CN108794407B - 一种阳离子型抗氧缓蚀剂及其制备方法 - Google Patents
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Abstract
Description
技术领域
本发明属于材料技术领域,尤其涉及一种阳离子型抗氧缓蚀剂及其制备方法。
背景技术
目前,我国大部分油田都处在油气田开发的中后期,原油的含水量逐步增加,采出水的矿化度不断提高,此外,注气开采中夹杂的O2与回注的采出水结合后具有强腐蚀性,对井筒的腐蚀异常严重,这也是油气田要解决的重要技术问题之一。据统计,全世界每年因腐蚀报废的钢铁设备约相当于年产量的1/3,给国民收入带来了严重的影响。而使用缓蚀剂防腐具有投资少、见效快、方便易行等优点,是近年来解决此类问题的一种很有效的方法,越来越受到企业的关注。
发明内容
本发明的目的在于提供一种新的阳离子型抗氧缓蚀剂及其制备方法。
一种阳离子型抗氧缓蚀剂,其结构式为:
结构式中R可以为CnH2n+1、CnH2n-1型脂肪烃链、苯基、甲氧基苯基、苯乙烯基、甲氧基苯乙烯基、苯丙烯基、甲氧基苯丙烯基中的一种或几种,其中n=6~22。
一种阳离子型抗氧缓蚀剂的制备方法,包括以下步骤:
步骤1:利用3-二甲氨基丙胺与酰氯进行酰胺化反应,得到酰胺中间体A;
步骤2:利用酰胺中间体A与4-氯甲基嘧啶加热回流反应,最终制备得到缓蚀剂。
进一步地,如上所述的方法,所述步骤1包括:将3-二甲氨基丙胺与酰氯混合后反应30min,室温下继续反应24h,得到粗产品,将所述粗产品纯化、干燥最终得到酰胺中间体A。
进一步地,如上所述的方法,所述纯化、干燥的步骤包括:将粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到酰胺中间体A。
进一步地,如上所述的方法,所述步骤2包括:将酰胺中间体A和4-氯甲基嘧啶混合,85℃加热回流反应12h,减压旋蒸除掉溶剂乙醇,得到所述缓蚀剂。
有益效果:
本发明制备的阳离子缓蚀剂其分子中引入了嘧啶杂环,增强了缓蚀剂与金属基体的化学吸附,同时保留了嘧啶环上的两个未成键的N原子,N原子的上的未成键的孤对电子可以与Fe原子形成更好的吸附;长链疏水基团可以在金属表面形成定向排列的疏水层,有效抑制腐蚀过程中的阴极腐蚀;酰胺基团中的O和N原子也能在金属表面形成吸附位点。本发明制备的阳离子缓蚀剂环境友好、制备简单,该缓蚀剂在80℃、持续饱和氧气的高矿化度地层水对P110、P110S、N80钢有很好的缓蚀作用。适用范围广,既可以应用与高矿化度地层水的氧气腐蚀防护,也适用于酸性条件下的碳钢腐蚀防护。
附图说明
图1为本发明制备的阳离子缓蚀剂其溶解分散效果图;
图2为本发明制备的阳离子缓蚀剂产品红外图谱。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面本发明中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
将0.22mol3-二甲氨基丙胺、0.2mol三乙胺加入到250mL三颈烧瓶中,同时加入适量的CH2Cl2做溶剂,将0.2mol的软脂酰氯溶于无水***中,于冰水浴下缓慢滴加到圆底烧瓶中,滴加结束后继续反应30min,室温下继续反应24h,粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到中间体硬脂酰胺丙基二甲胺。0.2mol中间体软脂酰胺丙基二甲胺溶于适量乙醇后加入到250mL圆底烧瓶中,加入0.2mol的4-氯甲基嘧啶,85℃加热回流反应12h,减压旋蒸除掉乙醇,得到软脂酰胺基阳离子缓蚀剂a。
实施例2:
将0.22mol3-二甲氨基丙胺、0.2mol三乙胺加入到250mL三颈烧瓶中,同时加入适量的CH2Cl2做溶剂,将0.2mol的邻甲氧基苯甲酰氯溶于无水***中,于冰水浴下缓慢滴加到圆底烧瓶中,滴加结束后继续反应30min,室温下继续反应24h,粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到中间体邻甲氧基苯甲酰胺丙基二甲胺。0.2mol中间体邻甲氧基苯甲酰胺丙基二甲胺溶于适量乙醇后加入到250mL圆底烧瓶中,加入0.2mol的4-氯甲基嘧啶,85℃加热回流反应12h,减压旋蒸除掉乙醇,得到邻甲氧基苯甲酰胺基阳离子缓蚀剂b。
实施例3:
将0.22mol3-二甲氨基丙胺、0.2mol三乙胺加入到250mL三颈烧瓶中,同时加入适量的CH2Cl2做溶剂,将0.2mol的肉桂酰氯溶于无水***中,于冰水浴下缓慢滴加到圆底烧瓶中,滴加结束后继续反应30min,室温下继续反应24h,粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到中间体对肉桂酰胺丙基二甲胺。0.2mol中间体肉桂酰胺丙基二甲胺溶于适量乙醇后加入到250mL圆底烧瓶中,加入0.2mol的4-氯甲基嘧啶,85℃加热回流反应12h,减压旋蒸除掉乙醇,得到肉桂酰胺基阳离子缓蚀剂c。
实施例4:
将0.22mol3-二甲氨基丙胺、0.2mol三乙胺加入到250mL三颈烧瓶中,同时加入适量的CH2Cl2做溶剂,将0.2mol的对甲氧基肉桂酰氯溶于无水***中,于冰水浴下缓慢滴加到圆底烧瓶中,滴加结束后继续反应30min,室温下继续反应24h,粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到中间体对甲氧基肉桂酰胺丙基二甲胺。0.2mol中间体对甲氧基肉桂酰胺丙基二甲胺溶于适量乙醇后加入到250mL圆底烧瓶中,加入0.2mol的4-氯甲基嘧啶,85℃加热回流反应12h,减压旋蒸除掉乙醇,得到对甲氧基肉桂酰胺基阳离子缓蚀剂d。
实施例5:缓蚀剂性能评价。
实施例6:在80℃,220000mg/L矿化度(其中Ca2+浓度为11272mg/L,Mg2+浓度为1161.84mg/L)的持续饱和氧气的地层水中用P110钢片进行72h腐蚀挂片实验,缓蚀剂使用浓度为300mg/L。对实施例1-4的合成缓蚀剂进行静态挂片腐蚀,结果如下:
缓蚀剂 | a | b | c | d |
缓蚀效率(%) | 95.2 | 93.7 | 96.4 | 97.5 |
实施例7:
在80℃,220000mg/L矿化度(其中Ca2+浓度为11272mg/L,Mg2+浓度为1161.84mg/L)的持续饱和氧气的地层水中用P110S钢片进行72h腐蚀挂片实验,缓蚀剂使用浓度为300mg/L。对实施例1-4的合成缓蚀剂进行静态挂片腐蚀,结果如下:
缓蚀剂 | a | b | c | d |
缓蚀效率(%) | 91.8 | 93.7 | 94.9 | 96.6 |
实施例8:
在80℃,220000mg/L矿化度(其中Ca2+浓度为11272mg/L,Mg2+浓度为1161.84mg/L)的持续饱和氧气的地层水中用N80钢片进行72h腐蚀挂片实验,缓蚀剂使用浓度为300mg/L。对实施例1-4的合成缓蚀剂进行静态挂片腐蚀,结果如下:
缓蚀剂 | a | b | c | d |
缓蚀效率(%) | 96.8 | 97.1 | 95.9 | 97.8 |
从上述实施案例能看出,以上缓蚀剂在使用量很低的情况下能表现出良好的减缓腐蚀的效果。
本发明提供的缓蚀剂在高矿化度地层水中拥有良好的溶解性和分散性,其溶解分散效果见图1。在高温下仍具有良好的缓蚀性能,对碳钢在高矿化度地层水中的氧腐蚀有明显抑制作用,120℃,缓蚀剂浓度为1000ppm时缓蚀率85%。
本发明的新型阳离子缓蚀剂为深红色固体,水溶性好。该缓蚀剂在80℃、持续饱和氧气的高矿化度地层水对P110、P110S、N80钢有很好的缓蚀作用。
制备工艺简单,产品纯度高,产品红外图谱见图2。3415cm-1和1633cm-1处分别为仲酰胺N-H和C=O伸缩振动吸收峰,2928cm-1和2847cm-1处分别为C-H的对称与反对称振动,1547cm-1处为N-H弯曲振动吸收,1465cm-1处为嘧啶环骨架的弯曲振动,1396cm-1处为与氮正离子相连的-CH2弯曲振动特征吸收峰,说明原料中叔胺N原子季铵化;
该缓蚀剂在低用量下仍具有良好的缓蚀性能,120℃、缓蚀剂浓度为500ppm时,碳钢在高矿化度地层水中氧腐蚀缓蚀率扔可达80%。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (2)
2.根据权利要求1所述的一种阳离子型抗氧缓蚀剂的制备方法,其特征在于,包括以下步骤:
步骤1:利用3-二甲氨基丙胺与酰氯进行酰胺化反应,得到酰胺中间体A;
步骤2:利用酰胺中间体A与4-氯甲基嘧啶加热回流反应,最终制备得到缓蚀剂;
所述步骤1包括:将3-二甲氨基丙胺与酰氯混合后反应30min,室温下继续反应24h,得到粗产品,将粗产品用饱和氯化钠溶液洗涤,再用二次去离子水洗涤,有机相用无水Na2SO4干燥过夜,过滤后将滤液减压旋蒸得到酰胺中间体A;
所述步骤2包括:将酰胺中间体A和4-氯甲基嘧啶混合,85℃加热回流反应12h,减压旋蒸除掉溶剂乙醇,得到所述缓蚀剂。
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