CN102264819B - 含纳米颗粒的抗腐蚀涂料和涂层 - Google Patents

含纳米颗粒的抗腐蚀涂料和涂层 Download PDF

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CN102264819B
CN102264819B CN200980149054.1A CN200980149054A CN102264819B CN 102264819 B CN102264819 B CN 102264819B CN 200980149054 A CN200980149054 A CN 200980149054A CN 102264819 B CN102264819 B CN 102264819B
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Abstract

本发明涉及抗腐蚀涂料和涂层的制剂，它基于环氧树脂、聚氨酯树脂、丙烯酸类树脂、烷基类树脂、聚酯树脂或其混合物，溶解于有机或无机溶剂，它包括大量主要二维生长的纳米颗粒，其横向尺寸和厚度分别为几百纳米和约1纳米，其中所述制剂的粘度低于55000mPa·s。

Description

含纳米颗粒的抗腐蚀涂料和涂层
本发明涉及含纳米片（nanoplatelet）的抗腐蚀涂料和涂层。
具体地本发明涉及含纳米颗粒的抗腐蚀涂料和涂层，所述纳米颗粒由片状的无机硅酸铝组成，下文中表示为纳米粘土（nanoclay）。
已知涂层、涂料和底漆制剂（primer formulations）基于包含固体颗粒，颜料，增塑剂和其他工艺助剂的聚合物溶解于有机溶剂(有机基涂层)或水(水基涂层)。
还已知目前市售的抗腐蚀涂料和涂层中，环氧树脂(epoxide)、聚氨酯或丙烯酸涂料和涂层具有良好的粘附力和耐久性，具体地，可广泛地用来涂覆钢结构来减少氧和湿气结合活性引起的腐蚀。
但是，这些涂料和涂层其固有组成的结果是它们吸收湿气，并且不能作为氧气的最佳屏障。湿气吸收和氧的通入是涂覆金属腐蚀过程的原因，导致金属-涂层界面上氧化物的形成。这一现象之后接着发生涂层分离(脱粘)，且金属基板劣化的加剧。
为了克服已知这些涂料和涂层的缺陷，美国专利第6,878,767号公开了一种渗透性降低的涂料制剂，它包括成膜剂、颜料和大量经化学处理的片状纳米颗粒，该纳米颗粒主要是二维生长的，其横向尺寸和厚度分别为几百纳米和约1纳米。根据上述专利，分散在制剂中的片(优选硅酸铝，均由水-不可渗透的材料组成)的体积百分比为1至10%，并且所述片经有机(例如胺基-或环氧基-封端的硅烷)或无机(例如脂肪酸)化合物处理，以促进其根据施涂涂料的基板的平行方向取向，从而增加所述片的分子间力。通过按照基板表面平行方向设置，所述片能降低腐蚀液体或气体分子可通过的空间，增加到达涂层和基板界面所需的距离，从而减少界面上氧化物形成和后续涂层脱粘的可能
另一方面，已经证明美国专利第6,878,767号的制剂不允许最佳的片取向，从而降低加入板的防水效果。通过显微分析，特别是透射电子显微镜法(TEM)，和渗透测量，可以证实由于制剂粘性过大，纳米粘土在纳米水平的顺序和排列被打乱，导致对湿气和氧的阻隔效果降低，增加了后续的腐蚀。事实的结果是，由于其形状具有相对于厚度特别延伸的表面(高纵横比)，加入涂料聚合树脂的所述片容易被聚合物分子固定而不能移动。
基于以上内容，明显需要提供一种包含纳米尺寸片的抗腐蚀涂料和涂层的制剂来克服美国专利第6,878,767号中所述制剂的缺陷。
本发明提供解决这一问题的方案，旨在提供一种包含纳米粘土的抗腐蚀涂料和涂层的制剂，其中所述纳米粘土经过化学处理，并且控制粘度，使其有利于纳米粘土的排列平行于制剂要施涂的基板。
因此本发明的目的是提供一种含纳米粘土的抗腐蚀涂料和涂层的制剂或其制备方法，它能消除现有技术方案的限制并得到上述技术效果。
本发明的另一个目的是采用上述制剂和方法能充分降低制备和操作成本。
本发明的另一个、但非最后一个目的是提供一种非常简单、安全和可靠的制剂和方法。
因此，本发明的第一个特定目的是提供一种基于环氧化物、聚氨酯、丙烯酸类、醇酸类(alkydic)、聚酯树脂或其混合物的抗腐蚀涂料和涂层溶解于有机或无机溶剂的制剂，它包括大量主要二维生长的纳米颗粒，其横向尺寸和厚度分别为几百纳米和约1纳米，其中所述制剂根据ASTM D4212在10rpm测定的转动粘度低于55000mPa·s，优选低于40000mPa·s。
具体地，本发明中所述纳米颗粒的量以所述制剂总重量计低于2wt.%，优选以所述制剂总重量计低于1wt.%，最优选以所述制剂总重量计等于0.5wt.%。
具体地，本发明中所述纳米颗粒由包含可进行离子交换反应的离子的材料组成，所述材料预先通过离子交换反应用长链分子的离子处理，优选至少16个碳原子的长链分子的离子，以达到良好的Na+纳米颗粒嵌入和与双酚A二缩水甘油醚基质的物理相容性。
根据本发明，优选所述纳米颗粒由硅铝酸盐(silico-aluminate)基材料组成，更优选由蒙脱石组成。
此外，根据本发明，所述长链分子的离子通过将胺或与其它制剂组分相容的其它化合物质子化得到。
本发明的另一个特定目的是提供一种基于环氧树脂、聚氨酯树脂、丙烯酸类树脂、醇酸(alkydic)树脂、聚酯树脂或其混合物的抗腐蚀涂料和涂层的浓缩制剂，它包括大量主要二维生长的纳米颗粒，其横向尺寸和厚度分别为几百纳米和约1纳米，在加入有机或无机溶剂之后，所述制剂的粘度低于55000mPa·s。
以下具体结合优选的实施方式和一些示例性的实施例所描述的本发明是示意性的，而非限制性的。
根据本发明，制备所述制剂的片经过化学处理以促进其按照施涂涂料的基板的平行方向取向，从而增加所述片的分子间力。此外，控制粘度不能达到阻碍所述片在由聚合物涂料组成的基质内方便地移动的数值，即通过用于在基板上涂覆涂料层的设备进行的力学作用的结果是得到平行于金属基板的排列(因此能提供尽量大的腐蚀保护)。此外，为得到足够低的粘度，可以向涂料中加入溶剂(在干燥过程中蒸发)或者减少环氧化物的固体含量(例如：常规涂料中使用的碳酸钙、金属氧化物和其它固体)。
实施例1纳米粘土的预处理
50g Cloisite Na纳米粘土(NC-Na)，CAS N.1318-93-0；95Meq/100g，购自南部粘土产品公司(Southern Clay Products)，在室温下将其分散在1500ml水中30分钟，然后将所得分散体在85℃加热并保持2小时。
另外制备第二溶液，在85℃将19g十八烷基胺(ODA)，C18H39N，CAS N.124-30-1，FW=269,51,购自福卡公司(Fluka),目录号N.74752溶解于1300ml水中得到第二溶液。然后加入37%盐酸(HCl)至pH为4.5，FW=36,5，搅拌溶液0.3小时。
再将该溶液加入上述水纳米粘土分散体，85℃混合1小时，然后冷却。
这种条件下，形成白色沉淀，再将沉淀从澄清液中分离并充分清洗，先用乙醇，再用水清洗三次。
然后收集固体沉淀，80℃加热干燥15小时，再在110℃干燥2小时。
干燥的沉淀由片状Cloisite Na官能化纳米粘土组成，可以加入涂料中使用。
处理纳米粘土的原则是允许Na+(或者要处理的纳米粘土中的其他离子)与包含长链的离子进行离子交换。这样形成陶瓷纳米粘土结构的片之间的距离增加，从而促进纳米粘土的分层，得到单层纳米粘土(1nm厚)。
可以使用的包含长链的离子是胺，用这样的酸量将其质子化：使得质子化作用得以进行，即铵离子与Na+离子交换(具体到实施例1中，十八烷基胺用盐酸质子化)。
当质子化的胺溶液加入陶瓷纳米粘土的水分散体时发生离子交换。所得沉淀由经ODA(是疏水的)处理的纳米粘土组成。
实施例2含功能化纳米粘土的底漆制剂(底漆)的制备
按照表1中所示的各种组成，将按实施例1方法制得的纳米粘土加入环氧底漆制剂(底漆)，混合直至得到均一的分散体。
将所得的各种底漆组合物分别施涂到相同的金属基板上，再进行分析，结果如表1所示。
表1
Figure GDA00003339910400041
具体地，表1中，%NC表示基于制剂总量的纳米粘土百分比，粘度是10rpm时按照ASTM D4212方法测得的旋转粘度，起泡数是暴露于盐水喷涂(盐喷涂测试：ASTM B117)700小时后测得的，电阻是暴露700小时后和根据电化学阻抗谱：ISO16773-3:2009厚度为80μm时测得的。
实施例3包含功能化纳米粘土的涂料制剂的制备
按照表2中所示的各种组成，将按实施例1方法制得的纳米粘土加入环氧涂料制剂，混合直至得到均一的分散体。
将所得的各种涂料组合物分别施涂到相同的金属基板上，再进行分析，结果如表1所示。
表2
具体地，表2中，%NC表示基于制剂总量的纳米粘土百分比，粘度是10rpm时按照ASTM D4212方法测得的旋转粘度，起泡数是暴露于盐水喷涂(盐喷涂测试：ASTM B117)700小时后测得的，电阻是暴露700小时后和根据电化学阻抗谱：ISO16773-3:2009厚度为150μm时测得的。
实施例4：包含功能化纳米粘土的涂料制剂分离强度的对比评估
按照表3中所示的不同组成，将按照实施例1方法得到的纳米粘土和未经同样处理的其他closite纳米粘土(30B closite)加入环氧涂料制剂(表中第一行表示未加入纳米粘土的制剂)；分别施涂到相同的金属基板(来形成低厚度涂层)，然后通过撕拉分析手段进行粘附力测试，所得结果如表3所示。
根据EN ISO4624方法的撕拉实验是旨在检验涂层质量的直接方法，通过破坏性测试来评价涂料涂层的分离强度。对每种制剂进行干湿条件下两种粘附力测试。
表3
Figure GDA00003339910400051
实施例证实本发明所述的新制剂通过金属表面上的保护涂层能抑制湿气和氧的渗透作用，从而将腐蚀作用降至最低。这种抑制作用是通过实施例1中处理方法得到的表面延伸的无机纳米粘土有序且平行取向的结果。
此外，实施例显示根据本发明加入功能化纳米粘土的抗腐蚀制剂比未加入功能化纳米粘土的制剂更有效。
对于本发明加入抗腐蚀涂料和涂层制剂的纳米粘土的量，使用的纳米粘土的量一定不能引起不希望的粘度升高。为得到所述目标粘度，所述涂料制剂可以方便地使用不会反应的试剂(有机或水基)稀释，来降低粘度水平，并在涂层固化之后蒸发除去。
根据优选的实施方式对本发明的描述是示例性的，而非限制性的，应理解本领域技术人员所作出的变化方式和/或改变未脱离以下所附权利要求所保护的范围。

Claims (8)

1.一种抗腐蚀涂料和涂层的制剂，它基于环氧树脂、聚氨酯树脂、丙烯酸类树脂、醇酸树脂、聚酯树脂或其混合物，并且，以所述制剂总重量计，包括大于0至小于2重量％的主要二维生长的纳米颗粒，其横向尺寸和厚度分别为几百纳米和约1纳米，其中所述纳米颗粒由包含能够进行离子交换反应的离子的材料组成，所述材料预先通过离子交换反应用具有至少16个碳原子的长链分子的离子进行处理，所述制剂在10rpm条件下根据ASTM D4212测得的转动粘度低于55000mPa·s。
2.如权利要求1所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述制剂的粘度低于40000mPa·s。
3.如权利要求2所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述纳米颗粒的量低于1wt.%，以所述制剂总重量计。
4.如权利要求3所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述纳米颗粒的量为0.5wt.%，以所述制剂总重量计。
5.如权利要求3或4所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述纳米颗粒由硅-铝酸盐基材料组成。
6.如权利要求3或4所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述纳米颗粒由蒙脱石组成。
7.如权利要求1-4中任一项所述的抗腐蚀涂料和涂层的制剂，其特征在于，所述长链分子离子通过对胺或者与制剂的其它组分相容的其它化合物进行质子化而得到。
8.一种抗腐蚀涂料和涂层的浓缩制剂，它基于环氧树脂、聚氨酯树脂、丙烯酸类树脂、醇酸树脂、聚酯树脂或其混合物，以所述制剂总重量计，包括大于0至小于2重量％的主要二维生长的纳米颗粒，其横向尺寸和厚度分别为几百纳米和约1纳米，其中所述纳米颗粒由包含能够进行离子交换反应的离子的材料组成，所述材料预先通过离子交换反应用具有至少16个碳原子的长链分子的离子进行处理，在加入有机或无机溶剂之后，所述制剂在10rpm条件下根据ASTM D4212测得的转动粘度低于55000mPa·s。
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