CN114164431B - 一种超支化有机离子液体型金属缓蚀剂及其制备方法 - Google Patents
一种超支化有机离子液体型金属缓蚀剂及其制备方法 Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- WMQUKDQWMMOHSA-UHFFFAOYSA-N 1-pyridin-4-ylethanone Chemical compound CC(=O)C1=CC=NC=C1 WMQUKDQWMMOHSA-UHFFFAOYSA-N 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- 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
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—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
- 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
- C07D213/24—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 with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D213/28—Radicals substituted by singly-bound oxygen or sulphur atoms
- C07D213/30—Oxygen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Pyridine Compounds (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
本发明涉及有机金属缓蚀剂领域,特别涉及一种超支化有机离子液体型金属缓蚀剂及其制备方法。本发明的一种超支化有机离子液体型金属缓蚀剂的合成方法简单、原料易得、收率高;且所述环境友好的枝状与超支化的季铵盐氮杂环类的有机离子液体分子用作缓蚀剂,能够在腐蚀性水溶液中能够发生自组装而形成规整的微‑纳米颗粒,能够在金属表面产生极强的吸附作用,实现在严酷腐蚀性水介质下对金属的高效缓蚀。
Description
技术领域
本发明涉及有机金属缓蚀剂领域,特别涉及一种超支化有机离子液体型金属缓蚀剂及其制备方法。
背景技术
金属如钢铁、铜、铝等常常需要在严酷腐蚀性介质中应用,如酸、碱、盐等水溶液中,因此金属极易被侵略性离子腐蚀破坏。金属的腐蚀不但会造成巨大的经济损失,且会造成安全事故、导致环境污染、以及造成生态失衡等严重后果。因此,化学工业生产中的金属生存性问题受到人们极大的关注。关于严酷腐蚀性水环境下的金属腐蚀与有效缓蚀的研究是关乎国计民生的重大战略,是化学工程与材料工程领域中急需解决的问题之一。
迄今为止,人们发展了一些方法用以抑制金属在侵略性介质中被腐蚀,如涂镀非金属和金属保护层、处理腐蚀介质、电化学保护等,但是这些方法要么防腐蚀效果可能不理想,要么对原体系可能造成破坏,以致产生其他问题,如成本高、工艺复杂、难以操作及应用范围受限。
但是,近年来人们发现某些含氧、氮、磷、硫等杂原子的极性基团,或含不饱和π键等的有机分子在酸、碱、盐等严酷腐蚀性水体系中能够有效地吸附在金属表面,从而减缓金属腐蚀。一般认为有机缓蚀剂通过其分子骨架上杂原子的孤对电子或共轭π键的离域电子云与金属原子的空轨道相互作用,形成化学配位键而在金属表面形成吸附层,阻挡了侵略性离子对金属表面的进攻。因其具有成本低、工艺简便、操作简便、适应性强、不需要特殊的复杂设备,且不会对被保护金属装置等产生破坏等优点,引起人们极大兴趣。因此,发展新型的有机缓蚀剂成为化学工程与材料工程领域中研究重点之一。
基于绿色化工与生态环境保护的要求,发展环境友好的绿色有机缓蚀剂成为必然。与硫、磷类有机缓蚀剂分子相比,含氮杂环的有机分子对生态环境影响更小。因此,难挥发、不燃烧、热稳定性较好、亲水性较优、化学配位较强的季铵盐氮杂环类的有机离子液体型分子成为首选。
发明内容
本发明针对传统抑制金属防腐蚀中存在的问题提出一种新型的超支化有机离子液体型金属缓蚀剂及其制备方法。
为了达到上述目的,本发明是采用下述的技术方案实现的:
本发明的目的在于提供一种超支化有机离子液体型金属缓蚀剂,其结构式如下:
。
本发明的另一目的在于提供一种超支化有机离子液体型金属缓蚀剂的制备方法,包括如下步骤:
将对羟基苯甲醛和4-乙酰吡啶加入锥形瓶,加入乙醇,搅拌均匀,将氢氧化钾加入到溶液中,搅拌1分钟,混合溶液变成棕色,然后加入浓氨水(25%),密封搅拌,反应24小时后加入冰醋酸调pH=7,有浅黄色沉淀出现,抽滤,乙腈重结晶,得到白色固体,即4-([4,2':6',4''-三联吡啶]-4'-基)苯酚。
反应方程式如下:
,其中a为C2H5OH,KOH,浓氨水,冰醋酸。
三颈烧瓶中加入THF溶液中,取三乙二醇加入瓶中,取PBr5缓慢加入到反应液中,室温搅拌2小时,TLC监测,反应完成后加入Na2CO3调pH至中性,萃取、干燥,柱层析(石油醚/乙酸乙酯=4:1),得到黄色油状产物,即1,2-双(2-溴乙氧基)乙烷。
反应方程式如下:
,其中b为PBr5,THF。
取1,2-双(2-溴乙氧基)乙烷和4-([4,2':6',4''-三联吡啶]-4'-基)苯酚于三颈烧瓶中,加入丙酮以及少量18-冠-6,回流反应12小时,得到浅黄色固体粉末,甲苯/环己烷重结晶,产率75%,即1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷。
反应方程式如下:
,其中C为K2CO3,18-C-6,丙酮。
取溴己烷和1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷于的乙腈(CH3CN)中,60℃搅拌8小时;得到黄色粉末状固体,抽滤,用乙腈/环己烷(1:4)混合溶液洗2-3次(15mL/次),得到较纯净的目标产物,即为4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物。
与现有技术相比,本发明的优点和积极效果在于:
本发明的一种超支化有机离子液体型金属缓蚀剂的合成方法简单、原料易得、收率高;且所述环境友好的枝状与超支化的季铵盐氮杂环类的有机离子液体分子用作缓蚀剂,能够在腐蚀性水溶液中能够发生自组装而形成规整的微-纳米颗粒,能够在金属表面产生极强的吸附作用,实现在严酷腐蚀性水介质下对金属的高效缓蚀。
附图说明
图1为实施例1中有机离子液体型金属缓蚀剂4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物分子的核磁共振氢谱图;
图2为实施例1中有机离子液体型金属缓蚀剂分子在0.15 mM下在0.5 mol/L的硫酸溶液中自组装2小时后的电镜图: (a) 扫描电子显微镜(SEM)的显微照片; (b) 透射电子显微镜(TEM)的显微图片
图3(a)为未浸泡实施例1中有机离子液体型金属缓蚀剂分子自组装体的空白铜试样表面的扫描电子显微镜(SEM)显微图片;(b)浸泡含有0.15 mM 实施例1中有机离子液体型金属缓蚀剂分子自组装体的0.5 mol/L H2SO4溶液15分钟后的金属铜表面的显微图片
图4 铜表面的扫描电子显微镜(SEM)的显微照片:(a) 在不含有实施例1中有机离子液体型金属缓蚀剂分子自组装体的0.5 mol/L的硫酸溶液中浸泡15天后;(b)铜在含有0.15 mM的实施例1中有机离子液体型金属缓蚀剂分子自组装体的溶液中充分吸附后,浸泡于0.5 mol/L硫酸液15 天后。
图5含有0.15 mM的实施例1中有机离子液体型金属缓蚀剂分子自组装体在0.5mol/L的硫酸溶液中对金属铜电极吸附不同时间后(分别为10 min、15 min) 的交流阻抗图。
具体实施方式
为了能够更清楚地理解本发明的上述目的、特征和优点,下面结合具体实施例对本发明做进一步说明。需要说明的是,在不冲突的情况下,本申请的实施例及实施例中的特征可以相互组合。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是,本发明还可以采用不同于在此描述的其他方式来实施,因此,本发明并不限于下面公开说明书的具体实施例的限制。
实施例1
本实施例提供有机离子液体型金属缓蚀剂4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物的制备。结构式如下:
。
(1)将1mmol对羟基苯甲醛和2mmol 4-乙酰吡啶加入50mL锥形瓶,加入10mL乙醇,搅拌均匀,将0.36g氢氧化钾加入到溶液中,200转/min转速下搅拌1分钟,混合溶液变成棕色,然后加入3mL质量分数25%的浓氨水,密封,300转/min转速下搅拌,反应24小时后加入冰醋酸调pH=7,有浅黄色沉淀出现,抽滤,乙腈75℃重结晶,得到白色固体,即4-([4,2':6',4''-三联吡啶]-4'-基)苯酚。
(2)三颈烧瓶中加入30mL THF溶液中,取三乙二醇1mmol加入瓶中,取2.5mmolPBr5缓慢加入到反应液中,室温搅拌2小时,TLC监测,反应完成后加入1mol/L Na2CO3水溶液调pH至中性,加入15ml二氯甲烷萃取、抽真空干燥,柱层析(石油醚/乙酸乙酯=4:1),得到黄色油状产物,即1,2-双(2-溴乙氧基)乙烷。
(3)取1,2-双(2-溴乙氧基)乙烷1mmol和2mmol4-([4,2':6',4''-三联吡啶]-4'-基)苯酚于三颈烧瓶中,加入50mL丙酮以及2ml的18-冠-6,回流反应12小时,得到浅黄色固体粉末,甲苯/环己烷(体积比1:1,20ml,70℃)重结晶,经检测产率为75%,即1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷。
(4)取7.2mmol的溴己烷和1.0mmol的1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷于300mL的乙腈(CH3CN)中,60℃搅拌8小时;得到黄色粉末状固体,抽滤,用乙腈/环己烷(1:4)混合溶液洗2-3次(15mL/次),得到较纯净的目标产物,即为4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双(1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物。经检测,产物的熔点为173.4-175.6℃。1H-NMR (400 MHz, DMSO-d 6 ) δ (ppm): 9.301-9.164(m, Ar-H, 8H),8.907-8.888(d, J=7.6 Hz, Ar-H, 4H), 8.224-8.108 (m, Ar-H, 8H), 7.177-7.124(m, Ar-H, 8H), 4.680 (s, -CH2, 12H), 4.111-4.104 (d, J=2.8 Hz, -CH2, 8H),1.969 (s, -CH2, 4H), 1.362-1.023 (m, -CH2, 48H), 0.851 (s, -CH3, 18H)。
其核磁共振氢谱如图1所示。
反应方程式如下:
。
实施例2
本实施例提供有机离子液体型金属缓蚀剂4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物的制备。本实施例未特殊说明之处,与实施例1一致。
(1)将2mmol对羟基苯甲醛和4mmol 4-乙酰吡啶加入50mL锥形瓶,加入10mL乙醇,搅拌均匀,将0.75g氢氧化钾加入到溶液中,200转/min转速下搅拌1分钟,混合溶液变成棕色,然后加入3mL质量分数25%的浓氨水,密封,500转/min转速下搅拌,反应24小时后加入冰醋酸调pH=7,有浅黄色沉淀出现,抽滤,8ml乙腈75℃重结晶,得到白色固体,即4-([4,2':6',4''-三联吡啶]-4'-基)苯酚。
(2)三颈烧瓶中加入61mL THF溶液中,取三乙二醇2mmol加入瓶中,取4.9mmolPBr5缓慢加入到反应液中,室温搅拌2.5小时,TLC监测,反应完成后加入1mol/L Na2CO3水溶液调pH至中性,加入25ml二氯甲烷萃取、抽真空干燥,柱层析(石油醚/乙酸乙酯=4:1),得到黄色油状产物,即1,2-双(2-溴乙氧基)乙烷。
(3)取1,2-双(2-溴乙氧基)乙烷1.5mmol和2.94mmol4-([4,2':6',4''-三联吡啶]-4'-基)苯酚于三颈烧瓶中,加入85mL丙酮以及4ml的18-冠-6,回流反应15小时,得到浅黄色固体粉末,甲苯/环己烷(体积比1:1,20ml,70℃)重结晶,经检测产率为76%,即1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷。
(4)取7.2mmol的溴己烷和1.0mmol的1,2-双(2-(4-([4,2':6',4''-三联吡啶]-4'-基)苯氧基)乙氧基)乙烷于300mL的乙腈(CH3CN)中,65℃搅拌7.5小时;得到黄色粉末状固体,抽滤,用乙腈/环己烷(1:4)混合溶液洗2-3次(20mL/次),得到较纯净的目标产物,即为4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物。经检测,产物的熔点为174.2-175.4℃。1H-NMR (400 MHz, DMSO-d 6 ) δ (ppm): 9.302-9.168(m, Ar-H,8H), 8.904-8.886(d, J=7.6 Hz, Ar-H, 4H), 8.221-8.105 (m, Ar-H, 8H), 7.175-7.123 (m, Ar-H, 8H), 4.681 (s, -CH2, 12H), 4.110-4.105 (d, J=2.8 Hz, -CH2,8H), 1.968 (s, -CH2, 4H), 1.363-1.021 (m, -CH2, 48H), 0.850 (s, -CH3, 18H).
有机离子液体型金属缓蚀剂性能检测。
以实施例1中制备得到的产物进行性能检测。
1. 4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物在腐蚀性水介质中自组装。
称取适量的4',4''''-(((((乙烷-1,2-二基双(氧))双(乙烷-2,1-二基))双(氧))双(4,1-亚苯基))双 (1,1',1''-三己基-[4,2':6',4''-三联吡啶]-1,1',1''-三)溴化物溶于含有腐蚀介质(此处以0.5 mol/L的硫酸为例)的水溶液中配成不同浓度的目标分子溶液,在室温的条件下用超声波超声30 s,使目标分子在水介质中分散均匀。最后将溶有离子液缓蚀剂的水体系在25 °C 恒温箱中静置自组装一段时间。目标分子发生自组装,形成了规则的有机微-纳米自组装体,将自聚体结构(形貌与尺寸)进行充分表征(扫描电镜和透射电镜分析)。
2. 金属表面吸附测试
将金属铜片逐级使用2000、3000、5000# 水磨砂纸进行打磨,然后依次使用二次蒸馏水、乙醇、丙酮超声清洗,于真空干燥箱干燥。处理过的铜片分别放入上述含有稳定分子自组装体的腐蚀溶液中和不含枝状和超支化目标分子组装体的空白腐蚀溶液中,一定时间后取出并用乙醇清洗,干燥,然后在扫描电镜(MIRA3 LMHSEM)下分析表面金属表面形态,使用时扫面电压为15 kV,扫描倍数为5000。
3. 金属防腐电化学测试
将工作电极的表面依次用400#、800#、1200#、2000# 的水性磨砂纸逐级打磨至呈光滑镜面,再依次放入蒸馏水、无水乙醇中进行超声处理,放入真空干燥箱干燥,然后将处理后的电极片放入含有枝状和超支化目标分子的稳定自组装体系的腐蚀溶液中进行吸附,达到吸附平衡后取出铜电极并用乙醇清洗,真空干燥箱干燥,取出安装于聚四氟乙烯电极套备用。利用电化学分析仪进行测试,试验体系为含有不同浓度枝状和超支化目标分子组装体的0.5 mol/L的硫酸溶液,以未添加枝状和超支化目标分子组装体的0.5 mol/L的硫酸溶液作为空白对照。先进行开路电位的测试,待开路电位稳定后,测试交流阻抗测试。
附图1是实施例1中一种超支化有机离子液体型金属缓蚀剂的核磁共振氢谱,可以看到其烷基链氢非常明显;附图2是一种超支化有机离子液体型金属缓蚀剂在0.15 mM的浓度下可以自组织形成柱状的微米级(长度)自组织体颗粒;附图3可以看到这些自主装体形成的微米级结构规整颗粒可以吸附在金属铜表面,形成致密的保护吸附层;附图4可以看到在0.5 mol/L硫酸水环境中,目标分子自组织体对金属起到良好的保护作用;附图5可以看到铜在含有0.15 mM的Target 1分子自组织体中的吸附速度在10 min左右在金属表面就可达到吸附平衡。虽然吸附10分钟后的Nyquist曲线阻抗弧相比于吸附15分钟略小,其缓蚀效率与吸附15 分钟非常接近,缓蚀效率可到97%以上,说明分子自组织体对铜表面吸附快速和高效,吸附层性质良好。
本发明提供了一种超支化有机离子液体型金属缓蚀剂及其制备方法。所述超支化有机离子液体型金属缓蚀剂分子是对羟基苯甲醛和4-乙酰吡啶为原料,经缩合、取代、成醚,最后与溴己烷成盐反应而得。所述一种超支化有机离子液体型金属缓蚀剂能够在腐蚀性水溶液中能够发生自组装而形成规整的微-纳米颗粒,能够在金属表面产生极强的吸附作用,形成良好的保护层,实现在严酷腐蚀性水介质下对金属的高效缓蚀,具有环保、绿色、高效防腐等特点。
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例应用于其它领域,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (5)
1.一种超支化有机离子液体型金属缓蚀剂,其特征在于,结构式如下:
。
2.权利要求1所述超支化有机离子液体型金属缓蚀剂制备方法,其特征在于,步骤如下:
(1)将对羟基苯甲醛和4-乙酰吡啶加入反应容器,加入乙醇,搅拌均匀得到混合溶液,将氢氧化钾加入到混合溶液中,搅拌至混合溶液变成棕色,
(2)加入浓氨水,密封搅拌反应,反应结束后加入冰醋酸调pH=7,出现浅黄色沉淀,抽滤,乙腈重结晶,得到白色固体;
(3)容器中加入THF溶液,加入三乙二醇,然后缓慢加入PBr5,室温搅拌反应,TLC监测,反应完成后加入Na2CO3调pH至中性;
(4)萃取、干燥,柱层析,得到黄色油状产物1,2-双(2-溴乙氧基)乙烷;
(5)取1,2-双(2-溴乙氧基)乙烷和4-([4,2':6',4''-三联吡啶]-4'-基)苯酚混合,加入丙酮以及少量18-冠-6,回流反应,得到浅黄色固体粉末,甲苯/环己烷重结晶,得到产物A;
(6)将溴己烷和产物A,加入乙腈中搅拌反应,得到黄色粉末状物质,抽滤,并用乙腈/环己烷混合溶液洗2-3次,得到目标产物。
3.根据权利要求2所述超支化有机离子液体型金属缓蚀剂制备方法,其特征在于,所述步骤(1)中对羟基苯甲醛:4-乙酰吡啶:氢氧化钾摩尔比为1:2:(6-7)。
4.根据权利要求2所述超支化有机离子液体型金属缓蚀剂制备方法,其特征在于,所述步骤(3)中PBr5:对羟基苯甲醛摩尔比为2.5:1;步骤(5)中1,2-双(2-溴乙氧基)乙烷与4-([4,2':6',4''-三联吡啶]-4'-基)苯酚摩尔比为1:2;步骤(6)中反应时间为55-60℃,反应时间为7-8小时。
5.权利要求2-4所述方法制备得到的超支化有机离子液体型金属缓蚀剂在腐蚀水体系金属缓释中的应用。
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