CN106634422B - 一种用于检测金属腐蚀的高分子涂层材料及其制备方法 - Google Patents
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Abstract
本发明属于腐蚀检测领域,具体涉及一种用于检测金属腐蚀的智能高分子涂层材料及其制备方法。本发明的用于检测金属腐蚀的高分子涂层材料,包括高分子树脂和荧光检测试剂,其中,所述荧光检测试剂包括二氧化硅和荧光分子/杂多酸复合物,所述荧光分子在高分子树脂中的浓度不低于5ppm。本发明的荧光检测试剂可以对pH发生响应性的荧光指示。当腐蚀发生时,腐蚀区域的pH值将升高,智能高分子涂层材料中荧光分子在碱性的高pH值下迅速做出反应,进而在腐蚀处具有强烈的荧光指示。
Description
技术领域
本发明属于腐蚀检测领域,具体涉及一种用于检测金属腐蚀的高分子涂层材料及其制备方法。
背景技术
腐蚀是当今社会面临的一个非常严峻的问题,据不完全统计,我国每年因腐蚀所造成的经济损失占每年GDP的3%,这个数字超过了因地震、暴风、洪水等各种自然灾害所造成的经济损失的总和。因此,腐蚀防护一直都是世界各国重点研究的科学领域。另一方面,人们迫切希望能够对腐蚀的发生进行检测,从而使人们能够及早发现腐蚀并采取适当的措施对腐蚀予以防护,以延长金属的使用寿命。现有针对腐蚀的检测方法多种多样,大致可以分为机械方法、无损检测法以及电化学法。其中,无损检测法因其对金属无破坏性及原位检测等优点得到了很大的发展。无损探测是通过利用声、光、电、热、磁等手段对金属材料内部结构的形态以及变化所作出的反应进行检测,从而查明材料内部是否存在异常或者缺陷。当腐蚀发生至一定程度时,金属材料表面的形态或组成会发生一定的变化,从而与周围正常金属材料产生区别,声、光、电、热、磁等信号在腐蚀区域会发生较大变化,从而实现对腐蚀的检测。例如,射线无损检测技术可通过X射线、γ射线以及中子射线等对材料的缺陷进行检测,由于射线穿过待检测材料时,在缺陷处的射线强度与周围的强度不同,从而在射线胶片上的感光程度也存在差异,呈现出不连续的图像信息。然而,这些检测手段必须在腐蚀对金属造成足够破坏并产生差异之后才能发挥作用,并不能在腐蚀发生的早期阶段进行检测,这将不利于更有效的延长金属的使用寿命。而且,这些检测手段所使用的仪器不仅价格昂贵,而且难以操作,对操作人员的专业知识需求较高,增加了腐蚀检测的难度。
荧光分子因其灵敏高效的发光特性而在细胞成像、荧光标记、靶基因的确定等生物领域得到了广泛的应用。因此,将荧光分子用于腐蚀的检测能够在腐蚀发生的早期阶段进行成像,不仅能够使人们更早更及时的发现腐蚀,而且其原位检测的特点可以无损的对腐蚀区域进行检测。但是,现有研究中采用的一些荧光分子在涂层中的添加当量较大(Anita Augustyniak,etal.,Progress in Organic Coatings,71(2011)406–412;J.Zhang,et al.,Corrosion,55(1999)957-967.),一般在0.5wt%以上,并且这些荧光分子直接加入到涂层中,易损失且与周围环境发挥相互作用而失效。
发明内容
本发明的目的在于提供一种用于检测金属腐蚀的智能高分子涂层材料。
本发明原理为:荧光检测试剂可以对pH发生响应性的荧光指示。当腐蚀发生时,腐蚀区域的pH值将升高,智能高分子涂层材料中荧光分子在碱性的高pH值下迅速做出反应,进而在腐蚀处具有强烈的荧光指示。
本发明的具体技术方案如下:
本发明的用于检测金属腐蚀的高分子涂层材料,其中,所述高分子涂层材料包括高分子树脂和荧光检测试剂,其中,所述荧光检测试剂包括荧光分子、杂多酸和二氧化硅,所述荧光分子在高分子树脂中的浓度不低于5ppm,最优添加浓度为10~100ppm。
根据本发明所述的高分子涂层材料,所述荧光检测试剂中杂多酸与荧光分子摩尔比应大于等于1,最优摩尔比为1~5。
根据本发明所述的高分子涂层材料,其中作为优选地,所述荧光分子可以为异硫氰酸荧光素、二氯荧光素、硫胺素、香豆素、2-萘酚、1-萘胺、2-萘胺、水杨酸或曙红中的一种或几种。
根据本发明所述的高分子涂层材料,其中,所述杂多酸的化学结构通式为HmXM12O40,其中,X=P、Si或As,M=Mo或W;或,所述杂多酸的化学结构通式为HnX2M18O62,其中,X=P、Si或As,M=Mo或W。
根据本发明所述的高分子涂层材料,其中作为优选地,所述高分子树脂可以为环氧树脂、聚氨酯树脂、丙烯酸树脂、醇酸树脂、酚醛树脂或者聚硅氧烷中的一种或几种。
本发明的上述高分子涂层材料的制备方法,包括以下步骤:
1)将荧光分子和杂多酸溶解,形成荧光分子/杂多酸复合物,然后加入二氧化硅纳米容器,搅拌后干燥,得到荧光检测试剂;
2)将荧光检测试剂复合至高分子树脂中,得到高分子涂层材料。
本发明中起显色作用的成分是荧光分子,只需保证换算出的荧光分子含量在高分子涂层中的含量不低于5ppm,所以本发明对二氧化硅的量不做限定,作为优选地,可以在采用的荧光检测试剂中,添加二氧化硅的质量百分比在95wt%~99wt%。
作为优选地,在步骤1中,加入二氧化硅之后搅拌0.5h以上,最优搅拌时间2~6h。
根据本发明所述的制备方法,步骤2中,所述的“复合”即混合,是指单纯的物理混合至均匀。
根据本发明所述的制备方法,其中优选地,步骤1)溶解所用溶剂为水、甲醇、乙醇、异丙醇或丙酮中的一种或几种。所述溶剂用量只要满足完全溶解荧光分子与杂多酸即可,本发明不做特别限定。
本发明所述的一种高分子涂层材料可以适用于各种金属及合金,例如包括但不限于钢,铁,铝,镁,铜,及它们的合金。
在本发明中,我们采用具有一种具有pH响应性的检测试剂加入到高分子涂层中,当金属部分区域发生腐蚀时,由于腐蚀造成的pH环境变化进而在其涂层保护处显示出强烈的荧光。此外,环境响应性的智能检测试剂可以在涂层中保持长久有效,涂层中的使用量仅仅在5ppm时,其在腐蚀发生时可以对腐蚀做出响应,可有效的智能自我检测腐蚀,以便于人们及时对金属腐蚀采取相应对策。
附图说明
图1为本发明金属钢的用于检测腐蚀的智能涂层材料在3.5%NaCl溶液中浸泡后的光学图片。
图2为本发明金属钢的用于检测腐蚀的智能涂层材料在3.5%NaCl溶液中浸泡后的激光共聚焦图片。
图3为本发明金属铜的用于检测腐蚀的智能涂层材料在3.5%NaCl溶液中浸泡后的激光共聚焦图片。
图4为本发明金属镁的用于检测腐蚀的智能涂层材料在3.5%NaCl溶液中浸泡后的激光共聚焦图片。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
将荧光分子异硫氰酸荧光素和H3PW12O40按摩尔比1:2溶解于水中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子异硫氰酸荧光素的二氧化硅(二氧化硅占95wt%)。将负载了荧光分子异硫氰酸荧光素的二氧化硅分散至环氧树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子异硫氰酸荧光素的当量含量为5ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。涂有用于检测金属腐蚀的智能高分子涂层材料的钢片在3.5%NaCl溶液中浸泡2h之后光学图片如图1所示,其激光共聚焦图见图2。图2显示在点状腐蚀的地方具有强烈的荧光指示。
实施例2
将荧光分子异硫氰酸荧光素和H3PMo12O40按摩尔比1:2溶解于甲醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子异硫氰酸荧光素的二氧化硅(二氧化硅占96wt%)。将负载了荧光分子异硫氰酸荧光素的二氧化硅分散至聚氨酯树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子异硫氰酸荧光素的当量含量为7ppm。将该树脂涂至铜片表面固化,然后浸入3.5%NaCl溶液中,检测铜片表面的腐蚀。涂有用于检测金属腐蚀的智能高分子涂层材料的铜片在3.5%NaCl溶液中浸泡2h之后的激光共聚焦图见图3。图3显示在涂层材料划痕破损引起的金属腐蚀处具有强烈的荧光指示。
实施例3
将荧光分子二氯荧光素和H4SiW12O40按摩尔比1:1溶解于水中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子二氯荧光素的二氧化硅(二氧化硅占99wt%)。将负载了荧光分子二氯荧光素的二氧化硅分散至丙烯酸树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子二氯荧光素的当量含量为10ppm。将该树脂涂至铝片表面固化,然后浸入3.5%NaCl溶液中,检测铝片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例4
将荧光分子异硫氰酸荧光素和H4SiMo12O40按摩尔比1:3溶解于异丙醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子异硫氰酸荧光素的二氧化硅(二氧化硅占95wt%)。将负载了荧光分子异硫氰酸荧光素的二氧化硅分散至醇酸树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子异硫氰酸荧光素的当量含量为15ppm。将该树脂涂至镁片表面固化,然后浸入3.5%NaCl溶液中,检测镁片表面的腐蚀。涂有用于检测金属腐蚀的智能高分子涂层材料的镁片在3.5%NaCl溶液中浸泡2h之后的激光共聚焦图见图4。图4显示在涂层材料划痕腐蚀处具有强烈的荧光指示。
实施例5
将荧光分子硫胺素和H3AsW12O40按摩尔比1:4溶解于丙酮中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子硫胺素的二氧化硅(二氧化硅占98wt%)。将负载了荧光分子硫胺素的二氧化硅分散至酚醛树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子硫胺素的当量含量为7ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例6
将荧光分子2-萘酚和H3AsMo12O40按摩尔比1:1溶解于丙酮中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子2-萘酚的二氧化硅(二氧化硅占99wt%)。将负载了荧光分子2-萘酚的二氧化硅分散至醇酸树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子2-萘酚的当量含量为15ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例7
将荧光分子水杨酸和H6P2W18O62按摩尔比1:5溶解于乙醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子水杨酸的二氧化硅(二氧化硅占96wt%)。将负载了荧光分子水杨酸的二氧化硅分散至环氧树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子水杨酸的当量含量为5ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例8
将荧光分子2-萘胺和H6P2Mo18O62按摩尔比1:2溶解于乙醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子2-萘胺的二氧化硅(二氧化硅占98wt%)。将负载了荧光分子2-萘胺的二氧化硅分散至丙烯酸树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子2-萘胺的当量含量为5ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例9
将荧光分子曙红和H8Si2W18O62按摩尔比1:3溶解于甲醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子曙红的二氧化硅(二氧化硅占96wt%)。将负载了荧光分子曙红的二氧化硅分散至酚醛树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子曙红的当量含量为20ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例10
将荧光分子异硫氰酸荧光素和H8Si2Mo18O62按摩尔比1:2溶解于异丙醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子异硫氰酸荧光素的二氧化硅(二氧化硅占96.5wt%)。将负载了荧光分子异硫氰酸荧光素的二氧化硅分散至醇酸树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子异硫氰酸荧光素的当量含量为100ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例11
将荧光分子1-萘胺和H6As2W18O62按摩尔比1:1溶解于异丙醇中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子1-萘胺的二氧化硅(二氧化硅占95wt%)。将负载了荧光分子1-萘胺的二氧化硅分散至酚醛树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子1-萘胺的当量含量为5ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
实施例12
将荧光分子异硫氰酸荧光素和H6As2Mo18O62按摩尔比1:4溶解于丙酮中,然后加入二氧化硅,搅拌一段时间后干燥,得到负载了荧光分子异硫氰酸荧光素的二氧化硅(二氧化硅占98wt%)。将负载了荧光分子异硫氰酸荧光素的二氧化硅分散至酚醛树脂中,得到用于检测金属表面腐蚀的环氧树脂涂层材料,其中荧光分子异硫氰酸荧光素的当量含量为50ppm。将该树脂涂至钢片表面固化,然后浸入3.5%NaCl溶液中,检测钢片表面的腐蚀。激光共聚焦图片显示腐蚀的地方具有强烈的荧光指示。
当然,本发明还可以有多种实施例,在不背离本发明精神及其实质的情况下,熟悉本领域的技术人员可根据本发明的公开做出各种相应的改变和变形,但这些相应的改变和变形都应属于本发明的权利要求的保护范围。
Claims (4)
1.一种用于检测金属腐蚀的高分子涂层材料,其特征在于,所述高分子涂层材料包括高分子树脂和荧光检测试剂,其中,所述荧光检测试剂包括荧光分子、杂多酸和二氧化硅纳米容器,所述荧光分子在高分子树脂中的浓度为5~100 ppm;所述荧光检测试剂中杂多酸与荧光分子摩尔比大于等于1;
其中,所述杂多酸的化学结构通式为HmXM12O40,其中,X = P、Si或As,M = Mo或W;或,所述杂多酸的化学结构通式为HnX2M18O62,其中,X = P、Si或As,M = Mo或W;
所述荧光分子为异硫氰酸荧光素、二氯荧光素、硫胺素、香豆素、2-萘酚、1-萘胺、2-萘胺、水杨酸或曙红中的一种或几种。
2.根据权利要求1所述的高分子涂层材料,其特征在于,所述高分子树脂为环氧树脂、聚氨酯树脂、丙烯酸树脂、醇酸树脂、酚醛树脂或者聚硅氧烷中的一种或几种。
3.一种权利要求1或2所述高分子涂层材料的制备方法,包括以下步骤:
1)将荧光分子和杂多酸溶解,然后加入二氧化硅纳米容器,搅拌后干燥,得到荧光检测试剂;
2)将荧光检测试剂复合至高分子树脂中,得到高分子涂层材料。
4.根据权利要求3所述的制备方法,其特征在于,步骤1)溶解所用溶剂为水、甲醇、乙醇、异丙醇或丙酮中的一种或几种。
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