CN114807948A - 一种便捷制备含碳点缓蚀剂的酸洗液方法 - Google Patents
一种便捷制备含碳点缓蚀剂的酸洗液方法 Download PDFInfo
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Abstract
本发明公开了一种便捷制备含碳点缓蚀剂的酸洗液方法,具体步骤为:以氨基酸为碳点缓蚀剂的原材料,加入水并搅拌,使氨基酸分散于水中,得到氨基酸溶液;向所得氨基酸溶液中加入浓度不低于95%的浓硫酸,边加边搅拌均匀;将所得混合溶液在50~90℃下均匀加热20~300min,溶液中的氨基酸在浓硫酸作用下发生脱水碳化反应;将所得反应后的溶液倒入水中稀释,边倒边搅拌,所得稀释溶液即为含碳点缓蚀剂的酸洗液。本方法简单便捷,可实现规模化制备含碳点缓蚀剂的酸洗液。更重要的是,所制备的碳点掺杂有氮元素,缓蚀效果更强,在碳点缓蚀剂的保护下,酸洗液可对碳钢、低合金钢、铜等金属高效清洗的同时,不伤害金属基体。
Description
技术领域
本发明涉及功能化材料制备及应用领域,具体涉及一种便捷制备含碳点缓蚀剂的酸洗液方法。
背景技术
碳点于2004年被首次发现,被定义为具有荧光效应、尺寸一般小于10nm的碳纳米粒子。绝大多数碳点由核心和表面基团两部分组成,其中核心一般由sp2杂化石墨碳或无定形碳组成,表面基团多为含氧或含氮基团。由于具有独特的荧光可调性、优异的光稳定性、小尺寸效应、良好的生物相容性、卓越的催化性、低毒环保等优点,被广泛应用于化学传感、生物成像、催化、光电器件、植物***、润滑、防腐等领域。
碳点在防腐领域的应用起步较晚。2017年,研究人员首次探索了碳点在防腐领域的应用。具体为使用抗生素氨基水杨酸为原材料,通过水热法制备出具有高水溶性和低细胞毒性的氮掺杂碳点,作为环保型缓蚀剂用于抑制碳钢在浓度为1M的盐酸溶液中腐蚀,缓释效率高达96%。受此启发,一些研究人员制备出各类不同类型碳点,作为铜、碳钢、铝等金属的缓蚀剂,在酸溶液和氯化钠中性溶液中均展现出优异的防腐性能,最佳缓蚀效率均高于90%。目前,大量研究证明了氮掺杂碳点由于含有氮元素,可通过氮与金属元素的化学吸附作用更好的形成防护膜,保护金属基体不被酸洗液腐蚀。
基于此,文件CN111662243A公开了一种柠檬酸基功能化碳点缓蚀剂及其制备方法与应用。本发明通过将柠檬酸在去离子水存在的条件下进行水热反应,待反应液冷却后,分别加入去离子水、无水乙醇和三乙胺并搅拌,然后加入4-二甲氨基吡啶,待搅拌溶解后,加入三聚氰胺粉末并搅拌溶解,然后加热进行酰胺化反应制得一种柠檬酸基功能化碳点缓蚀剂。该碳点缓蚀剂由于酰胺化反应从而具有氮元素,具有更高效的缓蚀性能。
上述文件所制备的碳点缓蚀剂,仍然存在不环保、制备效率低、原料昂贵等缺点。另外,若将其作为酸洗液的缓蚀剂,需要将上述所制备的碳点缓蚀剂先加入酸溶液中,然后搅拌混合,才能得到含有碳点缓蚀剂的酸洗液,过程较为繁琐。
发明内容
本发明的目的是针对现有制备碳点缓蚀剂方法中存在的不环保、制备效率低、原料昂贵、不能一步得到含碳点缓蚀剂的酸洗液等问题,提供一种便捷、高效、廉价、一步制备含碳点缓蚀剂的酸洗液方法。
本发明的技术方案:
一种便捷制备含碳点缓蚀剂的酸洗液方法,步骤如下:
步骤一:以氨基酸为碳点缓蚀剂的原材料,加入水并搅拌,使氨基酸分散于水中,得到氨基酸溶液;
步骤二:向步骤一所得氨基酸溶液中加入浓度不低于95%的浓硫酸,边加边搅拌均匀,防止浓硫酸产生“暴沸现象”;
步骤三:将步骤二所得混合溶液在50~90℃下均匀加热20~300min,溶液中的氨基酸在浓硫酸作用下发生脱水碳化反应,此时溶液颜色由无色变为黄色、棕色或褐色等颜色,证明生成了新物质——碳点,由于所使用的氨基酸中含有氮元素,故所得碳点为氮掺杂碳点,具有更高效的缓蚀效果;
步骤四:将步骤三所得反应后的溶液倒入水中稀释,边倒边搅拌,防止浓硫酸产生“暴沸现象”,搅拌均匀后,所得稀释溶液即为含碳点缓蚀剂的酸洗液。
上述的一种便捷制备含碳点缓蚀剂的酸洗液方法,步骤一所述的氨基酸为色氨酸、半胱氨酸、甘氨酸、丙氨酸、精氨酸、谷氨酸中的一种或多种。
上述的一种便捷制备含碳点缓蚀剂的酸洗液方法,步骤一所述的氨基酸质量占步骤三所得稀释溶液的质量分数范围为0.3%~5%。
上述的一种便捷制备含碳点缓蚀剂的酸洗液方法,步骤二中加入浓硫酸的质量大于步骤一中所加入水的质量的4倍,以确保浓硫酸可以有效地使氨基酸发生脱水碳化反应,从而高效地生成氮掺杂碳点。
上述的一种便捷制备含碳点缓蚀剂的酸洗液方法,步骤三中稀释所用水的质量根据浓硫酸的质量分数添加,使所得稀释溶液即含碳点缓蚀剂的酸洗液中含有的硫酸的质量分数范围为5%~20%。
本发明的有益效果是:(1)环保无有害物质产生;(2)成本低且制备效率高、可一步原位制备出含碳点缓蚀剂的酸洗液;(3)适合大规模制备。
附图说明
图1为本发明的制备流程图。
图2为实施例1所制备酸洗液中的碳点缓蚀剂的透射电镜(TEM)图。
图3为实施例2所制备酸洗液中的碳点缓蚀剂的TEM图。
图中:S1-S4对应本方法步骤一至步骤四。
具体实施方式
以下是本发明的2个具体实施例,并结合附图,对本发明的技术方案作进一步的描述。实施例中所使用的谷氨酸、半胱氨酸、浓硫酸等均购买于国药集团化学试剂有限公司,为分析纯级别,直接使用不做纯化处理。
实施例1
如图1所示,一种便捷制备含碳点缓蚀剂的酸洗液方法,具体步骤如下:
步骤一:以0.4g谷氨酸为碳点缓蚀剂的原材料,加入0.8mL去离子水并搅拌,使谷氨酸分散于水中,得到谷氨酸溶液;
步骤二:向步骤一所得谷氨酸溶液中加入4mL浓度为98%的浓硫酸,边加边搅拌均匀,防止浓硫酸产生“暴沸现象”;
步骤三:将步骤二所得混合溶液在75℃下加热150min,溶液中的谷氨酸在浓硫酸作用下发生脱水碳化反应,此时溶液颜色由无色变为黄色,证明生成了新物质——碳点,由于所使用的谷氨酸中含有氮元素,故所得碳点为氮掺杂碳点,具有更高效的缓蚀效果;
步骤四:将步骤三所得反应后的溶液倒入去离子水中稀释,边倒边搅拌,防止浓硫酸产生“暴沸现象”,所用稀释水的体积为74mL,搅拌均匀后,所得稀释溶液即为含碳点缓蚀剂的酸洗液。最后所得酸洗液中浓硫酸质量分数约为5%,不再加入其他任何添加剂。
为了证明所制备的酸洗液中生成了氮掺杂碳点,对所得酸洗液进行中和(氢氧化钠溶液作中和溶液)、旋蒸、乙醇萃取、冷冻干燥等操作,得到固体产物,并对其进行TEM表征(图2),产物为平均粒径约6.8nm的近圆形黑点,确定生成了碳点,使用X射线光电子能谱进一步验证了碳点中含有N元素,因此确定生成了氮掺杂碳点。
为了证明氮掺杂碳点缓蚀剂的缓蚀效果及酸洗液的清洗效果,将所制备的含碳点缓蚀剂的酸洗液和同等浓度的浓硫酸(5%)酸洗液,用于Q235碳钢除锈实验(将相同生锈情况的1cm*1cm*0.3cm的Q235碳钢块分别浸泡于两种酸洗液3h)。结果表明,同等浓度的浓硫酸(5%)酸洗液由于不含碳点缓蚀剂,会对Q235碳钢基体造成很大的腐蚀,使得表面不平整;而实施例1所制备的含碳点缓蚀剂的酸洗液仅去除Q235碳钢表面铁锈,未对基体造成腐蚀,使得表面平整光滑。因此,证明了碳点缓蚀剂的缓蚀效果及所制备酸洗液的清洗效果。
实施例2
一种便捷制备含碳点缓蚀剂的酸洗液方法,具体步骤如下:
步骤一:以0.4g半胱氨酸为碳点缓蚀剂的原材料,加入0.8mL去离子水并搅拌,使半胱氨酸分散于水中,得到半胱氨酸溶液;
步骤二:向步骤一所得半胱氨酸溶液中加入4mL浓度为98%的浓硫酸,边加边搅拌均匀,防止浓硫酸产生“暴沸现象”;
步骤三:将步骤二所得混合溶液在70℃下加热150min,溶液中的半胱氨酸在浓硫酸作用下发生脱水碳化反应,此时溶液颜色由无色变为黄色,证明生成了新物质——碳点,由于所使用的半胱氨酸中含有氮元素,故所得碳点为氮掺杂碳点,具有更高效的缓蚀效果;
步骤四:将步骤三所得反应后的溶液倒入去离子水中稀释,边倒边搅拌,防止浓硫酸产生“暴沸现象”,所用稀释水的体积为74mL,搅拌均匀后,所得稀释溶液即为含碳点缓蚀剂的酸洗液。最后所得酸洗液中浓硫酸质量分数约为5%,不再加入其他任何添加剂。
为了证明所制备的酸洗液中生成了氮掺杂碳点,对所得酸洗液进行中和(氢氧化钠溶液作中和溶液)、旋蒸、乙醇萃取、冷冻干燥等操作,得到固体产物,并对其进行TEM表征(图3),产物为粒径10nm以下近圆形黑点,确定生成了碳点,使用X射线光电子能谱进一步验证了碳点中含有N元素,因此确定生成了氮掺杂碳点。
为了证明氮掺杂碳点缓蚀剂的缓蚀效果及酸洗液的清洗效果,将所制备的含碳点缓蚀剂的酸洗液和同等浓度的浓硫酸(5%)酸洗液,用于Q235碳钢除锈实验(将相同生锈情况的1cm*1cm*0.3cm的Q235碳钢块分别浸泡于两种酸洗液3h)。结果表明,同等浓度的浓硫酸(5%)酸洗液由于不含碳点缓蚀剂,会对Q235碳钢基体造成很大的腐蚀,使得表面不平整;而实施例2所制备的含碳点缓蚀剂的酸洗液仅去除Q235碳钢表面铁锈,未对基体造成腐蚀,使得表面平整光滑。因此,证明了碳点缓蚀剂的缓蚀效果及所制备酸洗液的清洗效果。
Claims (5)
1.一种便捷制备含碳点缓蚀剂的酸洗液方法,其特征在于,步骤如下:
步骤一:以氨基酸为碳点缓蚀剂的原材料,加入水并搅拌,使氨基酸分散于水中,得到氨基酸溶液;
步骤二:向步骤一所得氨基酸溶液中加入浓度不低于95%的浓硫酸,边加边搅拌均匀;
步骤三:将步骤二所得混合溶液在50~90℃下均匀加热20~300min,溶液中的氨基酸在浓硫酸作用下发生脱水碳化反应;
步骤四:将步骤三所得反应后的溶液倒入水中稀释,边倒边搅拌,所得稀释溶液即为含碳点缓蚀剂的酸洗液。
2.根据权利要求1所述的一种便捷制备含碳点缓蚀剂的酸洗液方法,其特征在于,步骤一所述的氨基酸为色氨酸、半胱氨酸、甘氨酸、丙氨酸、精氨酸、谷氨酸中的一种或多种。
3.根据权利要求1或2所述的一种便捷制备含碳点缓蚀剂的酸洗液方法,其特征在于,步骤一所述的氨基酸质量占步骤三所得稀释溶液的质量分数范围为0.3%~5%。
4.根据权利要求1所述的一种便捷制备含碳点缓蚀剂的酸洗液方法,其特征在于,步骤二中加入浓硫酸的质量大于步骤一中所加入水的质量的4倍。
5.根据权利要求1所述的一种便捷制备含碳点缓蚀剂的酸洗液方法,其特征在于,步骤三中稀释所用水的质量根据浓硫酸的质量分数添加,使所得稀释溶液中含有的硫酸的质量分数范围为5%~20%。
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