CN106085087A - 一种复合钙质金属铜防腐涂层及其制备方法 - Google Patents
一种复合钙质金属铜防腐涂层及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种复合钙质金属铜防腐涂层,该涂层是由下述重量份的原料组成的:二甲基丙烷羧酸酯0.4‑1、烯丙基聚乙二醇3‑4、棕榈酸钙1‑2、乙烯基三甲氧基硅烷10‑14、1.8‑2g/l的柠檬酸溶液200‑300、硅烷偶联剂KBM510313‑17、正硅酸乙酯100‑110、丙烯酸六氟丁酯30‑37、偶氮二异丁腈0.1‑0.14、20‑25%的氨水5‑7、四氧化三铁4‑5、二氨基二苯醚0.1‑0.3、丙酸钙0.6‑1、1,2‑苯并异噻唑啉‑3‑酮0.2‑0.3、单油酸三乙醇胺酯0.7‑1。本发明可以形成各种不同形貌的杂化涂层表面,不同结构的涂层表面结合裸露在外的低表面能的乙烯基团,共同赋予了涂层具有超疏水特性。
Description
技术领域
本发明涉及金属防腐技术领域,尤其涉及一种复合钙质金属铜防腐涂层及其制备方法。
背景技术
近年来,随着人们环保意识的增强,传统的金属涂层保护或表面处理方法面临严峻挑战,如电镀虽可形成均勾、致密的保护层,但电镀过程会产生大量的废水、废气和废渣,其中含有重金属铬、氰酸盐等剧毒物质,给环境带来严重威胁;而金属表面的憐化处理技术,磷化工艺产生的沉渣及磷酸盐易造成水质的富氧化,亚硝酸盐、重金属离子对水质的污染等也需寻求新的表面处理方法。近年来,新的环境友好的表面涂层技术应运而生,如模仿生物体自修复功能原理的仿生自修复防腐涂层,自组装单分子膜技术,超疏水膜技术,值得一提的是,由于超疏水膜技术在防腐缓蚀、表面自清洁、抗霜冻、流动减阻及微流体无损输送、生物技术等领域表现出极大的应用价值而引起了人们的广泛关注,这一领域的研究非常活跃。超疏水膜技术是根据水滴可以在超疏水表面上自由滚动的现象-“荷叶效应”而提出的一种金属表面处理方法。在荷叶表面的微纳米结构及其表层錯质共同赋予了表面超疏水性能。超疏水表面微纳米结构可以提高静态接触角,使液滴难以渗入微纳米粗糙结构,造成金属与腐蚀性介质的物理隔离,达到防腐蚀的目的。基于超疏水膜技术的金属表面处理技术已被广泛应用于改善多种金属材料的耐腐蚀性能,也正是因为超疏水膜独特的自清洁和防腐蚀性能,成为一种非常有前景的金属表面防护方法;
影响固体表面浸润性的一个重要因素是表面自由能,当表面自由能降低时,疏水性能就会得到增加。然而,即使具有最低表面能的光滑固体表面与水的接触角也只有119°,因此,仅靠降低表面能是不能获得超疏水表面的。
已有的研究表明,构建超疏水表面主要通过两条途径,其一是在粗糖的基底表面修饰低表面能物质;其二是在疏水表面构建具有一定粗糖度的微纳米结构,根据这两条途径,科学家们发展了很多构建超疏水表面的方法,构建了不同表面结构的超疏水表面。
考虑到金属材料在环境中面临的腐蚀问题,且超疏水表面是非常有前景的金属表面防护方法之一;本发明的目的就是研究一种超疏水表面的金属防腐涂层。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种复合钙质金属铜防腐涂层及其制备方法。
本发明是通过以下技术方案实现的:
一种复合钙质金属铜防腐涂层,该涂层是由下述重量份的原料组成的:
二甲基丙烷羧酸酯0.4-1、烯丙基聚乙二醇3-4、棕榈酸钙1-2、乙烯基三甲氧基硅烷10-14、1.8-2g/l的柠檬酸溶液200-300、硅烷偶联剂KBM510313-17、正硅酸乙酯100-110、丙烯酸六氟丁酯30-37、偶氮二异丁腈0.1-0.14、20-25%的氨水5-7、四氧化三铁4-5、二氨基二苯醚0.1-0.3、丙酸钙0.6-1、1,2-苯并异噻唑啉-3-酮0.2-0.3、单油酸三乙醇胺酯0.7-1。
一种权利要求1所述的复合钙质金属铜防腐涂层的制备方法,包括以下步骤:
(1)将上述丙酸钙、四氧化三铁混合,球磨均匀,加入到1.8-2g/l的柠檬酸溶液中,超声分散1.7-2小时,抽滤,将滤饼用无水乙醇洗涤2-3次,在76-80℃下真空干燥10-20分钟,得酸修饰四氧化三铁;
(2)将上述棕榈酸钙、烯丙基聚乙二醇混合,在70-80℃下保温搅拌4-9分钟,加入上述硅烷偶联剂KBM5103重量的3-4%,搅拌至常温,得预混液;
(3)将上述二甲基丙烷羧酸酯加入到其重量17-20倍的无水乙醇中,搅拌条件下加入二氨基二苯醚,在50-60℃下保温搅拌20-30分钟,加入上述1,2-苯并异噻唑啉-3-酮,搅拌至常温,得醇分散液;
(4)将上述酸修饰四氧化三铁加入到其重量370-400倍的、30-35%的乙醇溶液中,超声20-30分钟,依次加入剩余的硅烷偶联剂KBM5103、正硅酸乙酯,700-1000转/分搅拌反应6-7小时,加入上述醇分散液,200-300转/分搅拌8-10分钟,抽滤,将滤饼用无水乙醇洗涤2-3次,在100-110℃下真空干燥20-25小时,得乙烯基封端复合材料;
(5)将上述乙烯基封端复合材料加入到其重量100-105倍的二甲基甲酰胺中,超声40-50分钟,通入氮气,加入上述丙烯酸六氟丁酯、偶氮二异丁腈,在70-80℃下反应5-7小时,加入上述预混液,搅拌均匀,冷却至室温,抽滤,将滤饼用二甲基甲酰胺洗3-4次,在80-90℃下真空干燥10-14小时,得氟化复合材料;
(6)将上述氟化复合材料加入到其重量15-17倍、95-97%的乙醇溶液中,超声分散10-20分钟,加入剩余各原料,搅拌均匀,放入清洗干净的铜片,浸泡20-26小时,取出,在60-65℃下干燥,即得所述涂层。
本发明的优点是:本发明首先采用柠檬酸修饰磁性Fe304纳米粒子,可以使其作为亲水相与硅烷偶联剂KBM5103共溶,然后通过硅烷偶联剂KBM5103和正硅酸乙酯的水解反应,在四氧化三铁表面引入乙烯基封端的硅氧烷,为接枝聚合反应提供乙烯基活性基团。丙烯酸六氟丁酯与乙烯基封端的四氧化三铁/硅氧烷复合粒子通过接枝聚合,在复合粒子表面形成含氟聚合物,然后将含氟聚合物复合粒子加入到硅烷醇液中,降低了涂层的表面能,提高涂层的疏水性能;该硅烷醇液以乙烯基三甲氧基硅烷为前驱体、氨水为催化剂,乙烯基三甲氧基硅烷先发生水解反应生成硅醇,然后在碱性条件下脱氢,对其他硅原子核发动亲核进攻,发生缩合反应形成Si-0-Si键,并伴随着脱水或脱醇,在铜基表面逐步聚集成核、生长,最终形成各种不同形貌的杂化涂层表面,不同结构的涂层表面结合裸露在外的低表面能的乙烯基团,共同赋予了涂层具有超疏水特性。本发明加入了丙酸钙、棕榈酸钙,可以有效的提高填料粒子在聚合物中的分散性,提高涂层的稳定性强度。
具体实施方式
一种复合钙质金属铜防腐涂层,该涂层是由下述重量份的原料组成的:
二甲基丙烷羧酸酯0.4、烯丙基聚乙二醇3、棕榈酸钙1、乙烯基三甲氧基硅烷10、1.8g/l的柠檬酸溶液200、硅烷偶联剂KBM510313、正硅酸乙酯100、丙烯酸六氟丁酯30、偶氮二异丁腈0.1、20%的氨水5、四氧化三铁4、二氨基二苯醚0.1、丙酸钙0.6、1,2苯并异噻唑啉酮0.2、单油酸三乙醇胺酯0.7。
一种权利要求1所述的复合钙质金属铜防腐涂层的制备方法,包括以下步骤:
(1)将上述丙酸钙、四氧化三铁混合,球磨均匀,加入到1.8g/l的柠檬酸溶液中,超声分散1.7小时,抽滤,将滤饼用无水乙醇洗涤2次,在76℃下真空干燥10分钟,得酸修饰四氧化三铁;
(2)将上述棕榈酸钙、烯丙基聚乙二醇混合,在70℃下保温搅拌4分钟,加入上述硅烷偶联剂KBM5103重量的3%,搅拌至常温,得预混液;
(3)将上述二甲基丙烷羧酸酯加入到其重量17倍的无水乙醇中,搅拌条件下加入二氨基二苯醚,在50℃下保温搅拌20分钟,加入上述1,2苯并异噻唑啉酮,搅拌至常温,得醇分散液;
(4)将上述酸修饰四氧化三铁加入到其重量370倍的、30%的乙醇溶液中,超声20分钟,依次加入剩余的硅烷偶联剂KBM5103、正硅酸乙酯,700转/分搅拌反应6小时,加入上述醇分散液,200转/分搅拌8分钟,抽滤,将滤饼用无水乙醇洗涤2次,在100℃下真空干燥20小时,得乙烯基封端复合材料;
(5)将上述乙烯基封端复合材料加入到其重量100倍的二甲基甲酰胺中,超声40分钟,通入氮气,加入上述丙烯酸六氟丁酯、偶氮二异丁腈,在70℃下反应5小时,加入上述预混液,搅拌均匀,冷却至室温,抽滤,将滤饼用二甲基甲酰胺洗3次,在80℃下真空干燥10小时,得氟化复合材料;
(6)将上述氟化复合材料加入到其重量15倍、95%的乙醇溶液中,超声分散10分钟,加入剩余各原料,搅拌均匀,放入清洗干净的铜片,浸泡20小时,取出,在60℃下干燥,即得所述涂层。
性能测试:
将本发明涂层处理的铜片在室内常温放置12个月以上, 仍具有超疏水特性;
清洗干净的铜片基材为亲水的(接触角小于90°),对水的静态接触角为85±1.1;本发明的涂层呈现为超疏水性,其接触角为154±1.5;
将不同pH的溶液滴在本发明的涂层表面,静置30分钟,再测量其接触角,在pH为2-12这个范围内,接触角都大于150°,说明强酸、强碱对超疏水表面结构及其化学成分几乎无影响,该复合颗粒形成的涂层具有很好的耐酸碱性能。
Claims (2)
1.一种复合钙质金属铜防腐涂层,其特征在于,该涂层是由下述重量份的原料组成的:
二甲基丙烷羧酸酯0.4-1、烯丙基聚乙二醇3-4、棕榈酸钙1-2、乙烯基三甲氧基硅烷10-14、1.8-2g/l的柠檬酸溶液200-300、硅烷偶联剂KBM510313-17、正硅酸乙酯100-110、丙烯酸六氟丁酯30-37、偶氮二异丁腈0.1-0.14、20-25%的氨水5-7、四氧化三铁4-5、二氨基二苯醚0.1-0.3、丙酸钙0.6-1、1,2-苯并异噻唑啉-3-酮0.2-0.3、单油酸三乙醇胺酯0.7-1。
2.一种权利要求1所述的复合钙质金属铜防腐涂层的制备方法,其特征在于,包括以下步骤:
(1)将上述丙酸钙、四氧化三铁混合,球磨均匀,加入到1.8-2g/l的柠檬酸溶液中,超声分散1.7-2小时,抽滤,将滤饼用无水乙醇洗涤2-3次,在76-80℃下真空干燥10-20分钟,得酸修饰四氧化三铁;
(2)将上述棕榈酸钙、烯丙基聚乙二醇混合,在70-80℃下保温搅拌4-9分钟,加入上述硅烷偶联剂KBM5103重量的3-4%,搅拌至常温,得预混液;
(3)将上述二甲基丙烷羧酸酯加入到其重量17-20倍的无水乙醇中,搅拌条件下加入二氨基二苯醚,在50-60℃下保温搅拌20-30分钟,加入上述1,2-苯并异噻唑啉-3-酮,搅拌至常温,得醇分散液;
(4)将上述酸修饰四氧化三铁加入到其重量370-400倍的、30-35%的乙醇溶液中,超声20-30分钟,依次加入剩余的硅烷偶联剂KBM5103、正硅酸乙酯,700-1000转/分搅拌反应6-7小时,加入上述醇分散液,200-300转/分搅拌8-10分钟,抽滤,将滤饼用无水乙醇洗涤2-3次,在100-110℃下真空干燥20-25小时,得乙烯基封端复合材料;
(5)将上述乙烯基封端复合材料加入到其重量100-105倍的二甲基甲酰胺中,超声40-50分钟,通入氮气,加入上述丙烯酸六氟丁酯、偶氮二异丁腈,在70-80℃下反应5-7小时,加入上述预混液,搅拌均匀,冷却至室温,抽滤,将滤饼用二甲基甲酰胺洗3-4次,在80-90℃下真空干燥10-14小时,得氟化复合材料;
(6)将上述氟化复合材料加入到其重量15-17倍、95-97%的乙醇溶液中,超声分散10-20分钟,加入剩余各原料,搅拌均匀,放入清洗干净的铜片,浸泡20-26小时,取出,在60-65℃下干燥,即得所述涂层。
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