CN102534623A - 一种聚丙烯酸类气相缓蚀剂的制备方法 - Google Patents
一种聚丙烯酸类气相缓蚀剂的制备方法 Download PDFInfo
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Abstract
本发明属腐蚀与防护技术领域,涉及一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于步骤依次为:⑴容器中以去离子水为溶剂,加入链转移剂异丙醇,搅拌并加热至65-75℃,再滴加丙烯酸单体和链引发剂过硫酸铵水溶液,保温反应两个小时左右得聚丙烯酸溶液;⑵所得聚丙烯酸中加入丙酮,再缓慢滴加与所述聚丙烯酸等摩尔量的有机胺吗啉,搅拌使其充分反应,并控制pH值为7-8,降温至60℃出料,得到淡黄色的聚丙烯酸吗啉粘稠液体,减压旋转蒸发蒸出溶剂后,得到聚丙烯酸吗啉固体粉末。本发明的有益效果是:在吸水性树脂分子上直接接枝吗啉基团,弥补气相缓蚀剂在高湿环境下防锈性能的不足,并具有较大的分子覆盖面积,增强防锈效果。
Description
技术领域
本发明属腐蚀与防护技术领域,涉及一种可用于机械、钢铁等行业金属制品储运期间防腐蚀的,具有吸水性的聚合物气相缓蚀剂,尤其涉及一种聚丙烯酸类气相缓蚀剂的制备方法。
背景技术
大气腐蚀是存在最广泛的一种腐蚀,所造成的损失占全部腐蚀损失的一半以上。传统的金属制品防锈包装工艺,是包装前在金属制品表面涂沫一层防锈油,在包装启封前需采用氟氯烃等有机溶剂脱除金属表面残留的油脂,不仅繁琐,而且氟氯烃可以破环地球的大气臭氧层,此法受到越来越多的限制。气相缓蚀剂(vapor phase inhibitor, 简称VPI),又叫挥发性缓蚀剂(volatile corrosion inhibitor, 简称VCI)或气相防锈剂,是一种在常温下能自动挥发的气体被吸附在金属的表面,从而防止金属腐蚀的防腐蚀化学品。气相缓蚀技术具有使用方便、干净、清洁的特点,已成为防止大气腐蚀技术发展的一个重要方向。目前,以气相缓蚀剂为核心的气相防锈材料和防锈工艺在国外已大量应用于工业设备的防锈管理中。
由于气相缓蚀剂的挥发受到环境温度、湿度的制约,潮湿的气氛可以影响它的防锈性能。所以在高湿的条件下使用气相缓蚀剂时,往往需要同时放置干燥剂。常用干燥剂为硅胶、三氧化铝、沸石分子筛等。将气相缓蚀剂和干燥剂按一定比例复合可以制成气相防锈干燥剂,国内外已有较多的文献报道气相防锈干燥剂的制备方法,如日本的藤田敏雄选择了孔径合适、pH值中性的天然沸石处理气相缓蚀剂,制备的两种气相防锈干燥剂,其中气相缓蚀剂的含量在20%-25%(重量比),主要成分有机酸的胺盐、亚硝酸盐和苯并三氮唑等。中国专利(200410051943.3)公开了一种气相缓蚀剂和干燥剂复合制成的气相防锈干燥剂,其特征在于:将气相缓蚀剂和干燥剂按比例制作成气相防锈干燥包,所述气相缓蚀剂和干燥剂的重量比为2%-40%,它们在同一包装密闭环境中同时起到防锈和吸湿的作用。但目前专利报道大都直接采用无机多孔载体,对气相缓蚀剂进行改性,制成的气相防锈干燥剂。其主要缺点是:无机多孔载体对气相缓蚀剂具有吸附作用,从而抑制气相缓蚀剂的挥发和扩散;另一方面,气相缓蚀剂被干燥剂的吸附,也抑制了干燥剂的吸水能力,从而导致其吸水能力不强。
吸水树脂是一种新型功能高分子材料,以其高吸液能力、高吸液速度和高保液能力,广泛应用于生理卫生用品,利用高吸水性树脂制作工业防潮剂也有报道。中国发明专利(CN101052747)公开了一种羟胺化合物和吸水性树脂结合的防锈剂,其特征在于:防锈剂由胺、羟胺或肼化合物构成,吸水性树脂为亲水性环氧树脂,并将防锈剂和吸水性树脂以及将被保护的金属部件共同保存在阻气性容器中。目前用于医药卫生用品的大部分吸水树脂是丙烯酸类高吸水聚合物,与其它类型高吸水剂比较,该类聚合物除了具备高吸水性能外,其还具有生产成本低,工艺简单,产品质量稳定,长时间储存不会变质等特点。但是采用聚丙烯酸吸水树脂和气相缓蚀剂复合的研究,将具有防锈功能的基团直接接枝到聚丙烯酸聚合物上,通过聚合物的吸水性能调控其防锈基团的释放,从而改善其挥发性能和气相缓蚀能力,尚未见报道。
发明内容
本发明所要解决的技术问题是提供一种聚丙烯酸类聚合物气相缓蚀剂的制备方法,在吸水性树脂分子上直接接枝有机胺基团,弥补气相缓蚀剂在高湿环境下防锈性能的不足,增强防锈效果。
为达到上述目的,采取的技术方案是:
一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于包括以下步骤:
⑴合成聚丙烯酸:在装有搅拌器,温度计和两个滴液漏斗的四口烧瓶中,加入60mL去离子水和60-80mL链转移剂,不断搅拌下加热至65-75℃,将分置于两个滴液漏斗中的21mL丙烯酸单体和链引发剂水溶液,在20min内同时开始滴加,并在2-3小时内滴完,保持回流温度反应两个小时左右得聚丙烯酸溶液;采用端基分析法,分析测定聚丙烯酸的分子量,然后改成蒸馏装置,加热蒸出链转移剂以回收利用;
⑵制备聚丙烯酸气相缓蚀剂:步骤⑴所制得的聚丙烯酸烧杯中加入20mL左右的丙酮,再缓慢逐滴加入与所述聚丙烯酸等摩尔量的有机胺,搅拌使其充分反应,并控制pH值为7-8,滴加完毕再搅拌20min,降温至60℃出料,最后得到淡黄色的聚丙烯酸有机胺粘稠液体,所得产物经减压旋转蒸发、蒸出溶剂后,得到的固体产品研磨得到淡黄色的聚丙烯酸有机胺固体粉末。
所述丙烯酸与有机胺的摩尔比为1∶(1.1~1.2)。
所述链引发剂为过硫酸铵、或过硫酸钾、或过氧化苯甲酰、或过氧化月桂酰。
所述链转移剂为异丙醇、或疏基乙醇。
所述有机胺为吗啉、或环己胺、或二环己胺、或哌啶。
本发明的有益效果是:采用聚丙烯酸吗啉聚合物,在吸水性树脂分子上直接接枝吗啉基团,通过吸水性树脂的吸水和固水过程,置换出防锈基团,弥补气相缓蚀剂在高湿环境下防锈性能的不足,同时具有较大的分子覆盖面积,从而增强防锈效果。
具体实施方式
以下通过具体实施例,对本发明作进一步描述。然而,必须说明的是本发明并不局限于这些具体的实施例。
实施例1和实施例2中,以有机胺为吗啉,链引发剂为过硫酸铵,链转移剂为异丙醇为例。
实施例中所述聚丙烯酸分子量的测定是采用端基分析法,分析其数均分子量,具体步骤为:称量由步骤⑴得到的约0.1g样品,放入100mL烧杯中,加入1mol/L的氯化钠溶液250mL,用0.1mol/L的氢氧化钠标准溶液滴定之,测定其pH值;用消耗的氢氧化钠标准溶液毫升数对pH值作图,找出终点所消耗的碱量,计算其分子量。
在模拟大气腐蚀水(100mg/L SO4 2-+100mg/L CL-+100mg/L HCO3 -)中,分别加入由实施例1得到的聚丙烯酸吗啉固体粉末1和由实施例2得到聚丙烯酸吗啉固体粉末2,配制缓蚀溶液,将打磨光滑的碳钢片全浸于缓蚀溶液中、或悬挂于盛有1g缓蚀剂的称量瓶内液面之上气相位置中,作所得产品的防腐蚀性能评价,实验结论分别示于表1(实施例3)和表2(实施例4)。
实施例1
一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于:包括以下步骤:
⑴合成聚丙烯酸:在装有搅拌器,温度计和两个滴液漏斗的250毫升四口烧瓶中,烧瓶内加入60mL去离子水和60mL链转移剂异丙醇,不断搅拌下加热至65-75℃,将分置于两个滴液漏斗中的21mL丙烯酸单体和3mL 100g/L链引发剂过硫酸铵水溶液,在20min内同时开始滴加,并在2-3小时内滴完,保持回流温度反应两个小时左右得聚丙烯酸溶液;采用端基分析法,分析测定聚丙烯酸的数均分子量为3300:然后改成蒸馏装置,加热蒸出链转移剂异丙醇以回收利用;
⑵制备聚丙烯酸气相缓蚀剂:步骤⑴所制得的聚丙烯酸烧杯中加入20mL左右的丙酮,再缓慢逐滴加入27mL吗啉(0.31mol),搅拌使其充分反应,滴加完毕再搅拌20min,并控制pH值为7.2,降温至60℃出料,最后得到淡黄色的聚丙烯酸吗啉粘稠液体,所得产物经减压旋转蒸发、蒸出溶剂后,得到的固体产品研磨得到淡黄色的聚丙烯酸吗啉固体粉末1。
实施例2
一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于:包括以下步骤:
⑴合成聚丙烯酸:在装有搅拌器,温度计和两个滴液漏斗的250毫升四口烧瓶中,烧瓶内加入60mL去离子水和80mL链转移剂异丙醇,不断搅拌下加热至65-75℃,将丙烯酸单体和链引发剂过硫酸铵水溶液分置于两个滴液漏斗中,在20min内同时开始滴加,并在2-3小时内将滴液漏斗中的21mL丙烯酸单体和4mL 100g/L链引发剂过硫酸铵溶液滴入瓶内;滴完后,保持回流温度反应两个小时左右得聚丙烯酸溶液;采用端基分析法,分析测定聚丙烯酸的分子量3300:然后改成蒸馏装置,加热蒸出链转移剂异丙醇以回收利用;
⑵制备聚丙烯酸气相缓蚀剂:步骤⑴所制得的聚丙烯酸烧杯中加入20mL左右的丙酮,再缓慢逐滴加入31mL吗啉(0.36mol),搅拌使其充分反应,滴加完毕再搅拌20min,pH值为7.8,降温至60℃出料,最后得到淡黄色的聚丙烯酸吗啉粘稠液体,所得产物经减压旋转蒸发、蒸出溶剂后,得到的固体产品研磨得到淡黄色的聚丙烯酸吗啉固体粉末2。
实施例3
称量一定量的聚丙稀酸吗啉,用模拟大气腐蚀水,配置10mg/L的聚丙稀酸吗啉缓蚀溶液和10mg/L丙烯酸吗啉缓蚀溶液,然后将打磨光滑的碳钢片全浸放置于所述缓蚀溶液中,在40℃的水浴中加热一个星期,最后称量,得出碳钢片的失重,计算其失重率。
表1全浸实验结果
浓度 | 失重 | 缓蚀率 |
空白 | 0.1291 g | — |
聚丙烯酸吗啉固体粉末1 | 0.0114 g | 91.2% |
聚丙烯酸吗啉固体粉末2 | 0.0169 g | 86.9% |
丙烯酸吗啉 | 0.0711 g | 44.9% |
由表1,可以看出聚丙烯酸吗啉和对比参照物丙烯酸吗啉都有一定的缓蚀作用,但聚丙烯酸吗啉的缓蚀率远远高于单体丙烯酸吗啉的缓蚀率,这是由于聚丙烯酸吗啉分子内有多个缓蚀基团,形成多中心吸附。
实施例4
对实施例1、2所得目标产物和对比参照物丙烯酸吗啉进行气相防锈甑别试验:在锥形瓶放入盛有1g气相缓蚀剂的称量瓶,将50mm×25mm×2mm的45#钢试片挂入,于50℃烘箱中恒温饱和2h。同时作空白试验:然后用移液管注入15mL的蒸馏水,置于恒温箱中保持温度50℃,每天加热8h,每24h为一周期,共进行7周期试验,每天观察一次,检查试片锈蚀的情况,记录锈蚀出现的时间。或在规定时间后洗净、检查锈蚀情况并评级。最后称量处理后的挂片,得出试片的减重。试验结束后用橡皮擦去挂入试片表面的腐蚀产物,称重,计算腐蚀率,结果见表2。
表2气相防锈甑别试验结果
失重 | 缓蚀率 | |
空白 | 0.0560g | — |
聚丙烯酸吗啉1 | 0.0068g | 87.9% |
聚丙烯酸吗啉2 | 0.0089g | 84.1% |
丙烯酸吗啉 | 0.0376g | 32.9% |
由表2可以看出,气相防锈甑别试验与全浸实验结果规律相同,聚丙烯酸吗啉的缓蚀率远远高于单体的丙烯酸吗啉,同时结合表1也可以看出,缓蚀剂在气相防锈甑别试验的缓蚀率低于溶液全浸实验的缓蚀率,这是因为,在薄层电解质中,氧的交换和流动较溶液中快,从而气相防锈的缓蚀能力低于全浸在溶液中的缓蚀能力。
本发明制备聚丙烯酸类聚合物气相缓蚀剂,将具有防锈功能的基团吗啉直接接枝到聚丙烯酸聚合物上,其吸水基团和防锈官能团结合在同一分子内,外界环境的水分可以通过和吸水基团结合,置换出防锈官能团,达到吸水和防锈官能团释放过程的统一。研究表明这种聚合物气相缓蚀剂具有良好的气相缓蚀性能和吸湿能力,可以用于金属的防锈产品的制造中。
以上所述内容仅为本发明构思下的基本说明和最佳实施例,目的是使本领域技术人员能理解和实施本发明,而非用于限制本发明。
Claims (2)
1.一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于包括以下步骤:
⑴合成聚丙烯酸:在装有搅拌器,温度计和两个滴液漏斗的四口烧瓶中,加入60mL去离子水和60-80mL链转移剂异丙醇,搅拌加热至65-75℃,将分置于两个滴液漏斗中的21mL丙烯酸单体和3-4mL 100g/L链引发剂过硫酸铵水溶液,在20min内同时开始滴加,并在2-3小时内滴完,保持回流温度反应两个小时左右得聚丙烯酸溶液;
⑵制备聚丙烯酸气相缓蚀剂:步骤⑴所制得的聚丙烯酸烧杯中加入20mL左右的丙酮,再缓慢逐滴加入与所述聚丙烯酸等摩尔量的吗啉,搅拌使其充分反应,并控制pH值为7-8,滴加完毕再搅拌20min,降温至60℃出料,最后得到淡黄色的聚丙烯酸吗啉粘稠液体,所得产物经减压旋转蒸发、蒸出溶剂后,得到的固体产品研磨得到淡黄色的聚丙烯酸吗啉固体粉末。
2.根据权利要求1所述一种聚丙烯酸类气相缓蚀剂的制备方法,其特征在于所述丙烯酸与吗啉的摩尔比为1∶(1.1~1.2)。
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109342258A (zh) * | 2018-11-27 | 2019-02-15 | 上海电力学院 | 一种热交换金属表面阻垢性能的评价方法 |
CN110790947A (zh) * | 2019-11-19 | 2020-02-14 | 南通赛博通信有限公司 | 高吸水树脂预处理用处理液及高吸水树脂预处理方法 |
CN111088497A (zh) * | 2019-12-27 | 2020-05-01 | 国网浙江平湖市供电有限公司 | 一种调湿控释型气相缓蚀剂 |
CN114808479A (zh) * | 2022-05-19 | 2022-07-29 | 福建华夏合成革有限公司 | 一种水性耳机套皮革制备方法 |
CN115522202A (zh) * | 2022-08-01 | 2022-12-27 | 杭州巨星科技股份有限公司 | 一种防锈材料及其在金属制品包装盒中的应用 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1800489A (zh) * | 2006-01-06 | 2006-07-12 | 华南理工大学 | 一种不锈钢材防护垫纸的制备方法 |
CN101323886A (zh) * | 2008-07-04 | 2008-12-17 | 陕西科技大学 | 用于高弹性皮革复鞣的丙烯酸类聚合物复鞣剂的制备方法 |
WO2010092360A1 (en) * | 2009-02-13 | 2010-08-19 | Alpha Fry Limited | Heat transfer fluid |
CN102142295A (zh) * | 2010-02-03 | 2011-08-03 | 高欣宝 | 一种高保水性膨润土降阻剂的制备方法 |
CN102168271A (zh) * | 2010-01-28 | 2011-08-31 | 艾克索防腐研究有限公司 | 汽相腐蚀抑制剂组合物、其制备方法及其用于抗腐蚀的临时保护的用途 |
WO2011126059A1 (ja) * | 2010-04-07 | 2011-10-13 | 株式会社日本触媒 | ポリ(メタ)アクリル酸系重合体水溶液およびその製造方法 |
-
2012
- 2012-02-06 CN CN 201210024779 patent/CN102534623B/zh not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1800489A (zh) * | 2006-01-06 | 2006-07-12 | 华南理工大学 | 一种不锈钢材防护垫纸的制备方法 |
CN101323886A (zh) * | 2008-07-04 | 2008-12-17 | 陕西科技大学 | 用于高弹性皮革复鞣的丙烯酸类聚合物复鞣剂的制备方法 |
WO2010092360A1 (en) * | 2009-02-13 | 2010-08-19 | Alpha Fry Limited | Heat transfer fluid |
CN102168271A (zh) * | 2010-01-28 | 2011-08-31 | 艾克索防腐研究有限公司 | 汽相腐蚀抑制剂组合物、其制备方法及其用于抗腐蚀的临时保护的用途 |
CN102142295A (zh) * | 2010-02-03 | 2011-08-03 | 高欣宝 | 一种高保水性膨润土降阻剂的制备方法 |
WO2011126059A1 (ja) * | 2010-04-07 | 2011-10-13 | 株式会社日本触媒 | ポリ(メタ)アクリル酸系重合体水溶液およびその製造方法 |
Non-Patent Citations (2)
Title |
---|
《河南科学》 20110131 李天仚等 "低分子量聚丙烯酸铵分散剂的合成研究" 第17-19页 1-2 第29卷, 第1期 * |
李天仚等: ""低分子量聚丙烯酸铵分散剂的合成研究"", 《河南科学》, vol. 29, no. 1, 31 January 2011 (2011-01-31), pages 17 - 19 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109342258A (zh) * | 2018-11-27 | 2019-02-15 | 上海电力学院 | 一种热交换金属表面阻垢性能的评价方法 |
CN110790947A (zh) * | 2019-11-19 | 2020-02-14 | 南通赛博通信有限公司 | 高吸水树脂预处理用处理液及高吸水树脂预处理方法 |
CN111088497A (zh) * | 2019-12-27 | 2020-05-01 | 国网浙江平湖市供电有限公司 | 一种调湿控释型气相缓蚀剂 |
CN114808479A (zh) * | 2022-05-19 | 2022-07-29 | 福建华夏合成革有限公司 | 一种水性耳机套皮革制备方法 |
CN115522202A (zh) * | 2022-08-01 | 2022-12-27 | 杭州巨星科技股份有限公司 | 一种防锈材料及其在金属制品包装盒中的应用 |
CN115522202B (zh) * | 2022-08-01 | 2024-03-15 | 杭州巨星科技股份有限公司 | 一种防锈材料及其在金属制品包装盒中的应用 |
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