CN108642500A - 一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用 - Google Patents

一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用 Download PDF

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CN108642500A
CN108642500A CN201810679781.XA CN201810679781A CN108642500A CN 108642500 A CN108642500 A CN 108642500A CN 201810679781 A CN201810679781 A CN 201810679781A CN 108642500 A CN108642500 A CN 108642500A
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corrosion inhibiter
bipyridyl
ammonium salt
quaternary ammonium
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CN108642500B (zh
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张光华
董秋辰
张万斌
张策
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Shaanxi Liyuan Technology Co ltd
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    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
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    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/22—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing two or more pyridine rings directly linked together, e.g. bipyridyl
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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Abstract

一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用，此类缓蚀剂的结构特点是在4,4‑联吡啶的两端通过季铵化反应连接了两个对称的氯化苄单体，该缓蚀剂的制备方法为：以4,4‑联吡啶和氯化苄为原料，溶于有机溶剂后，在40～80℃的条件下，经季铵化反应制备而得，该发明的有益效果在于，这种缓蚀剂的制备方法涉及的原料易得，反应条件温和，合成步骤简单。同时其具有良好的水溶性和缓蚀性能，在20ppm用量下，缓蚀率可达到96％以上，缓蚀时间长且稳定性好，制备工艺简单，适用于规模化应用。

Description

一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用
技术领域
本发明涉及石油化工和表面活性剂技术领域，特别涉及一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用。
背景技术
在油气开采和运输的过程中，由于高流速和各种腐蚀介质的联合作用，输送管道和金属设备会受到严重的腐蚀和磨蚀，使得设备的寿命减短，造成巨大的经济损失，同时也易出现安全隐患。据国外权威机构估计，如果防腐蚀技术能被充分有效的利用，腐蚀的损失可以挽回30％～40％。实践表明，缓蚀剂是防止金属材料及其合金在使用环境介质中发生腐蚀的有效防护措施，其广泛应用于石油化工、化学清洗、工业用水等领域。
目前，国内外大量采用亚硝酸盐、乌洛托品等作为水溶性缓蚀剂，这类缓蚀剂虽然性能良好，但是用量较大，缓蚀率低，而且当缓蚀剂用量不足时反而会导致严重的局部腐蚀，并且一般都有毒，由于生态环境日益受到重视，所以这类物质已被禁止或限制使用。
发明内容
为了克服上述现有技术的不足，本发明的目的在于提供一种水溶性联吡啶双子季铵盐缓蚀剂及其制备方法及应用，具有合成工艺简单，原料廉价易得，适用于规模化生产的特点。
为了实现上述目的，本发明采用的技术方案是：
一种水溶性联吡啶双子季铵盐缓蚀剂，通过季铵化反应，将两个氯化苄单体引入4,4-联吡啶的两端，其具有以下的结构：
一种水溶性联吡啶双子季铵盐缓蚀剂的制备方法，包括以下步骤：
步骤1：在装有搅拌棒和冷凝管的三口烧瓶中加入4,4-联吡啶、氯化苄以及有机溶剂，升温进行季铵化反应，反应结束后，得到混合液Ⅰ；
步骤2：将所述的混合液Ⅰ经过滤除去有机溶剂，得到固体粗产品Ⅱ；
步骤3：将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。
所述步骤1中的4,4-联吡啶和氯化苄的投料摩尔比为1:2～2.2；反应物原料与有机溶剂的质量比为1:1～1.5。
所述步骤1中的反应温度为40～80℃，反应时间为4～8小时。
所述步骤1中的有机溶剂包括丙酮、N,N-二甲基甲酰胺、乙醇、四氢呋喃、氯仿中的任意一种或两种以上的组合；优选的，所述的有机溶剂选自丙酮或N,N-二甲基甲酰胺。
一种水溶性联吡啶双子季铵盐缓蚀剂应用于金属酸洗、水处理等金属防腐蚀领域。
本发明的有益效果：
1、发明所提出的联吡啶双子季铵盐缓蚀剂，其合成工艺简单，原料廉价易得，反应条件温和，水溶性良好，绿色环保且对环境无污染，适用于规模化生产。
2、发明所提出的联吡啶双子季铵盐缓蚀剂，与现有技术相比，其使用方法简单，用水稀释即可，缓蚀时间长且稳定性好，制备方法简单，且用量少，使用效果好。例如当该含联苯基的缓蚀剂在20ppm用量下，缓蚀率可达到96％以上，可适用于大规模的应用。
附图说明
图1为本发明制备流程图。
图2为本发明核磁共振氢谱谱图及各化学位移的归属。
具体实施方式
下面结合实施例对本发明作进一步详细说明。
一、制备实施例
实施例1
(1)在装有搅拌棒和冷凝管的三口烧瓶中加入15.62g4,4-联吡啶(100mmol)、25.32g氯化苄(200mmol)以及51ml有机溶剂丙酮，升温至40℃，进行季铵化反应5个小时。反应结束后，得到混合液Ⅰ；(2)将所述的混合液Ⅰ利用过滤除去多余的丙酮，得到固体粗产品Ⅱ；
(3)将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。产率为79％。(如图1所示)
实施例2
(1)在装有搅拌棒和冷凝管的三口烧瓶中加入15.62g4,4-联吡啶(100mmol)、27.85g氯化苄(220mmol)以及81ml有机溶剂丙酮，升温至50℃，进行季铵化反应6个小时。反应结束后，得到混合液Ⅰ；
(2)将所述的混合液Ⅰ利用过滤除去多余的丙酮，得到固体粗产品Ⅱ；
(3)将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。产率为90％。
实施例3
(1)在装有搅拌棒和冷凝管的三口烧瓶中加入15.62g4,4-联吡啶(100mmol)、25.32g氯化苄(200mmol)以及43ml有机溶剂N,N-二甲基甲酰胺，升温至70℃，进行季铵化反应8个小时。反应结束后，得到混合液Ⅰ；
(2)将所述的混合液Ⅰ利用过滤除去多余的N,N-二甲基甲酰胺，得到固体粗产品Ⅱ；
(3)将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。产率为83％。
实施例4
(1)在装有搅拌棒和冷凝管的三口烧瓶中加入15.62g4,4-联吡啶(100mmol)、27.85g氯化苄(220mmol)以及68ml有机溶剂N,N-二甲基甲酰胺，升温至80℃，进行季铵化反应7个小时。反应结束后，得到混合液Ⅰ；
(2)将所述的混合液Ⅰ利用过滤除去多余的N,N-二甲基甲酰胺，得到固体粗产品Ⅱ；
(3)将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。产率为88％。
实施例5
(1)在装有搅拌棒和冷凝管的三口烧瓶中加入15.62g4,4-联吡啶(100mmol)、27.85g氯化苄(220mmol)以及81ml有机溶剂丙酮，升温至55℃，进行季铵化反应6个小时。反应结束后，得到混合液Ⅰ；
(2)将所述的混合液Ⅰ利用过滤除去多余的丙酮，得到固体粗产品Ⅱ；
(3)将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。产率为92％。
二实验例
1水溶性实验(如图2所示)
观察实施例1和实施例4中所制备的水溶性缓蚀剂在100ppm浓度下的水溶性，发现缓蚀剂的溶解速度快，溶解后溶液明显澄清；同时，通过紫外光谱的透过率测试，发现溶液的透过率分别为96％和97％。这说明发明所涉及的含联苯基的缓蚀剂具有良好的水溶性。
2缓蚀性能实验
在30℃下，利用失重法测试了实施例1、实施例3、实施例5中所制备的水溶性缓蚀剂在1M HCl腐蚀介质中对Q235普通碳钢的缓蚀率。经4h测试后发现：加入量为20ppm时缓蚀率分别为96％、95％、96％，均表现出优良的缓蚀性能。另外，经测试在高温环境中这种缓蚀剂的缓蚀效果依然良好。

Claims (6)

1.一种水溶性联吡啶双子季铵盐缓蚀剂，其特征在于，通过季铵化反应，将两个氯化苄单体引入4,4-联吡啶的两端，其具有以下的结构：
2.基于权利要求1所述缓蚀剂的制备方法，其特征在于，包括以下步骤：
步骤1：在装有搅拌棒和冷凝管的三口烧瓶中加入4,4-联吡啶、氯化苄以及有机溶剂，升温进行季铵化反应，反应结束后，得到混合液Ⅰ；
步骤2：将所述的混合液Ⅰ经过滤除去多余的有机溶剂，得到固体粗产品Ⅱ；
步骤3：将所述的粗产品Ⅱ使用乙酸乙酯进行多次重结晶后，经过滤、干燥即可得到这种水溶性联吡啶双子季铵盐缓蚀剂。
3.根据权利要求2所述的一种水溶性联吡啶双子季铵盐缓蚀剂的制备方法，其特征在于，所述步骤1中的4,4-联吡啶和氯化苄的投料摩尔比为1:2～2.2，反应原料与有机溶剂的质量比为1:1～1.5。
4.根据权利要求2所述的一种水溶性联吡啶双子季铵盐缓蚀剂的制备方法，其特征在于，所述步骤1中的反应温度为40～80℃，反应时间为4～8小时。
5.根据权利要求2所述的一种水溶性联吡啶双子季铵盐缓蚀剂的制备方法，其特征在于，所述步骤1中的有机溶剂包括丙酮、N,N-二甲基甲酰胺、乙醇、四氢呋喃、氯仿中的任意一种或两种以上的组合；优选的，所述的有机溶剂选自丙酮或N,N-二甲基甲酰胺。
6.根据权利要求1或2所述的一种水溶性联吡啶双子季铵盐缓蚀剂应用于金属酸洗、水处理等金属防腐蚀领域。
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CN111441056A (zh) * 2020-04-20 2020-07-24 中国石油天然气集团公司 双十二烷基-二甲酰胺联吡啶季铵盐水溶缓蚀剂及其制备方法和应用
CN111441056B (zh) * 2020-04-20 2022-05-20 中国石油天然气集团公司 双十二烷基-二甲酰胺联吡啶季铵盐水溶缓蚀剂及其制备方法和应用
CN114591224A (zh) * 2020-12-03 2022-06-07 中国石油天然气股份有限公司 一种具备水合物抑制功能的缓蚀剂及其制备方法和应用
CN114591224B (zh) * 2020-12-03 2024-04-30 中国石油天然气股份有限公司 一种具备水合物抑制功能的缓蚀剂及其制备方法和应用
CN114231266A (zh) * 2021-12-31 2022-03-25 成都劳恩普斯科技有限公司 一种兼具杀菌性能的不起泡无硫缓蚀剂及其制备方法
CN114231266B (zh) * 2021-12-31 2022-12-02 成都劳恩普斯科技有限公司 一种兼具杀菌性能的不起泡无硫缓蚀剂及其制备方法

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