CN110305554A - 一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法 - Google Patents
一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法,以丙烯酰胺为单体、偶氮二异丁腈为引发剂、氧化镍纳米粒子为掺杂剂、丙烯海松酸(乙二胺)酰胺为交联剂,通过热聚合方法制备了一种高点蚀电位的氧化亚钴纳米粒子掺杂的松香基热聚合防腐膜,该膜层具有较高的点蚀电位,耐点腐蚀性能良好、简单实用,克服了以往防腐膜层腐蚀电位低的缺点。该膜层可应用于空调、电热水器、空调、冰箱等电气设备及拖拉机、起重机等机械设备的金属零部件的防腐工程。
Description
技术领域
本发明涉及防腐蚀涂膜领域,尤其是涉及一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法。
背景技术
由于空调、电热水器、空调、冰箱等电气设备及拖拉机、起重机等机械设备的金属零部件,由于材料点蚀电位(Pitting corrosion potential)较低,极易受到周围环境的腐蚀,特别是金属零部件长期处于在潮湿、腐蚀介质的环境中极易引起点蚀、起粉、起泡等现象。目前处理的方法是在高分子涂层中添加大量的六价铬盐或四氧化三铅等重金属化合物,然而这类防腐涂层不断地有这些重金属铅等离子析出,严重污染海洋、河流及土壤环境,给全球生态环境及人体造成严重影响。但是由于目前没有适合的替代技术,因此,寻找适合的替代技术具有重要意义。
聚丙烯酰胺由于存在氨基、羰基,可以形成很多氢键, 所以聚丙烯酰胺涂层具有较好的耐腐蚀性、抗渗透性、耐磨性以及较好的附着力等特性, 广泛在用于空调、电热水器、空调、冰箱等电气设备及拖拉机、起重机等机械设备的金属零部件防腐,但聚丙烯酰胺涂层性能单一,这样制备的涂层点蚀电位较低,如果涂层长期处于潮湿、腐蚀介质中会引起点蚀、起泡、起粉等现象,防腐性能不佳,满足不了实际恶劣环境的需要。
发明内容
本发明要解决的技术问题是提供一种设备简单、制造容易一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法。
为解决上述技术问题,本发明采用如下技术方案:为解决上述技术问题,本发明采用如下技术方案:以丙烯酰胺为单体、偶氮二异丁腈为引发剂、氧化镍纳米粒子为掺杂剂、丙烯海松酸(乙二胺)酰胺为交联剂制备。
上述一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法,以丙烯酰胺为单体、偶氮二异丁腈为引发剂、氧化镍纳米粒子为掺杂剂、丙烯海松酸(乙二胺)酰胺为交联剂,混匀后,将金属部件浸入其混合溶液中10分钟,再取出部件加热聚合即得。
上述一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法,包括以下过程:
<1>0.012克氯化镍、1克丙三醇、100克蒸馏水加入到烧杯中,搅拌10分钟,待氯化镍溶解后,慢慢滴入浓度为0.01克/氢氧化钠10毫升并剧烈搅拌30分钟,然后转入200毫升的内衬聚四氟乙烯的不锈钢的高压反应釜中,在摄氏温度160的条件下反应1小时,然后离心收集沉淀,并用去离子水及乙醇洗涤三次,并在摄氏温度280的条件下烘干1小时即得氧化镍纳米粒子;
<2> 向1 L溶剂乙醇中,依次加入0.0 1 mol~0.50 mol的单体丙烯酰胺、0. 001 mol~0.01 mol的引发剂偶氮二异丁腈、步骤<1>制备的0.001 mol ~0.009 mol氧化镍纳米粒子为掺杂剂、0.01mol ~0.50 mol的交联剂丙烯海松酸(乙二胺)酰胺,每加入一种化学试剂超声波溶解2分钟;
<3> 将干净光滑的金属部件浸入步骤<2>的混合物中10分钟,再取出部件置于85 ℃的真空干燥箱内热聚合 1.5小时即得。
实验发现,以丙烯酰胺为单体、偶氮二异丁腈为引发剂、氧化镍纳米粒子为掺杂剂、丙烯海松酸(乙二胺)酰胺为交联剂,混匀后,将6063铝合金片浸入其中10分钟,再取出铝合金片加热聚合即得。采用电化学工作上测试,裸露面积为1 平方厘米,点蚀电位提高近80 mV;另外,将浸有该热聚合膜的6063铝合金片,在3.5% 的氯化钠溶液中浸泡100小时时没点蚀,也不起泡、不起粉。因此,制备的松香基与丙烯酰胺热聚合防腐膜具有较高的抗点蚀性能,而且其它防腐性能也较优良,超过目前的丙烯酰胺热聚合防腐膜,并且设备简单、制作容易。
附图说明
图1是实施例1中制备的氧化镍纳米粒子扫描电镜图;
图2是实施例1中一种高点蚀电位的含丙烯海松酸(乙二胺)酰胺及氧化镍纳米粒子的聚合防腐膜与不含丙烯海松酸(乙二胺)酰胺及氧化镍纳米粒子的聚合防腐膜的极化曲线图。
具体实施方式
实施例1
一、6063铝合金片的处理
将6063铝合金片在抛光布上依次用1.0 μm、0.3 μm的氧化铝粉抛光,然后放入5%的盐酸中超声5 min,再放入去离子水中超声清洗5 min,最后放入无水乙醇中超声6 min后烘干备用。
二、防腐蚀膜的制备
<1> 0.012克氯化镍、1克丙三醇、100克蒸馏水加入到烧杯中,搅拌10分钟,待氯化镍溶解后,慢慢滴入浓度为0.01克/氢氧化钠10毫升并剧烈搅拌30分钟,然后转入200毫升的内衬聚四氟乙烯的不锈钢的高压反应釜中,在摄氏温度160的条件下反应1小时,然后离心收集沉淀,并用去离子水及乙醇洗涤三次,并在摄氏温度280的条件下烘干1小时即得氧化亚镍纳米粒子;
<2> 向1 L溶剂乙醇中,依次加入0.20 mol的单体丙烯酰胺、0. 005 mol mol的引发剂偶氮二异丁腈、步骤<1>制备的0.005 mol氧化镍纳米粒子为掺杂剂、0.20 mol的交联剂丙烯海松酸(乙二胺)酰胺,每加入一种化学试剂超声波溶解2分钟;将干净光滑的金属部件浸入混合物中10分钟,再取出部件置于85℃的真空干燥箱内热聚合 1.5小时即得松香基氧化镍纳米粒子掺杂白丙烯海松酸(乙二胺)酰胺与丙烯酰胺热聚合防腐膜;
<3> 丙烯酰胺的热聚合防腐膜制备过程除了不加丙烯海松酸(乙二胺)酰胺及掺杂剂氧化镍纳米粒子外,其它过程与步骤<2>完全相同,即得丙烯酰胺的热聚合防腐膜。
<4> 含掺杂剂氧化镍纳米粒子的丙烯酰胺热聚合防腐膜制备过程除了不加丙烯海松酸(乙二胺)酰胺外,其它过程与步骤<2>完全相同,即得含氧化镍纳米粒子的丙烯酰胺热聚合防腐膜。
三、防腐蚀性能测试
<1> 将制备的3块涂有丙烯酰胺的热聚合防腐膜、含氧化镍纳米粒子的丙烯酰胺热聚合防腐膜及含松香基丙烯海松酸(乙二胺)酰胺及与氧化镍纳米粒子的丙烯酰胺热聚合防腐膜的6063铝合金片,使涂膜的裸露面积为1 平方厘米,然后在3.5% 的氯化钠溶液中进行电化学极化曲线测试,比较腐蚀电流及点蚀电位,发现加了氧化镍纳米粒子的丙烯酰胺热聚合防腐膜的腐蚀电流显著降低了,含松香基丙烯海松酸(乙二胺)酰胺及与氧化镍纳米粒子的热聚合防腐膜,不但腐蚀电流显著降低了,点蚀电位提高近80 mV。
<2> 将制备的3块涂有丙烯酰胺的热聚合防腐膜、含氧化镍纳米粒子的丙烯酰胺热聚合防腐膜及含松香基丙烯海松酸(乙二胺)酰胺及与氧化镍纳米粒子的丙烯酰胺热聚合防腐膜的6063铝合金片,浸泡于3.5% 的氯化钠溶液中,浸泡100小时,含松香基丙烯海松酸(乙二胺)酰胺及与氧化镍纳米粒子的热聚合防腐膜的6063铝合金片,无点蚀、无起泡、无开裂、无脱落现象;含氧化镍纳米粒子的防腐磁漆有点蚀,但无起粉、无起泡等现象;但不含丙烯海松酸(乙二胺)酰胺及氧化镍纳米粒子的丙烯酰胺发生严重的点蚀、起泡、开裂、脱落现象。
因此,本发明制备的丙烯海松酸(乙二胺)酰胺及氧化镍纳米粒子的聚合防腐膜具有较高的防点蚀性能及其它防腐蚀性能。
Claims (1)
1.一种高点蚀电位的氧化镍纳米粒子掺杂的松香基热聚合防腐膜的制备方法,其特征在于以0.0 1 mol/L~0.50 mol/L的丙烯酰胺为单体、0. 001 mol /L~0.01 mol/mL的偶氮二异丁腈为引发剂、0.001 mol/L ~0.009 mol/L的氧化镍纳米粒子为掺杂剂、0. 01mol/L~0.50 mol/L丙烯海松酸(乙二胺)酰胺为交联剂,混匀后,将金属部件浸入其混合溶液中10分钟,再取出部件加热聚合,即得;
具体按以下操作进行:
<1> 0.012克氯化镍、1克丙三醇、100克蒸馏水加入到烧杯中,搅拌10分钟,待氯化镍溶解后,慢慢滴入浓度为0.01克/氢氧化钠10毫升并剧烈搅拌30分钟,然后转入200毫升的内衬聚四氟乙烯的不锈钢的高压反应釜中,在摄氏温度160的条件下反应1小时,然后离心收集沉淀,并用去离子水及乙醇洗涤三次,并在摄氏温度280的条件下烘干1小时即得氧化镍纳米粒子;
<2> 向1 L溶剂乙醇中,依次加入0.0 1 mol~0.50 mol的单体丙烯酰胺、0. 001 mol~0.01 mol的引发剂偶氮二异丁腈、步骤<1>制备的0.001 mol ~0.009 mol氧化亚镍纳米粒子为掺杂剂、0. 01mol ~0.50 mol的交联剂丙烯海松酸(乙二胺)酰胺,每加入一种化学试剂超声波溶解2分钟;
<3> 将干净光滑的金属部件浸入步骤<2>的混合物中10分钟,再取出部件置于85 ℃的真空干燥箱内热聚合 1.5小时即得。
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JPH01161078A (ja) * | 1987-12-18 | 1989-06-23 | Toagosei Chem Ind Co Ltd | エマルジョン型粘着剤の製造方法 |
CN101417823A (zh) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | 无需模板的氧化镍空心微球的湿化学制备方法 |
CN107880280A (zh) * | 2017-11-14 | 2018-04-06 | 南京林业大学 | 一种松香基多活性位点丙烯酰胺复合水凝胶的制备方法 |
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JPH01161078A (ja) * | 1987-12-18 | 1989-06-23 | Toagosei Chem Ind Co Ltd | エマルジョン型粘着剤の製造方法 |
CN101417823A (zh) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | 无需模板的氧化镍空心微球的湿化学制备方法 |
CN107880280A (zh) * | 2017-11-14 | 2018-04-06 | 南京林业大学 | 一种松香基多活性位点丙烯酰胺复合水凝胶的制备方法 |
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