CN113549919B - 一种万寿菊提取物复配缓蚀剂及其制备方法与应用 - Google Patents
一种万寿菊提取物复配缓蚀剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种万寿菊提取物复配缓蚀剂及其制备方法与应用。所述的万寿菊提取物复配缓蚀剂包括万寿菊提取物0.1~1.0g/L，阳离子表面活性剂十八烷基二甲基叔铵0.1~0.2g/L，椰油酸二乙醇酰胺0.1~0.5 g/L，氯化锶0.01~0.1 g/L，余量为酸洗液。制备方法是将配方配比的各原料混合搅拌均匀得到目标物万寿菊提取物复配缓蚀剂。应用为所述的万寿菊提取物复配缓蚀剂在制备钢铁材料缓蚀剂中的应用。
Description
技术领域
本发明属于材料技术领域，具体涉及一种万寿菊提取物复配缓蚀剂及其制备方法与应用。
背景技术
万寿菊（Tagetes erecta L）为菊科万寿菊属一年生草本植物，茎直立，粗壮，具纵细条棱，分枝向上平展。叶羽状分裂；沿叶缘有少数腺体。头状花序单生；总苞杯状，顶端具齿尖；舌状花黄色或暗橙色；管状花花冠黄色。瘦果线形，基部缩小，黑色或褐色，被短微毛；冠毛有1-2个长芒和2-3个短而钝的鳞片。花期7-9月。原产墨西哥。中国各地均有分布。可生长在海拔1150米至1480米的地区，多生在路边草甸。万寿菊常于春天播种，因其花大、花期长，故常用于花坛布景。酸洗缓蚀剂大多数是针对单一酸种，单一金属的缓蚀，专一性很强，效果差异大，有的化学性质不稳定，需要现场配置，工作强度大，易造成操作失误，使得设备腐蚀事故发生的风险较大，并且大多数缓蚀剂存在价格昂贵、毒性大、污染环境等问题，因此，开发一种能解决入侵植物万寿菊入侵难题是非常必要的。
发明内容
本发明的第一目的在于提供一种万寿菊提取物复配缓蚀剂；第二目的在于提供所述的万寿菊提取物复配缓蚀剂的制备方法；第三目的在于提供所述的万寿菊提取物复配缓蚀剂的应用。
本发明的第一目的是这样实现的，所述的万寿菊提取物复配缓蚀剂包括万寿菊提取物0.1~1.0g/L，阳离子表面活性剂十八烷基二甲基叔铵0.1~0.2g/L，椰油酸二乙醇酰胺0.1~0.5 g/L，氯化锶0.01~0.1 g/L，余量为酸洗液。
本发明的第二目的是这样实现的，是将配方配比的各原料混合搅拌均匀得到目标物万寿菊提取物复配缓蚀剂。
本发明的第三目的是这样实现的，所述的万寿菊提取物复配缓蚀剂在制备钢铁材料缓蚀剂中的应用。
本发明克服了绝大多数缓蚀剂价格昂贵、毒性大、污染环境之不足，而以入侵植物万寿菊为原料制备得到万寿菊提取物，加入协同阳离子表面活性剂十八烷基二甲基叔铵0.1~0.2g/L，椰油酸二乙醇酰胺0.1~0.5 g/L，氯化锶0.01~0.1 g/L，余量为酸洗液制备得到的金属缓蚀剂存在协同增效作用。本发明所述的金属缓蚀剂具有无毒、成本低、适应性强且明显抑制了酸对金属材料的腐蚀作用，使用后无污染、使用安全、方便。
具体实施方式
下面结合实施例对本发明作进一步的说明，但不以任何方式对本发明加以限制，基于本发明教导所作的任何变换或替换，均属于本发明的保护范围。
本发明所述的万寿菊提取物复配缓蚀剂包括万寿菊提取物0.1~1.0g/L，阳离子表面活性剂十八烷基二甲基叔铵0.1~0.2g/L，椰油酸二乙醇酰胺0.1~0.5 g/L，氯化锶0.01~0.1 g/L，余量为酸洗液。
所述的万寿菊提取物是以入侵植物万寿菊为原料，经前处理、提取、浓缩、萃取和后处理步骤制备得到，具体包括：
A、前处理：将万寿菊干燥粉碎过筛得到万寿菊粉a；
B、提取：将万寿菊粉a中加入万寿菊粉体积20~40倍的乙醇溶液在5~35℃下浸泡2~4h得到物料b；将物料b于温度50~80℃水浴回流提取2~6h经抽滤得到提取液c；
C、浓缩：将提取液c浓缩至提取液c体积的1/2~1/3得到浓缩液d；
D、萃取：将浓缩液d中加入浓缩液d体积2~5倍的石油醚，充分震荡后静置12~48h，得到石油醚层e和下层提取液f，石油醚层e进行回收，下层提取液f中再次加入下层提取液f体积2~3倍的石油醚，充分震荡后静置分层，每隔10~30min换一次石油醚，直至石油醚层无色得到提取液g；
E、后处理：将提取液g经蒸发、干燥得到目标物万寿菊提取物。
A步骤所述的干燥包括风干和恒温干燥步骤，具体是将万寿菊风干后放于鼓风烘箱中，于50~70℃恒温干燥48~60h。
A步骤中所述的万寿菊粉a的粒度为300~1000μm。
B步骤中所述的乙醇溶液的体积百分浓度为20~80%。
E步骤中所述的蒸发是采取旋转蒸发。
E步骤中所述的干燥是在温度50~70℃下干燥12~24h。
本发明所述的万寿菊提取物复配缓蚀剂的制备方法，是将配方配比的各原料混合搅拌均匀得到目标物万寿菊提取物复配缓蚀剂。
本发明所述的万寿菊提取物复配缓蚀剂的应用为所述的万寿菊提取物复配缓蚀剂在制备钢铁材料缓蚀剂中的应用。
所述的钢铁材料为冷轧钢。
本发明所述的万寿菊提取物的制备方法具体操作如下：
A、前处理：收集万寿菊后，风干后放于鼓风烘箱中，于60℃恒温干燥48 ~ 60 h，取出自然冷却至室温后粉碎，粒径为300~1000 μm的万寿菊粉；
B、提取：将万寿菊粉加浓度为20~80%乙醇溶液室温（5 ~ 35℃）浸泡2~4 h，固液比1：20 ~ 1：40，然后在50~80℃水浴回流提取2~6 h；
C、浓缩：将回流得到的乙醇提取液真空抽滤，以除去其中含有的万寿菊残渣粉末，然后取其在旋转蒸发仪上40~80℃把溶液旋转蒸发浓缩至1/2~1/3体积；
D、萃取：将浓缩后的乙醇提取液中加入体积2~5倍的石油醚，充分震荡后静置12~48 h，将上层的石油醚与下层的提取液分开，回收上层液，下层液体再次加入分液漏斗中并加体积2~3倍石油醚，充分震荡静置分层，每隔10~30分钟换一次石油醚，直到上层液体到无色为止；
E、后处理：将萃取后的下层液进行旋转蒸发，蒸到40~60ml，蒸发过的液体放到蒸发皿中，置于鼓风干燥箱中于50~70℃干燥12~24h，用结晶铲铲下固体，即为目标万寿菊提取物。
下面以具体实施案例对本发明做进一步说明：
实施例1
万寿菊提取物的制备
A、前处理：收集万寿菊后，风干后放于鼓风烘箱中，于60℃ ~ 70℃恒温干燥60 ~72 h，取出自然冷却至室温后粉碎，粒径为150~2000 μm的万寿菊粉；
B、提取：将万寿菊粉加浓度为10~70%乙醇溶液室温（5~35℃）浸泡2~6h，固液比1:25~50，然后在60~85℃水浴回流提取3~9 h；
C、浓缩：将回流得到的乙醇提取液真空抽滤，以除去其中含有的万寿菊残渣粉末，然后取其在旋转蒸发仪上45~75℃把溶液旋转蒸发浓缩至1/4~1/2体积；
D、萃取：将浓缩后的乙醇提取液中加入体积2~6倍的石油醚，充分震荡后静置15~60 h，将上层的石油醚与下层的提取液分开，回收上层液，下层液体再次加入分液漏斗中并加体积2~5倍石油醚，充分震荡静置分层，每隔20~40分钟换一次石油醚，直到上层液体到无色为止；
E、后处理：将萃取后的下层液进行旋转蒸发，蒸到40~60ml，蒸发过的液体放到蒸发皿中，置于鼓风干燥箱中于50~70℃干燥12~24h，用结晶铲铲下固体，即为目标万寿菊提取物。
实施例2
一种万寿菊复提取物配金属缓蚀剂的制备
取实施例1万寿菊提取物0.10 g、十二烷基二甲基叔铵0.2 g、椰油酸二乙醇酰胺0.5g、氯化锶0.1g，加入体积为1 L的浓度0.5~5.0 mol/L的盐酸洗液，搅拌均匀即得到目标物万寿菊复配缓蚀剂。
实施例3
一种万寿菊复配金属缓蚀剂的制备
取实施例1万寿菊提取物1.0 g、十二烷基二甲基叔铵0.2 g、椰油酸二乙醇酰胺0.3 g、氯化锶 0.5g，加入体积为1 L的浓度0.5~5.0 mol/L的硫酸洗液，搅拌均匀即得到目标物万寿菊复配缓蚀剂。
实施例4
一种万寿菊复配金属缓蚀剂的制备
取实施例1万寿菊提取物0.8 g、十二烷基二甲基叔铵 0.2 g、两性表面活性剂月桂酰胺丙基羟磺基甜菜碱0.5 g、非离子表面活性剂OP-10 0.1 g，加入体积为1 L的浓度0.5~10.0 mol/L的磷酸洗液，搅拌均匀即得到目标物万寿菊复配缓蚀剂。
试验例1
钢铁材料的酸洗
钢铁材料选择为冷轧钢片，将实施例2复配好的缓蚀剂注入,混合均匀，缓蚀性能在不同温度（20 ~ 50℃）不同腐蚀浸泡时间（6 ~156 h）均能在96%以上。表1为1.0 mol/LHCl试验数据，方法为失重法。
表1 万寿菊复配缓蚀剂对冷轧钢在1.0 mol/L HCl中的缓蚀率
。
试验例2
钢铁材料的酸洗
钢铁材料选择为冷轧钢片，将实施例3复配好的缓蚀剂注入,混合均匀，缓蚀性能在不同温度（20 ~ 50℃）不同腐蚀浸泡时间（6 ~48 h）均能在93%以上。表2为3.0 mol/LHCl试验数据，方法为失重法。
表2 万寿菊复配缓蚀剂对冷轧钢在3.0 mol/L HCl中的缓蚀率
。
试验例3
钢铁材料的酸洗
钢铁材料选择为冷轧钢片，将实施例3复配好的缓蚀剂注入,混合均匀，缓蚀性能在不同温度（20 ~ 50℃）不同腐蚀浸泡时间（6 ~96 h）均能在95%以上。表3为1.0 mol/LH2SO4试验数据，方法为失重法。
表3 万寿菊复配缓蚀剂对冷轧钢在1.0 mol/L H2SO4中的缓蚀率
。
试验例4
钢铁材料的酸洗
钢铁材料选择为冷轧钢片，将实施例4复配好的缓蚀剂注入,混合均匀，缓蚀性能在不同温度（20 ~ 50℃）不同腐蚀浸泡时间（6 ~120 h）均能在96%以上。表4为1.0 mol/LH3PO4试验数据，方法为失重法。
表4 万寿菊复配缓蚀剂对冷轧钢在1.0 mol/L H3PO4中的缓蚀率
。
试验例5
钢铁材料的酸洗
钢铁材料选择为冷轧钢片，将实施例4复配好的缓蚀剂注入,混合均匀，缓蚀性能在不同温度（20 ~ 50℃）不同腐蚀浸泡时间（6 ~120 h）均能在91%以上。表5为9.0 mol/LH3PO4试验数据，方法为失重法。
表5 万寿菊复配缓蚀剂对冷轧钢在9.0 mol/L H3PO4中的缓蚀率
。
Claims (9)
1.一种万寿菊提取物复配缓蚀剂，其特征在于所述的万寿菊提取物复配缓蚀剂包括万寿菊提取物0.1~1.0g/L，阳离子表面活性剂十八烷基二甲基叔铵0.1~0.2g/L，椰油酸二乙醇酰胺0.1~0.5g/L，氯化锶0.01~0.1g/L，余量为酸洗液；所述的万寿菊提取物是以入侵植物万寿菊为原料，经前处理、提取、浓缩、萃取和后处理步骤制备得到，具体包括：
A、前处理：将万寿菊干燥粉碎过筛得到万寿菊粉a；
B、提取：将万寿菊粉a中加入万寿菊粉体积20~40倍的乙醇溶液在5~35℃下浸泡2~4h得到物料b；将物料b于温度50~80℃水浴回流提取2~6h经抽滤得到提取液c；
C、浓缩：将提取液c浓缩至提取液c体积的1/2~1/3得到浓缩液d；
D、萃取：将浓缩液d中加入浓缩液d体积2~5倍的石油醚，充分震荡后静置12~48h，得到石油醚层e和下层提取液f，石油醚层e进行回收，下层提取液f中再次加入下层提取液f体积2~3倍的石油醚，充分震荡后静置分层，每隔10~30min换一次石油醚，直至石油醚层无色得到提取液g；
E、后处理：将提取液g经蒸发、干燥得到目标物万寿菊提取物。
2.根据权利要求1所述的万寿菊提取物复配缓蚀剂，其特征在于A步骤所述的干燥包括风干和恒温干燥步骤，具体是将万寿菊风干后放于鼓风烘箱中，于50~70℃恒温干燥48~60h。
3.根据权利要求1所述的万寿菊提取物复配缓蚀剂，其特征在于A步骤中所述的万寿菊粉a的粒度为300~1000μm。
4.根据权利要求1所述的万寿菊提取物复配缓蚀剂，其特征在于B步骤中所述的乙醇溶液的体积百分浓度为20~80%。
5.根据权利要求1所述的万寿菊提取物复配缓蚀剂，其特征在于E步骤中所述的蒸发是采取旋转蒸发。
6.根据权利要求1所述的万寿菊提取物复配缓蚀剂，其特征在于E步骤中所述的干燥是在温度50~70℃下干燥12~24h。
7.一种权利要求1~6任一所述的万寿菊提取物复配缓蚀剂的制备方法，其特征在于是将配方配比的各原料混合搅拌均匀得到目标物万寿菊提取物复配缓蚀剂。
8.一种权利要求1~6任一所述的万寿菊提取物复配缓蚀剂的应用，其特征在于所述的万寿菊提取物复配缓蚀剂在制备钢铁材料缓蚀剂中的应用。
9.根据权利要求8所述的万寿菊提取物复配缓蚀剂的应用，其特征在于所述的钢铁材料为冷轧钢。
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