷为含有Si-O-Si构成的无机笼状骨架，具有优异的热稳定性，其侧基含氟原子，其特殊的三维纳米结构赋予其优异的疏水、疏油的特性，该组分在涂层中一方面通过其侧基的特性使得涂层界面具有良好的疏水性，从而能够一定程度上阻止水分子通过涂层进入混凝土结构，即相应的降低了腐蚀介质对整体混凝土、钢筋结构的侵蚀；另一方面该型倍半硅氧烷可以进一步提高水性非离子型环氧树脂的交联度，形成杂化环氧树脂，进而提高涂层的粘结性能、拉伸强度以及断裂强度，从而表现出涂层不易在恶劣环境下出现裂纹。
本发明通过抗氧化剂和紫外吸收剂的相互配合，进而改善材料的抗老化性及高温稳定性，能够有效增加涂层的防腐蚀工作年限。
水滑石是由带正电荷的金属氢氧化物层和带负电荷的层间阴离子构成的层状双羟基金属复合氢氧化物。具有较大的比表面积和孔径，易接受客体分子，焙烧后会失去层间阴离子和水，可获得高比表面积的焙烧产物，能够通过再次固定阴离子还原为原始层状结构。同时水滑石的层间阴离子具有迁移性及离子交换特性，处于层间的阴离子可被介质中的其他阴离子所置换。因此，镁铝水滑石粉是一种良好的氯离子固定剂，其均匀分散在涂层中能够有效吸附氯离子，进一步阻止了氯离子穿透涂层进入混凝土结构。
本发明通过制备自修复微胶囊添加至涂层中，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。
本发明一方面通过以上物质之间的作用，使混凝土表面涂覆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。
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洋工程混凝土耐腐蚀涂层的制备。
2、本申请首次利用笼型倍半硅氧烷的特性使得涂层具有优异的粘结性，并进一步配合附着力促进剂的使用，从而在粗糙的混凝土结构表面形成结合牢固的涂层。
3、本发明的涂层具有优异的粘结性和防腐蚀性，同时能够实现耐腐蚀涂层的自修复性和阻止氯离子的迁移，进而延长了混凝土结构的使用寿命。可以广泛应用于海洋工程混凝土结构的防护，也可以应用一般环境下的混凝土结构的保护。
附图说明
图1为实施例1、对比例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
一种海洋工程混凝土耐腐蚀涂层，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，
其中A组分按重量份计包括：水性非离子型环氧树脂80份、C10烷基缩水甘油醚5份、十三氟辛基丙基笼型倍半硅氧烷1份、锌粉末2份、镁铝水滑石粉1份、分散剂聚氧乙烯异癸基醚0.1份、有机硅类消泡剂0.1份；
其中B组分按重量份计包括：改性芳香胺类固化剂50份、C10烷基缩水甘油醚5份、自修复微胶囊5份、流平剂有机硅聚醚类共聚物1份、抗氧化剂4-叔丁基邻苯二酚1份、附着力促进剂BYK-4511 0.1份、紫外吸收剂2-羟基-4-甲氧基二苯甲酮1份。
所述自修复微胶囊通过如下步骤制备：将0.5g十二烷基苯磺酸分散于500mL去离子水中，搅拌的过程中缓慢加入30g桐油形成乳液，持续5min后加入15g尿素和5g六甲氧基三聚氰胺树脂；然后加入3g氯化铵和3g间苯二酚，继续搅拌10min后滴加稀盐酸调节乳液pH至为5.5，随后加入10g饱和甲醛溶液和3滴辛醇，升高温度至60℃进行反应120min；反应结束后停止搅拌、静置5min后进行过滤，对过滤后的物质进行冲洗后在30℃下干燥即得自修复微胶囊。具体耐腐蚀涂层的制备方法相应的如发明内容记载的方法制备。
实施例2
一种海洋工程混凝土耐腐蚀涂层，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，
其中A组分按重量份计包括：水性非离子型环氧树脂90份、C11烷基缩水甘油醚8份、十二氟庚基丙基笼型倍半硅氧烷3份、锌粉末2.5份、镁铝水滑石粉1.5份、分散剂聚氧乙烯苯乙烯基苯基醚0.3份、有机硅类消泡剂0.3份；
其中B组分按重量份计包括：改性芳香胺类固化剂60份、C11烷基缩水甘油醚8份、自修复微胶囊7份、流平剂有机硅聚醚类共聚物1.5份、抗氧化剂2,2-亚甲基-双(4-甲基-6-叔丁基苯酚)5份、附着力促进剂AP-507 0.7份、增稠剂羧甲基纤维素2份。
所述自修复微胶囊通过如下步骤制备：将0.8g十二烷基苯磺酸分散于500mL去离子水中，搅拌的过程中缓慢加入40g桐油形成乳液，持续7min后加入17g尿素和8g六甲氧基三聚氰胺树脂；然后加入4g氯化铵和4g间苯二酚，继续搅拌15min后滴加稀盐酸调节乳液pH至为6，随后加入12g饱和甲醛溶液和4滴辛醇，升高温度至60℃进行反应100min；反应结束后停止搅拌、静置8min后进行过滤，对过滤后的物质进行冲洗后在40℃下干燥即得自修复微胶囊。
具体耐腐蚀涂层的制备方法相应的如发明内容记载的方法制备。
实施例3
一种海洋工程混凝土耐腐蚀涂层，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，
其中A组分按重量份计包括：水性非离子型环氧树脂100份、C12烷基缩水甘油醚10份、十二氟庚基丙基笼型倍半硅氧烷5份、镁粉末3份、镁铝水滑石粉2份、分散剂聚氧乙烯苯乙烯基苯基醚0.5份、有机硅类消泡剂0.5份；
其中B组分按重量份计包括：改性芳香胺类固化剂50份、C12烷基缩水甘油醚10份、自修复微胶囊10份、流平剂有机硅聚醚类共聚物3份、抗氧化剂2,6-二叔丁基-对甲酚5份、附着力促进剂AP-507 0.5份、紫外吸收剂2-羟基-4-甲氧基二苯甲酮3份。
所述自修复微胶囊通过如下步骤制备：将1g十二烷基苯磺酸分散于500mL去离子水中，搅拌的过程中缓慢加入50g桐油形成乳液，持续10min后加入20g尿素和10g六甲氧基三聚氰胺树脂；然后加入5g氯化铵和5g间苯二酚，继续搅拌20min后滴加稀盐酸调节乳液pH至为6.5，随后加入15g饱和甲醛溶液和5滴辛醇，升高温度至65℃进行反应60min；反应结束后停止搅拌、静置10min后进行过滤，对过滤后的物质进行冲洗后在50℃下干燥即得自修复微胶囊。
具体耐腐蚀涂层的制备方法相应的如发明内容记载的方法制备。
为了更好的体现本申请组分的作用，申请人以几种主要成分做了对比例来说明，但这并不是说其他组分的作用和效果不重要。
对比例1
对比例1与实施例1相同，区别在于对比例1不含锌粉末。
对比例2
对比例2与实施例1相同，区别在于对比例2不含自修复微胶囊。
对比例3
对比例3与实施例1相同，区别在于对比例3不含锌粉末和自修复微胶囊。
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。
2、对上述制备的混凝土结构涂层以及未涂覆耐腐蚀涂层的空白样进行盐雾测试，测试在盐雾试验箱、5wt％NaCl作为盐雾源，混凝土结构完全被耐腐蚀涂层包覆，喷雾时间为1500h。盐雾结束后将混凝土结构切开，沿着靠近涂层边缘喷洒硝酸银溶液，根据出现白色AgCl沉淀的情况记录氯离子渗透深度。结果如表1。
表1
Figure BDA0002879293260000071
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。尽管不明显，根据对比例的结果也可以推断出，其他组分对整体的性能也是有一定的降低。
另外，耐腐蚀涂层具有优异的自修复性和阻止氯离子的迁移特性，耐腐蚀涂层几乎能够阻挡氯离子的侵蚀。在不含有自修复微胶囊的对比例来看，混凝土表面的涂层还是存在一定的裂纹或孔隙使得氯离子穿透涂层进入混凝土内部。由此可见，自修复微胶囊的应用能够修复涂层，从而保证涂层的致密性。
3、对实施例1以及对比例1-3的混凝土结构耐腐蚀涂层进行腐蚀性能测试，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3.5％的NaCl溶液，测试样品的极化曲线，其中曲线a-d分别对应实施例1、对比例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
实施例1 对比例1 对比例2 对比例3
腐蚀电位(V) -0.94 -1.05 -1.02 -1.16
腐蚀电流密度(A) 8.7×10<sup>-8</sup> 2.1×10<sup>-7</sup> 1.3×10<sup>-7</sup> 6.5×10<sup>-6</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且腐蚀电流密度低至级10-8数量，由此说明，涂层具有优异的耐腐蚀性能。在不含锌粉的涂层中，其腐蚀电位负移、腐蚀电流密度明显增大，说明书耐腐蚀性相比更差；而且在不含锌粉和自修复微胶囊的涂层，腐蚀电流密度相比负移更大、腐蚀电流密度高达10-6数量级，可见涂层的耐腐蚀性显著降低。由此可见，本发明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。
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 (8)

1.一种海洋工程混凝土耐腐蚀涂层，所述耐腐蚀涂层通过A组分和B组分混合均匀后喷涂或刷涂于混凝土表面，其特征在于，
其中A组分按重量份计包括：水性非离子型环氧树脂80～100份、C10～C12烷基缩水甘油醚5～10份、笼型倍半硅氧烷1～5份、金属粉末2～3份、镁铝水滑石粉1～2份、分散剂0.1～0.5份、消泡剂0.1～0.5份；
其中B组分按重量份计包括：改性芳香胺类固化剂50～70份、C10～C12烷基缩水甘油醚5～10份、自修复微胶囊5～10份、流平剂1～3份、抗氧化剂1～5份、附着力促进剂0.1～1份、其他助剂1～3份；
所述金属粉末为锌粉或镁粉，所述金属粉末的粒径在10～20μm；所述镁铝水滑石粉的粒径在10～20μm；
所述自修复微胶囊通过如下步骤制备：将0.5～1g十二烷基苯磺酸分散于500mL去离子水中，搅拌的过程中缓慢加入30～50g桐油形成乳液，持续5～10min后加入15～20g尿素和5～10g六甲氧基三聚氰胺树脂；然后加入3～5g氯化铵和3～5g间苯二酚，继续搅拌10～20min后滴加稀盐酸调节乳液pH至为5.5～6.5，随后加入10～15g饱和甲醛溶液和3～5滴辛醇，升高温度至60～65℃进行反应60～120min；反应结束后停止搅拌、静置5～10min后进行过滤，对过滤后的物质进行冲洗后在30～50℃下干燥即得自修复微胶囊。
2.根据权利要求1所述的耐腐蚀涂层，其特征在于，所述笼型倍半硅氧烷为十三氟辛基丙基笼型倍半硅氧烷或十二氟庚基丙基笼型倍半硅氧烷。
3.根据权利要求1所述的耐腐蚀涂层，其特征在于，所述分散剂选自聚氧乙烯异癸基醚、聚氧乙烯苯乙烯基苯基醚中的一种或多种；所述消泡剂为有机硅类消泡剂；所述流平剂为有机硅聚醚类共聚物。
4.根据权利要求1所述的耐腐蚀涂层，其特征在于，所述抗氧化剂选自4-叔丁基邻苯二酚、2-叔丁基氢醌、2,6-二叔丁基-对甲酚、2,2-亚甲基-双(4-甲基-6-叔丁基苯酚)中的一种或多种。
5.根据权利要求1所述的耐腐蚀涂层，其特征在于，所述附着力促进剂为BYK-4511或AP-507。
6.根据权利要求1所述的耐腐蚀涂层，其特征在于，所述其他助剂包括增稠剂、紫外吸收剂中的一种或多种。
7.根据权利要求6所述的耐腐蚀涂层，其特征在于，所述增稠剂选自乙基纤维素、羟甲基纤维素、羟乙基纤维素、羧甲基纤维素中的一种或多种；所述紫外吸收剂选自2-羟基-4-正辛氧基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-(2-羟基3,5-二叔丁基苯基)-5-氯代苯并三唑中的一种或多种。
8.一种如权利要求1～7任一项所述海洋工程混凝土耐腐蚀涂层的制备方法，其特征在于，包括以下步骤：
（1）对混凝土表面进行清理；
（2）将分散剂、金属粉末、镁铝水滑石粉依次加入反应器中，开启搅拌，加热至30～50℃后加入水性非离子型环氧树脂、C10～C12烷基缩水甘油醚，加入消泡剂，继续搅拌20～30min进行抽真空脱泡后，得到A组分；
（3）将改性芳香胺类固化剂、C10～C12烷基缩水甘油醚5～10份加入反应器中，开启搅拌，并升温至70～80℃，搅拌全溶后，缓慢加入自修复微胶囊，降温至室温，依次加入流平剂、抗氧化剂、附着力促进剂、其他助剂，继续搅拌20～30min，得到B组分；
（4）将A组分和B组分等体积混合搅拌均匀后备用；
（5）将步骤（4）的混合物喷涂或刷涂于混凝土表面，干燥后重复喷涂或刷涂2～3次，干燥后在25～30℃、空气相对湿度50～70%下养护2～3天。
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