CN108355615B - 一种离子液体改性的玉米芯基材料的制备方法及其在降解土壤农药残留中的应用 - Google Patents
一种离子液体改性的玉米芯基材料的制备方法及其在降解土壤农药残留中的应用 Download PDFInfo
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Abstract
本发明涉及一种离子液体改性的玉米芯基材料的制备方法及其在降解土壤农药残留中的应用，本发明通过使用离子液体和巯基乙酸处理玉米芯得到一种对土壤中农药残留具有强清除作用的新型玉米芯基材料。该材料有望被开发作为环境修复剂，尤其是在清除有机氯农药或氨基甲酸酯类农药残留方面，清除率达90％以上。
Description
技术领域
本发明属于材料及环境保护领域，具体涉及一种离子液体改性的玉米芯基材料的制备方法及其在降解土壤农药残留中的应用。
背景技术
玉米芯是一种年产量很大的农业副产物，我国年产玉米量一亿多吨，副产物玉米芯约二万吨，每年都有大量玉米芯被丢弃，或作燃料，造成很大浪费。玉米芯表面有很多活性官能团，如羟基、羧基、氨基等，这些官能团可以与重金属离子、有机物中的活性基团发生离子交换或化学吸附。但原玉米芯对重金属及有机物的吸附容量不高，为了提高玉米芯对环境(例如水、土壤中)重金属、有机物的清除率，本发明提供一种能高效清除环境中重金属和农药残留的离子液体与巯基乙酸改性的玉米芯基材料。
发明内容
本发明提供一种玉米芯基材料，其特征在于所述玉米芯基材料的制备方法包括如下步骤：
(1)将玉米芯清洗去杂、烘干至恒重，粉碎得物料；
(2)于60-70℃下将离子液体与步骤(1)得到的物料混匀，保温2-3小时后加入巯基乙酸，升温至85-90℃，保温4-5小时后加水、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气或惰性气体保护下，于450-550℃保温1-2 小时后即得所述玉米芯基材料。
步骤(1)所述的粉碎优选粉碎至40-60目；
步骤(2)中离子液体、物料、巯基乙酸的质量比为15-25：10：0.3-0.5，优选为15-20：10：0.3-0.5；
步骤(2)中所述水优选为去离子水，其用量为离子液体质量的0.5-1.0倍；所述离子液体选自1-烯丙基-3-甲基咪唑卤盐，优选1-烯丙基-3-甲基咪唑氯盐。
本发明的另一实施方案提供上述玉米芯基材料的制备方法，其特征在于包括如下步骤：
(1)将玉米芯清洗去杂、烘干至恒重，粉碎得物料；
(2)于60-70℃下将离子液体与步骤(1)得到的物料混匀，保温2-3小时后加入巯基乙酸，升温至85-90℃，保温4-5小时后加水、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气或惰性气体保护下，于450-550℃保温1-2 小时后即得所述玉米芯基材料。
步骤(1)所述的粉碎优选粉碎至40-60目；
步骤(2)中离子液体、物料、巯基乙酸的质量比为15-25：10：0.3-0.5，优选为15-20：10：0.3-0.5；
步骤(2)中所述水优选为去离子水，其用量为离子液体质量的0.5-1.0倍；所述离子液体选自1-烯丙基-3-甲基咪唑卤盐，优选1-烯丙基-3-甲基咪唑氯盐。
本发明的另一实施方案提供上述玉米芯基材料在环境修复中的应用。
本发明的另一实施方案提供上述玉米芯基材料在清除土壤、水中重金属方面的应用。所述重金属优选六价铬。
本发明的另一实施方案提供上述玉米芯基材料在去除农药残留中的应用。所述农药优选有机氯农药或氨基甲酸酯类农药。有机氯农药优选氯丹、毒杀酚，氨基甲酸酯类农药优选速灭威、西维因。
与现有技术相比，本发明的优点在于：本发明通过使用离子液体和巯基乙酸处理玉米芯得到一种对重金属及农药具有强清除作用的新型玉米芯基材料。该材料有望被开发作为环境修复剂，尤其是在清除重金属及农药残留方面。
附图说明
图1为产品A的SEM图；
图2为产品A-E对水中六价铬的清除效果图。
具体实施方式
为了便于对本发明的进一步理解，下面提供的实施例对其做了更详细的说明。但是这些实施例仅供更好的理解发明而并非用来限定本发明的范围或实施原则，本发明的实施方式不限于以下内容。
实施例1
(1)将玉米芯清洗去杂、烘干至恒重，粉碎至40-60目得物料(10kg)；
(2)于60℃下将1-烯丙基-3-甲基咪唑氯盐(20kg)与步骤(1)得到的物料(10kg)混匀，保温2小时后加入巯基乙酸(300g)，升温至85-90℃，保温 5小时后加去离子水(10kg)、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气下，于450℃保温2h后即得所述玉米芯基材料(以下简称产品A)。
实施例2
(1)将玉米芯清洗去杂、烘干至恒重，粉碎至40-60目得物料(6kg)；
(2)于70℃下将1-烯丙基-3-甲基咪唑氯盐(9kg)与步骤(1)得到的物料(6kg)混匀，保温3小时后加入巯基乙酸(300g)，升温至85-90℃，保温4 小时后加水(9kg)、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氩气下，于550℃保温1h后即得所述玉米芯基材料(以下简称产品B)。
实施例3
(1)将玉米芯清洗去杂、烘干至恒重，粉碎至40-60目得物料(10kg)；
(2)于60℃下将1-烯丙基-3-甲基咪唑氯盐(20kg)与步骤(1)得到的物料(10kg)混匀，保温2小时后加入乙酸(300g)，升温至85-90℃，保温5小时后加去离子水(10kg)、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气下，于450℃保温2h后即得玉米芯基材料(以下简称产品C)。
实施例4
(1)将玉米芯清洗去杂、烘干至恒重，粉碎至40-60目得物料(10kg)；
(2)于60℃下将1-烯丙基-3-甲基咪唑氯盐(20kg)与步骤(1)得到的物料(10kg)混匀，保温2小时后，升温至85-90℃，保温5小时后加去离子水(10 kg)、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气下，于450℃保温2h后即得玉米芯基材料(以下简称产品D)。
实施例5
(1)将玉米芯清洗去杂、烘干至恒重，粉碎至40-60目得物料(10kg)；
(2)步骤(1)得到的物料(10kg)加入巯基乙酸(300g)混匀，升温至85-90℃，保温5小时后加去离子水(10kg)、冷却至室温，过滤，水洗至中性，得沉淀；
(3)步骤(2)得到的沉淀在氮气下，于450℃保温2h后即得玉米芯基材料(以下简称产品E)。
实施例6重金属清除实验
(1)水中六价铬清除实验
各取100mL六价铬标准溶液(20mg/L)，分别加入15mg产品A、B、C、 D、E，搅拌反应100min；实验结果表明本发明产品A、B对六价铬吸附清除效果远优于产品C-E(图2)。
(2)土壤中铅清除实验
各取100g含铅的土壤样本(每克土壤含铅2.5mg)，分别加入6mg产品A、 C、E，加水混匀使之成泥浆状，吸附8小时后，再分别补加6mg相应的产品A、 C、E，混匀，继续吸附6小时后检测，结果表明产品A对土壤样本中铅的清除率达79.6％，产品C对土壤样本中铅的清除率为36.2％，产品E对土壤样本中铅的清除率低于10％。
实施例7土壤中农药残留的降解试验
土壤样品选择：样品1：氯丹、毒杀酚的含量均为500mg/kg；样品2：速灭威、西维因的含量均为500mg/kg。
实验方法：各取5份10kg样品1和2，分别加入产品A-E(各1.5g)，混合均匀，保证含水量在20％-30％，36小时后，再分别各自补加相应的产品A-E(各 1.0g)，混合均匀后，36小时后，检测土壤中农药的含量，结果见下表。
Claims (2)
1.一种玉米芯基材料在去除农药残留中的应用，其特征在于所述农药选自氨基甲酸酯类农药，所述玉米芯基材料的制备方法包括如下步骤：
（1）将玉米芯清洗去杂、烘干至恒重，粉碎得物料；
（2）于60-70℃ 下将离子液体与步骤（1）得到的物料混匀，保温2-3小时后加入巯基乙酸，升温至85-90℃ ，保温4-5小时后加水、冷却至室温，过滤，水洗至中性，得沉淀；
（3）步骤（2）得到的沉淀在惰性气体保护下，于450-550℃保温1-2小时后即得所述玉米芯基材料；
步骤（1）所述的粉碎为粉碎至40-60目；
步骤（2）中离子液体、物料、巯基乙酸的质量比为15-25：10：0.3-0.5；所述水为去离子水，其用量为离子液体质量的0.5-1.0倍；所述离子液体选自1-烯丙基-3-甲基咪唑氯盐。
2.权利要求1所述的应用，其特征在于所述氨基甲酸酯类农药选自速灭威、西维因。
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| CN107098426A (zh) * | 2017-05-18 | 2017-08-29 | 付主枝 | 一种低碳环保降解染料废水的方法 |
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