CN112779541A - 一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法 - Google Patents
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Abstract
本发明公开了一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，包括以下步骤：称取一定质量的生姜粉末，选用乙醇为溶剂，采用超声辅助溶剂提取法得到姜辣素提取液，将提取液过滤浓缩后，冷冻干燥，得到姜辣素粗提物，将姜辣素粗提物加入盐酸溶液中，分别配制含有不同浓度缓蚀剂的盐酸介质溶液，然后将碳钢浸入盐酸介质溶液中一段时间，分别通过失重法、电化学测试法来计算缓蚀效率，评估姜辣素粗提物作为缓蚀剂的抑制效果，结果表明姜辣素粗提物作为一种缓蚀剂，对碳钢的腐蚀具有很好的抑制作用。本发明缓蚀剂制备方法简单，实验操作步骤便捷，对生产设备要求低，缓蚀剂成本低，缓蚀效果好；评估方法科学合理，具有说服力。
Description
技术领域
本发明涉及缓蚀剂技术领域，具体涉及一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法。
背景技术
碳钢是工业上常用钢材，由于受到酸洗、油井酸化等影响，这些钢材都会受到不同程度上的腐蚀，带来了经济损失、设备损耗、环境污染等问题。为解决此类腐蚀问题，多会采取防腐手段。而在众多防腐手段中，添加缓蚀剂是最有效也是最经济实用的。目前工业上采用的最多的是含N、O、S等原子的杂环以及多重键的有机化合物，这些有机化合物虽然缓蚀效果好，但由于其成本较高，有毒性且不易降解，无法大范围的在工业上使用。在缓蚀剂制备中，多数采用失重法来评估缓蚀剂的抑制效果，并无相关专利报道其他方法。大量研究发现植物中含有天然的缓蚀成分，可以被提取出来作为绿色缓蚀剂，提取工艺简单，具有资源丰富、成本低廉、无毒无害等优点。
专利CN110863208A（李惠静，一种基于黄精多糖的碳钢酸洗缓蚀剂）公开了一种黄精多糖缓蚀剂，可防止碳钢及其制品在酸洗过程中金属或酸液消耗，该方法来源广泛，但该方法中黄精多糖的提取工艺步骤复杂，成本较高，萃取使用的溶剂易对环境造成污染。专利CN110983344A（邓书端，一种油茶果壳复配缓蚀剂及其制备方法与应用）公开了一种利用油茶果壳提取物、芳醛类化合物、阴离子表面活性剂等复配缓蚀剂的方法，可降低碳钢在酸洗过程中的腐蚀，但该方法提取与复配工艺复杂，成本较高，并且仅采用失重法说明缓蚀剂的缓蚀效果，不具有说服力。与现有技术相比，本发明制备方法更为简单便捷，对实验操作要求低，生姜更是一种常见植物，实验成本较为低廉，提取工艺简单，对环境友好，并且采用失重法和电化学方法同时评估姜辣素粗提物作为缓蚀剂对碳钢片在酸性溶液中的缓蚀效果。结果表明姜辣素粗提物作为缓蚀剂，缓蚀效率非常高，并且目前未有将姜辣素作为缓蚀剂的相关文章与专利报道。
生姜是亚洲传统药食两用植物，其根茎是日常烹饪中常用的调味品，姜的根茎、姜皮、叶均可入药。姜辣素是生姜中主要活性成分，并且大量研究证明姜辣素具有较强的抗氧化性，使其作为绿色缓蚀剂具备了理论上的可能性。因此利用生姜中姜辣素粗提物作为缓蚀剂，探究其对碳钢在酸性溶液中腐蚀的抑制效果，此类缓蚀剂对环境友好，减少工业上碳钢腐蚀所造成的经济损失，为生姜资源的开发和利用提供了新的途径。
发明内容
本发明的目的是利用生姜中姜辣素粗提物作为缓蚀剂，并通过失重法和电化学方法评估其对碳钢在酸性溶液中腐蚀的抑制效果。本发明通过采用超声辅助溶剂提取法得到姜辣素粗提物，然后将姜辣素粗提物作为缓蚀剂，加入盐酸溶液中，将碳钢分别浸泡在含有不同浓度缓蚀剂的盐酸介质溶液中，利用失重法和电化学测试法计算碳钢的缓蚀效率，评估姜辣素作为缓蚀剂的抑制效果。为了解决以上技术问题，本发明提供了如下解决方案：
1.一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，包括如下步骤：
（1）选用乙醇为溶剂，将一定质量的生姜粉末置于圆底烧瓶中，加入200～400 mL的乙醇超声30～60 min, 再加热回流1～3 h，得到姜辣素粗提液；
（2）将上述提取液过滤后，浓缩至20～40 mL，冷冻干燥后得到姜辣素粗提物；
（3）分别多次称取上述粗提物，加入1 M盐酸溶液中，配制成多种含有一定浓度缓蚀剂的盐酸介质溶液；
（4）一定温度下，将碳钢分别浸入含有不同浓度缓蚀剂的盐酸介质溶液中，浸没3～4 h；
（5）采用失重法，对上述碳钢分别在浸入前和浸入后称重，分别记为W0和W1，通过公式计算腐蚀速率和缓蚀效率；
（6）采用电化学法，分别对碳钢在含有不同浓度缓蚀剂的盐酸介质溶液中进行测试；
进一步，上述步骤（5）中，失重法的腐蚀速率和缓蚀效率的计算公式分别为：
ν=(W0-W1)/(St), 其中ν为腐蚀速率，单位g·m-2·h-1；S为钢片表面积，单位m2；t为腐蚀时间，单位h；W0、W1分别为腐蚀前和腐蚀后的质量，单位g。
η=(ν0-ν1)/ν0×100%，其中η为缓蚀效率，%；ν0和ν1分别为未含有和含有缓蚀剂的腐蚀速率，单位g·m-2·h-1。
进一步，上述步骤（6）中电化学法测试是动电位极化曲线测试和交流阻抗测试，均利用电化学工作站（CHI-660E型，上海辰华仪器有限公司）进行的；
进一步，上述步骤（6）中极化曲线扫描区间为开路电位±250 mV, 扫描速度为1mV/s，通过极化曲线计算缓蚀效率（η），计算公式为：
η=（J0-J)/J×100%，J0和J分别为碳钢在未含有和含有缓蚀剂盐酸介质溶液中的电流密度，单位mA/cm2，E为腐蚀电位，单位mV；
进一步，上述步骤（6）中，交流阻抗的（EIS）测量频率范围为1～100000 Hz，振幅为10 mV。通过交流阻抗计算缓蚀效率（η），计算公式为：
η=（Rct-Rct 0)/Rct×100%, Rct 0和Rct分别为碳钢在未含有和含有缓蚀剂盐酸介质溶液中的电荷转移电阻，通过软件Z View 3.0模拟得到，单位Ω·cm2，Rs为溶液电阻，单位Ω·cm2。
附图说明：
附图1为实施例1中碳钢在含有不同浓度缓蚀剂盐酸介质中的腐蚀速率变化曲线。
附图2为实施例1中碳钢含有不同浓度缓蚀剂盐酸介质中的缓蚀效率变化曲线。
附图3为实施例2中碳钢在含有不同浓度缓蚀剂盐酸介质溶液中的极化曲线。
附图4为实施例2中碳钢在含有不同浓度缓蚀剂盐酸介质溶液中的交流阻抗谱图。
具体实施方式：
以下结合实施例对本发明做具体的说明：
实施例1：失重法测试
（1）选用乙醇为溶剂，将10.0 g生姜粉末置于圆底烧瓶中，加入200 mL乙醇超声30min, 80℃加热回流提取2 h，得到姜辣素粗提液；
（2）将上述提取液过滤后，浓缩至20 mL，冷冻干燥后得到姜辣素粗提物；
（3）称取上述粗提物，加入1 M盐酸溶液中，分别配制成0 g/L、0.2 g/L、0.6 g/L、1.0 g/L、1.4 g/L、1.8 g/L的盐酸介质溶液；
（4）25℃下，将碳钢分别浸入上述含有不同浓度缓蚀剂的盐酸介质溶液中，浸没4h；
（5）对上述碳钢分别在浸入前和浸入后称重，通过公式计算碳钢的腐蚀速率和缓蚀效率；
通过附图1和附图2可以看到，一定温度下，随着缓蚀剂浓度的增加，碳钢的腐蚀速率逐渐下降，缓蚀效率逐渐增加，表明姜辣素粗提物是一种有效的缓蚀剂，对碳钢在盐酸中的腐蚀具有较好的抑制性能。
实施例2：电化学法测试
（1）同实施例1得到姜辣素粗提物，同样配制含有不同浓度缓蚀剂的盐酸介质溶液；
（2）利用环氧树脂对碳钢封样，留出1 cm2工作面积；
（3）将碳钢浸入含有不同浓度缓蚀剂的盐酸介质溶液中1 h, 得到稳定的开路电位；
（4）利用电化学工作站（CHI-660E型，上海辰华仪器有限公司）对碳钢分别进行动电位极化曲线测试和交流阻抗测试；
表1 碳钢在盐酸溶液中的极化参数
| 浓度 (g/L) | -E/mV | -J/(mA·cm<sup>-2</sup>) | η（%) |
| 0.2 | 0.40 | 0.00255 | 83.16 |
| 0.6 | 0.40 | 0.00126 | 91.68 |
| 1.0 | 0.40 | 0.00056 | 96.30 |
| 1.4 | 0.40 | 0.00049 | 96.76 |
| 1.8 | 0.40 | 0.00020 | 98.67 |
| 空白 | 0.38 | 0.01514 | / |
如表1所示，通过腐蚀电流密度计算得到缓蚀效率，可以看到缓蚀效率随着缓蚀剂浓度的增加而增加，与失重法所测得的趋势一致，表明姜辣素粗提物作为缓蚀剂具有良好的抑制效果；
如表2所示，通过电荷转移电阻计算得到缓蚀效率，可以看到缓蚀效率随着缓蚀剂浓度的增加而增加，与失重法、极化曲线测试结果趋势一致，再次表明姜辣素粗提物是一种有效的缓蚀剂，能够有效地抑制碳钢在盐酸介质溶液中的腐蚀作用。
表2 碳钢在盐酸溶液中的阻抗参数
| 浓度 (g/L) | R<sub>s</sub>/(Ω·cm<sup>-2</sup>) | R<sub>ct</sub>/(Ω·cm<sup>-2</sup>) | η（%) |
| 0.2 | 1.53 | 50.08 | 78.29 |
| 0.6 | 2.02 | 76.82 | 85.85 |
| 1.0 | 1.75 | 111.20 | 90.22 |
| 1.4 | 1.52 | 130.00 | 91.64 |
| 1.8 | 1.43 | 206.00 | 94.72 |
| 空白 | 1.57 | 10.87 | / |
因此，通过超声辅助溶剂提取法制备得到姜辣素粗提物，然后分别采用失重法、电化学法评估其作为缓蚀剂的效果，结果表明姜辣素粗提物对碳钢的腐蚀具有较强的抑制作用，并且其浓度越高，抑制作用越强。
Claims (6)
1.一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，包括如下步骤：
（1）选用乙醇为溶剂，将一定质量的生姜粉末置于圆底烧瓶中，加入200～400 mL的乙醇超声30～60 min, 再加热回流提取1～3 h，得到姜辣素粗提液；
（2）将上述提取液过滤后，浓缩至20～40 mL，冷冻干燥后得到姜辣素粗提物；
（3）分别多次称取上述粗提物，加入1 M盐酸溶液中，配制成多种含有一定浓度缓蚀剂的盐酸介质溶液；
（4）一定温度下，将碳钢分别浸入含有不同浓度缓蚀剂的盐酸介质溶液中，浸没3～4h；
（5）采用失重法，对上述碳钢分别在浸入前和浸入后称重，分别记为W0和W1，通过公式计算腐蚀速率和缓蚀效率；
（6）分别对碳钢在含有不同浓度缓蚀剂的盐酸介质溶液中进行电化学法测试。
2.如权利要求1所述的一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，其特征在于，步骤（1）中生姜粉末质量为10.0 g。
3.如权利要求1所述的一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，其特征在于，步骤（3）中缓蚀剂的浓度为0 g/L～2.0 g/L。
4.如权利要求1所述的一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，其特征在于，步骤（4）中温度为25℃～60℃。
5.如权利要求1所述的一种抑制碳钢腐蚀的缓蚀剂制备及其评估方法，其特征在于，步骤（6）中电化学测试方法为动电位极化曲线测试和交流阻抗测试。
6.权利要求1至6任何一项所述得到抑制碳钢腐蚀的缓蚀剂制备及其评估方法。
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