CN113292447A - 一种双缩合席夫碱酸化缓蚀剂、制备方法及其应用 - Google Patents
一种双缩合席夫碱酸化缓蚀剂、制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种双缩合席夫碱酸化缓蚀剂、制备方法及其应用,属于油气田开采化学防腐应用技术领域,该制备方法包括:在合成装置中,添加无水乙醇和肉桂醛溶液,充分搅拌后,对其进行加热,加热至回流温度后,向该合成装置中滴加二乙烯三胺溶液,回流反应;待反应结束后,将所得产物放入冰水浴中进行冷却,待固体析出后用乙醇洗涤,并用乙醇和氯仿重结晶,干燥后即得。本发明制备得到的肉桂醛缩二乙烯三胺双席夫碱缓蚀剂分子的共辄程度高,能形成大兀键以平面构型吸附于金属表面上,附着力强,使缓蚀率大为提高,且席夫碱合成容易,原料价格低,生产规模大,成本和毒性比其他缓蚀剂低,可作为碳钢缓蚀剂,具有良好的缓蚀效果。
Description
技术领域
本发明属于油气田开采化学防腐应用技术领域,具体涉及一种双缩合席夫碱酸化缓蚀剂、制备方法及其应用。
背景技术
添加缓蚀剂是控制腐蚀的常用且经济有效的手段。其主要用途之一是用于金属酸洗的酸洗槽。盐酸和硫酸是酸洗过程中最常用的酸,酸洗过程伴随着金属的显著溶解,并且腐蚀过程是不可精确检测的,会导致许多腐蚀问题的发生。因此,在这一过程中使用适当有效的缓蚀剂是防止腐蚀发生的重要手段。不同种类的缓蚀剂都可以减缓金属在酸性环境中的溶解,有机抑制剂大多含有杂原子、不饱和键中的电子以及芳香环,能够与没有任何氧化层金属表面成键,对金属起到较好的保护作用,应用也是最广泛的。
席夫碱是一种有机缓蚀剂,对在盐酸和硫酸环境中低碳钢,不锈钢,铜,铝和青铜都能起到有效地保护作用。席夫碱的特殊官能团是-C=N。席夫碱结构中含杂原子的杂环和电子的存在使这些化合物的自发吸附,并在钢基底上形成保护和粘合层。与伯胺和醛相比,由于甲亚胺基团的存在,席夫碱的腐蚀效率更高。并且席夫碱合成容易,原料价格低,生产规模大,成本和毒性比其他缓蚀剂低。由于芳香环上的-OH和CH3的存在,使得它们具有更大的给电子特性。此外大多数有机缓蚀剂的商业应用主要受限于它们对环境和人类的毒性,而席夫碱缓蚀剂又较为低毒环保。在此基础上发展的双席夫碱缓蚀剂由于具有更多的活性位点以及更大的共轭体系,有望对金属基体起到更好的保护效果。因此,探究双席夫碱类缓蚀剂作为酸化环境用缓蚀剂,以及揭示缓蚀剂的作用效果与分子结构之间的关系具有更有意义的研究价值。
发明内容
本发明的目的之一在于提供一种双缩合席夫碱酸化缓蚀剂的制备方法,其以肉桂醛和二乙烯三胺为原料,制备得到的肉桂醛缩二乙烯三胺双席夫碱缓蚀剂分子的共辄程度高,能形成大兀键以平面构型吸附于金属表面上,附着力强,使缓蚀率大为提高。
为了实现上述目的,本发明采用了以下技术方案:
一种双缩合席夫碱酸化缓蚀剂的制备方法,依次包括以下步骤:
a、在合成装置中,添加无水乙醇和肉桂醛溶液,充分搅拌后,对其进行加热,加热至回流温度后,向该合成装置中滴加二乙烯三胺溶液,回流反应;
b、反应结束后,将所得产物放入冰水浴中进行冷却,待固体析出后用乙醇洗涤,并用乙醇氯仿重结晶,干燥后即得。
上述技术方案直接带来的有益技术效果为:
通过选用肉桂醛和二乙烯三胺作为原料来制备双缩合席夫碱酸化缓蚀剂,其原料价格低,而且缓蚀率也得到了提高。
作为本发明的一个优选方案,步骤a中,无水乙醇的体积为30~50mL。
作为本发明的另一个优选方案,肉桂醛和二乙烯三胺的摩尔比为2:1。
进一步优选,步骤a中,用油浴锅进行加热,加热至温度为70~90℃,回流反应4~6h。
进一步优选,步骤b中,乙醇和氯仿的体积比为3:1。
本发明的另一目的在于提供上述的一种双缩合席夫碱酸化缓蚀剂的制备方法制备得到的双缩合席夫碱酸化缓蚀剂。
本发明的再一目的在于提供上述的双缩合席夫碱酸化缓蚀剂在油气田开采化学防腐中的应用。
与现有技术相比,本发明带来了以下有益技术效果:
本发明提供了一种双缩合席夫碱酸化缓蚀剂的制备方法,制备得到的肉桂醛缩二乙烯三胺双席夫碱缓蚀剂分子的共辄程度高,能形成大兀键以平面构型吸附于金属表面上,附着力强,使缓蚀率大为提高,且席夫碱合成容易,原料价格低,生产规模大,成本和毒性比其他缓蚀剂低。可作为碳钢缓蚀剂,具有良好的缓蚀效果。
本发明提供的双缩合席夫碱酸化缓蚀剂能对金属基体起到更好的保护作用。
附图说明
下面结合附图对本发明做进一步说明:
图1为本发明肉桂醛缩二乙烯三胺缓蚀剂的1H NMR谱图。
具体实施方式
本发明提出了一种双缩合席夫碱酸化缓蚀剂、制备方法及其应用,为了使本发明的优点、技术方案更加清楚、明确,下面结合具体实施例对本发明做详细说明。
本发明所需原料均可通过商业渠道购买获得。
本发明制备得到的双缩合席夫碱酸化缓蚀剂的分子结构如式(1)所示。
实施例1:
双缩合席夫碱酸化缓蚀剂的制备方法,具体包括以下步骤:
在合成装置中,添加30mL的无水乙醇,3.69g肉桂醛溶液,充分搅拌后,用油浴锅加热至80℃,到达回流温度后,滴加1.44g二乙烯三胺溶液,滴速控制在15-20min内滴完,回流5h,反应结束后,放入冰水浴中冷却,待固体析出后用乙醇洗涤,并用乙醇氯仿(体积比3:1)重结晶三次,干燥后即得所需产品。
对实施例1中获得的特定双缩合席夫碱型酸化缓蚀剂进行核磁谱图分析;
检测仪器;布鲁克AV400
实验结果见图1所示,肉桂醛缩二乙烯三胺的核磁共振氢谱中:δ7.254(s,h 2H;C=N)为碳氮双键上氢的质子峰,由于N原子的吸电子能力强导致碳上的氢电子云密度降低进而使化学位移向低场移动;a-e:δ7.541(s,a、e 4H;trizole CH),δ7.33(s,c 2H;trizoleCH),δ7.388-7.675(s,b、d 4H;trizole CH);分别对应芳香环分子上的3组氢质子峰,电子云密度受与苯环相连基团吸电子作用而降低,进而氢的化学位移向低场移动。δ4.855(s,f2H,CH);δ5.251(s,g 2H,CH)分别为连接C=C上的两个氢;i-j:δ3.325-3.903(s,i 4H;CH),δ2.551-3.003(s,j 4H;CH)为CH上的活泼氢,由于分子内氢键的影响导致化学位移向低场移动,峰面积比例同缓蚀剂RGQ结构中的氢质子个数比例一致。
下面对实施例1制备得到的双缩合席夫碱型酸化缓蚀剂的应用做主要说明。
以失重法来测试肉桂醛缩二乙烯三胺在15%(质量百分数)的盐酸溶液对N80钢片的缓蚀性能。肉桂醛缩二乙烯三胺由本文上述方法制备,其余盐酸、乙醇等试剂均采用国内试剂厂家的分析纯级别产品。实验过程所用金属为N80碳钢。
失重试验
将金属试片用乙醇和丙酮分别清洗,烘干后称重,将其挂入空白和加入缓蚀剂的实验室配置的15wt.%HCl溶液中,浸泡一定时间,取出挂片,用酸洗液洗出腐蚀产物,之后用清水、乙醇、丙酮分别清洗,烘干后称重。
式(2)中:rcorr-匀腐蚀速率,mm/年;m-实验前的试片质量,g;mt-实验后的试片质量,g;S1-试片的总面积;ρ-试片材料的密度,g/cm2;t-实验时间,h。
式(3)中:η1-缓蚀率;Δm0-空白实验中挂片的质量损失,g;Δm1-加入缓蚀剂的实验中挂片的质量损失,g。
由(2)、(3)计算平均腐蚀速率和缓蚀效率。
表1不同浓度缓蚀剂在15%盐酸溶液中的失重法结果
采用常压静态失重法了研究缓蚀剂的添加量对腐蚀行为的影响,该一系列的实验分别测试了在15wt.%HCl的作用效果。
从表1可以看出,肉桂醛缓蚀剂的缓蚀率随缓蚀剂浓度的增加而增大,这主要也是由于缓蚀剂分子在碳钢表面的吸附和覆盖程度随缓蚀剂浓度的增加而增大。当缓蚀剂的添加浓度仅为0.02wt.%,金属的腐蚀速率将发生了明显的下降,腐蚀速率由239.93g·m-2·h-1减小至38.72g·m-2·h-1。当缓蚀剂的添加量为0.1wt.%时,其腐蚀速率减小至9.59g·m-2·h-1,其最高缓蚀效率可达96%。
实施例2:
双缩合席夫碱酸化缓蚀剂的制备方法,具体包括以下步骤:
在合成装置中,添加50mL的无水乙醇,3.69g肉桂醛溶液,充分搅拌后,用油浴锅加热至70℃,到达回流温度后,滴加1.44g二乙烯三胺溶液,滴速控制在15-20min内滴完,回流4h,反应结束后,放入冰水浴中冷却,待固体析出后用乙醇洗涤,并用乙醇氯仿(体积比3:1)重结晶三次,干燥后即得所需产品。
实施例3:
双缩合席夫碱酸化缓蚀剂的制备方法,具体包括以下步骤:
在合成装置中,添加40mL的无水乙醇,3.69g肉桂醛溶液,充分搅拌后,用油浴锅加热至90℃,到达回流温度后,滴加1.44g二乙烯三胺溶液,滴速控制在15-20min内滴完,回流6h,反应结束后,放入冰水浴中冷却,待固体析出后用乙醇洗涤,并用乙醇氯仿(体积比3:1)重结晶三次,干燥后即得所需产品。
本发明中未述及的部分借鉴现有技术即可实现。
需要说明的是:在本说明书的教导下本领域技术人员所做出的任何等同方式或明显变型方式均应在本发明的保护范围内。
Claims (7)
1.一种双缩合席夫碱酸化缓蚀剂的制备方法,其特征在于,依次包括以下步骤:
a、在合成装置中,添加无水乙醇和肉桂醛溶液,充分搅拌后,对其进行加热,加热至回流温度后,向该合成装置中滴加二乙烯三胺溶液,回流反应;
b、反应结束后,将所得产物放入冰水浴中进行冷却,待固体析出后用乙醇洗涤,并用乙醇和氯仿重结晶,干燥后即得。
2.根据权利要求1所述的一种双缩合席夫碱酸化缓蚀剂的制备方法,其特征在于:步骤a中,无水乙醇的体积为30~50mL。
3.根据权利要求1所述的一种双缩合席夫碱酸化缓蚀剂的制备方法,其特征在于:肉桂醛和二乙烯三胺的摩尔比为2:1。
4.根据权利要求1所述的一种双缩合席夫碱酸化缓蚀剂的制备方法,其特征在于:步骤a中,用油浴锅进行加热,加热至温度为70~90℃,回流反应4~6h。
5.根据权利要求1所述的一种双缩合席夫碱酸化缓蚀剂的制备方法,其特征在于:步骤b中,乙醇和氯仿的体积比为3:1。
6.根据权利要求1~5任一项所述的一种双缩合席夫碱酸化缓蚀剂的制备方法制备得到的双缩合席夫碱酸化缓蚀剂。
7.根据权利要求6所述的双缩合席夫碱酸化缓蚀剂在油气田开采化学防腐中的应用。
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