CN109134359B - 一种2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法 - Google Patents

一种2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法 Download PDF

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CN109134359B
CN109134359B CN201811035907.6A CN201811035907A CN109134359B CN 109134359 B CN109134359 B CN 109134359B CN 201811035907 A CN201811035907 A CN 201811035907A CN 109134359 B CN109134359 B CN 109134359B
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刘峥
韩佳星
梁楚欣
李汝
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Shaanxi Ruiyi Longke Environmental Protection Technology Co.,Ltd.
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Abstract

本发明公开了一种2,6‑二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法。(1)将1.1106 g乙醛酸置于盛有15mL无水乙醇的圆底烧瓶中。（2）将0.5456 g的2,6‑二氨基吡啶加入20mL无水乙醇中，溶解，加入到步骤（1）所得物中。(3)滴加0.15mL冰醋酸，70℃搅拌，反应6小时，氮气保护。（4）室温下冷却，得到褐色沉淀，减压抽滤，用无水乙醇淋洗，滤饼真空干燥，再放入装有40mL无水乙醇的烧杯中，搅拌，减压抽滤，滤饼真空干燥，得2,6‑二氨基吡啶缩乙醛酸双席夫碱缓蚀剂。缓蚀剂能应用于酸洗液中对碳钢的防腐蚀。本发明工艺简单、重复性好、产率高，缓蚀剂对稀硫酸中碳钢的缓蚀效果良好。

Description

一种2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法
技术领域
本发明涉及有机合成领域，涉及一种含双席夫碱缓蚀剂的制备方法，具体涉及一种2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法。
背景技术
碳钢是指碳含量低于2％，并有少量硅、锰以及磷、硫等杂质的铁碳合金[1]。它广泛用于机械制造各个方面，特别是自18世纪的工业革命以来，全球对碳钢作为各种产品和结构(包括建筑物，车辆，电子设备，管道和家用电器等)的原材料的需求不断增加。在日常运输、热轧、表面处理、作业和储存中不可避免地形成锈蚀层，同时钢铁工业中的轧钢等需要酸洗去除钢铁表面的氧化铁皮和其它污物，酸洗过程对酸洗终点无法确定，所以容易造成″过酸洗″现象。缓蚀剂是一种防腐蚀化学品，它少量加入环境介质中就能显著地降低金属的腐蚀速率。与其它防腐蚀方法相比，缓蚀剂具有使用方便、经济有效的特点，广泛地应用于工业生产和社会生活中。近年来世界各国都十分关注缓蚀剂的研究开发和应用，在我国不断深入研究开发绿色环保型缓蚀剂产品及其应用技术，减少因腐蚀造成的资源浪费和环境污染，对推进″资源节约型、环境友好型″社会建设，具有十分重要的意义。
目前，金属的腐蚀防护方法有：隔离法、缓蚀剂法和电化学保护法。其中，缓蚀剂在使用过程中无须专门设备，无须改变金属构件的性质，并且具有成本低、适应性强等优点，同时在腐蚀环境中加入少量缓蚀剂就能和金属表面发生物理作用和化学作用，从而显著降低金属材料的腐蚀。因此，深入研究开发高效、绿色环保的缓蚀剂，对推动缓蚀剂在各领域中应用，丰富缓蚀剂技术具有重要的意义。
本发明公开了2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法。所述方法是以2，6-二氨基吡啶和乙醛酸为原料，以冰醋酸为催化剂，即可制备2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂。
发明内容
本发明的目的是提供一种2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法。
具体步骤为：
(1)量取1.1106g乙醛酸置于盛有15mL无水乙醇的圆底烧瓶中，磁力搅拌均匀。
(2)将0.5456g的2，6-二氨基吡啶加入20mL无水乙醇中，用超声波震荡溶解完全，缓慢加入到步骤(1)所得物中充分混合。
(3)再向步骤(2)所得物中滴加0.15mL分析纯冰醋酸催化剂，70℃恒温条件下，磁力搅拌，回流反应6小时，全程氮气保护。
(4)将步骤(3)所得的溶液室温下冷却，得到褐色沉淀，减压抽滤，用无水乙醇不断淋洗，取出滤饼，将滤饼进行真空干燥，再放入装有40mL无水乙醇的烧杯中，用磁力搅拌2小时，以除去过量的乙醛酸、冰醋酸等杂质，再减压抽滤，取滤饼真空干燥，最后得2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂。
所述2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂能应用于酸洗液中对碳钢的防腐蚀，2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的用量为0.001-0.01mol/L。
本发明具有工艺简单、重复性好、产率高等优点。2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂应用于酸洗液中，对碳钢的缓蚀，效果良好。
附图说明
图1为本发明实施例中2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂红外光谱图。
图2为本发明实施例中2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的质谱图。
具体实施方式
下面结合具体实施例进一步阐明本发明，但实施例并不限制本发明的保护范围。
实施例：
制备上述2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的具体步骤为：
(1)量取1.1106g乙醛酸置于盛有15mL无水乙醇的圆底烧瓶中，磁力搅拌均匀。
(2)将0.5456g的2，6-二氨基吡啶加入20mL无水乙醇中，用超声波震荡溶解完全，缓慢加入到步骤(1)所得物中充分混合。
(3)向步骤(2)所得物中滴加0.15mL分析纯冰醋酸催化剂，70℃恒温条件下，磁力搅拌，回流反应6小时，全程氮气保护。
(4)将步骤(3)所得的溶液室温下冷却，得到褐色沉淀，减压抽滤，用无水乙醇不断淋洗，取出滤饼，将滤饼进行真空干燥，再放入装有40mL无水乙醇的烧杯中，用磁力搅拌2小时，以除去过量的乙醛酸、冰醋酸等杂质，再减压抽滤，取滤饼真空干燥，最后得0.9367g 2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂，收率85.46％。
反应式如下：
Figure BDA0001790869880000031
利用VECTOR22型红外光谱仪，采用KBr压片，对所制备的2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂在4000～500cm-1范围内扫描，进行红外光谱结构表征。由附图1可知，在3384cm-1附近没有出现-NH2的伸缩振动峰，在1749cm-1 附近没有发现醛基(-COH)伸缩振动峰，而出现新的化学键C＝N特征吸收峰，说明有席夫碱的生成。
利用美国布鲁克道尔顿公司APEX IV型傅立叶变换高分辩质谱仪在ESI+ 模式，150V电压下得到2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的质谱图。由附图1可知：[M+H]+m/z 225.07处的分子离子峰与被测物质的相对分子质量 221.21相吻合；在m/z 247.11处的分子离子峰是被测物质经裂分失去羟基后与 K+离子结合形成的，而K的相对分子质量是39.1，修正4.5ppm实验误差，则被测物质的相对分子质量为220.61，同样与理论被测物质的相对分子质量221.21 基本一致。
采用失重法考察取2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂缓蚀效果。干燥备用的3组实验碳钢试样在分析天平上准确称量，将处理过的低碳钢片浸泡在不添加和添加不同浓度分别为0.001mol/L，0.005mol/L，0.01mol/L2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的50mL 1mol/L稀硫酸中，30℃下浸泡4小时。然后取出样品，用蒸馏水冲洗，乙醇中脱水，丙酮中脱脂，干燥4小时后称重。平行试验三次，计算缓蚀率。0.001mol/L，0.005mol/L，0.01mol/L2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂对稀硫酸中碳钢的缓蚀率分别为90.28％、95.11％、 96.96％。2，6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的缓蚀性能较好的原因与其结构中含有多个电负性较大的配位氮原子有关，配位点较多，会产生有多个吸附点，同时分子结构中共轭体系较大，能够在碳钢表面形成致密的覆盖层，减少腐蚀。

Claims (1)

1.一种2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的制备方法，其特征在于具体步骤为：
(1)量取1.1106 g 乙醛酸置于盛有15mL无水乙醇的圆底烧瓶中，磁力搅拌均匀；
（2）将0.5456 g 的2,6-二氨基吡啶加入20mL无水乙醇中，用超声波震荡溶解完全，缓慢加入到步骤（1）所得物中混合；
(3) 向步骤（2）所得物中滴加0.15mL分析纯冰醋酸催化剂，70℃恒温条件下，磁力搅拌，回流反应6小时，全程氮气保护；
（4）将步骤（3）所得的溶液室温下冷却，得到褐色沉淀，减压抽滤，用无水乙醇淋洗，取出滤饼，将滤饼进行真空干燥，再放入装有40mL无水乙醇的烧杯中，用磁力搅拌2小时，再减压抽滤，取滤饼真空干燥，得2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂；
所述2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂能应用于酸洗液中对碳钢的防腐蚀，2,6-二氨基吡啶缩乙醛酸双席夫碱缓蚀剂的用量为0.001-0.01 mol/L。
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