CN107899541A - 一种用于吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法 - Google Patents
一种用于吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法。本发明以聚苯乙烯作为碳源基体，以环氧氯丙烷为改性剂，采用化学催化接枝法来实现聚苯乙烯改性；以七水合硫酸亚铁和六水合氯化铁，正辛酸为表面活性剂，采用共沉淀法制备纳米四氧化三铁；以纳米四氧化三铁、壳聚糖和1‑丁基‑3‑甲基氯化咪唑鎓为原料制备壳聚糖包覆四氧化三铁纳米复合材料；最后将壳聚糖包覆四氧化三铁与改性聚苯乙烯反应，并采用高温退火工艺将制备的基体复合材料在氮气气氛，煅烧，制备出四氧化三铁/壳聚糖‑改性聚苯乙烯基磁性碳纳米复合材料。本发明所得的材料能有效吸附六价铬离子，从而对含有六价铬离子的废水进行处理，达到排放标准，保护环境。
Description
技术领域
本发明属于环境保护技术领域，具体涉及一种用于含铬废水处理的高效磁性碳纳米复合材料的制备方法。
背景技术
随着大量工业废水被排放到生态环境中，重金属离子为水体中常见的污染物。重金属离子难以在自然界中降解，而且毒性大，可在生态系统中大量富集，并通过食物链进入人体，对人体健康造成严重危害。由于高毒性和高移动性的特点，六价铬离子被认为是最常见的有害重金属离子之一。美国环保局规定饮用水中全部铬离子的含量不能超过100 μgL-1，世界卫生组织则宣布饮用水中六价铬离子的含量不能超过50 μg L-1。因此，重金属离子废水的治理问题迫在眉睫。为了最大限度的避免重金属离子污染对生态系统造成严重影响，人们正在努力寻找高效且经济的处理重金属离子废水的新技术。由于操作费用低、吸附效率高等优点，吸附法是一种非常有应用前景的废水处理方法，可以有效吸附废水中的重金属六价铬离子。
发明内容
本发明提供一种用于有效吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法。
为了实现上述目的，本发明采用以下技术方案：
本发明提出的一种用于吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法，具体步骤如下：
（１）将七水合硫酸亚铁 （0.2-0.5 g）和六水合氯化铁（0.5-0.8 g）加入到25mL去离子水中，室温下在磁力搅拌器中搅拌至固体颗粒完全溶解，缓慢滴加0.5-3 mL正辛酸后，调节搅拌速度为500-1000 r min-1，逐滴加入氨水调节溶液的pH值为8-12，加热至60-100℃并维持0.5-3 h；反应结束后，用去离子水和95%乙醇各洗涤3次，置于30-90℃烘箱中干燥4-8 h；最后将干燥好的样品在管式炉中于200-500℃的氮气氛围中煅烧1-3 h，制备出四氧化三铁纳米颗粒；
（２）将0.1-0.5g步骤（１）得到的纳米四氧化三铁、0.1-0.5g壳聚糖和5.0-10 g 1-丁基-3-甲基氯化咪唑鎓分别加入到烧杯中，将烧杯置于电热恒温水浴锅中，加热至30-80℃，并机械搅拌0.5-3 h，最后将混合物转移至装有去离子水的烧杯中超声5-30 min，抽滤混合物溶液，得到滤饼，将滤饼用去离子水和95%乙醇各洗涤3次后，放入30-90℃真空烘箱中干燥8-15 h，制备出壳聚糖包覆的四氧化三铁纳米颗粒；
（３）利用乙酸乙酯、丙酮和环己烷混合溶剂溶解0.5-3g聚苯乙烯，将0.1-2g无水三氯化铝的3-8mL无水乙醇溶液加入到步骤（２）所得溶液中，室温下磁力搅拌10-50 min，得到混合溶液；将0.5-3mL环氧氯丙烷逐滴加入到该混合溶液中，室温下磁力搅拌10-50 min；完成聚苯乙烯的环氧基官能团接枝；
（４）将改性聚苯乙烯溶液转移至三口烧瓶中，称取0.1-2 g 四氧化三铁/壳聚糖纳米复合材料加入接枝改性聚苯乙烯溶液中并超声分散，然后在恒温水浴锅中加热至50-100℃回流0.5-3 h，控制机械搅拌速度为100-500 r min-1；反应完成后将混合溶液用无水乙醇洗涤5次，并置于30-90℃真空烘箱中干燥8-15 h；将干燥后的样品研磨成粉末状后置于管式炉中，在氮气气氛和300-800℃、5-60 min煅烧时间条件下煅烧，得到磁性碳纳米复合材料。
本发明具有以下有益效果：
本发明制备的磁性碳纳米复合材料稳定性较好，耐酸耐腐蚀性较强，再生性能良好，可以利用磁铁有效地回收再利用，经脱附后吸附效率仍保持在较高水平，大大地节约了成本。本发明采用聚苯乙烯和壳聚糖为碳源，制备出新一代可再生利用的、多功能化的磁性碳纳米复合材料，既可以实现水环境污染治理，也为聚合物纳米复合材料废弃物处理以及绿色高分子材料的有效利用提供新指导。
附图说明
图1为磁性碳纳米复合材料SEM图像，（a）为4万放大倍数，（b）为8万放大倍数。
具体实施方式
下面结合具体含铬溶液的六价铬离子吸附实验进一步说明本发明。
为提高含铬废水的六价铬离子吸附效率，本发明经过多次反复实验，研究以四氧化三铁/壳聚糖化学键合接枝改性聚苯乙烯为碳源前驱体，通过高温退火工艺制备了磁性碳纳米复合材料，通过控制高温退火工艺参数，如温度、煅烧时间等来控制磁性碳纳米复合材料的晶体结构、微观形貌和表面官能团，研究各种因素包括溶液pH值、六价铬离子初始浓度及磁性碳纳米复合材料的投加量等对六价铬离子吸附影响，采用准二级吸附动力学对其吸附过程动力学进行拟合，采用Langmuir等温吸附方程对其等温吸附过程进行拟合。该材料的场发射电子扫描显微镜图像如图1所示。
实施例 1
将1.125g 本发明制备的磁性碳纳米复合材料加入到2L的反应器中（玻璃钢材质，工作容积为1.5L，内径10cm，高26cm，呈圆柱形），向其中加入1.5L铬浓度为2mg L-1的含铬废水，处理温度为25℃，pH为3，超声处理15s，铬吸附率达77%。
实施例 2
将1.5g 本发明制备的磁性碳纳米复合材料加入到2L的反应器中（玻璃钢材质，工作容积为1.5L，内径10cm，高26cm，呈圆柱形），向其中加入1.5L铬浓度为2mg L-1的含铬废水，处理温度为25 ℃，pH为3，超声处理15s，铬吸附率达95%。用永磁体回收并经过脱附处理后，
重复上述过程，铬吸附率为94.2%。
实施例3
将1.875g 本发明制备的磁性碳纳米复合材料加入到2L的反应器中（玻璃钢材质，工作容积为1.5L，内径10cm，高26cm，呈圆柱形），向其中加入1.5L铬浓度为2mg L-1的含铬废水，处理温度为25 ℃，pH为3，超声处理15s，铬吸附率达100%。
上述对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施案例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (1)
1.一种用于吸附废水中六价铬离子的磁性碳纳米复合材料的制备方法，其特征在于具体步骤如下：
（1）将0.2-0.5 g七水合硫酸亚铁和0.5-0.8 g六水合氯化铁加入到25mL去离子水中，室温下在磁力搅拌器中搅拌至固体颗粒完全溶解，缓慢滴加0.5-3 mL正辛酸后，调节搅拌速度为500-1000 r min-1，逐滴加入氨水调节溶液的pH值为8-12，加热至60-100℃并维持0.5-3 h；反应结束后，用去离子水和95%乙醇各洗涤3次，置于30-90℃烘箱中干燥4-8 h；最后将干燥好的样品在管式炉中于200-500℃的氮气氛围中煅烧1-3 h，制备出四氧化三铁纳米颗粒；
（２）将0.1-0.5g步骤（1）得到的纳米四氧化三铁、0.1-0.5g壳聚糖和5.0-10 g 1-丁基-3-甲基氯化咪唑鎓分别加入到烧杯中，将烧杯置于电热恒温水浴锅中，加热至30-80℃，并机械搅拌0.5-3 h，最后将混合物转移至装有去离子水的烧杯中超声5-30 min，抽滤混合物溶液，得到滤饼，将滤饼用去离子水和95%乙醇各洗涤3次后，放入30-90℃真空烘箱中干燥8-15 h，制备出壳聚糖包覆的四氧化三铁纳米颗粒；
（３）利用乙酸乙酯、丙酮和环己烷混合溶剂溶解0.5-3g聚苯乙烯，将含有0.1-2g无水三氯化铝的3-8mL无水乙醇溶液加入到步骤（２）所得溶液中，室温下磁力搅拌10-50 min，得到混合溶液；将0.5-3mL环氧氯丙烷逐滴加入到该混合溶液中，室温下磁力搅拌10-50 min；完成聚苯乙烯的环氧基官能团接枝；
（４）将改性聚苯乙烯溶液转移至三口烧瓶中，称取0.1-2 g 四氧化三铁/壳聚糖纳米复合材料加入接枝改性聚苯乙烯溶液中并超声分散，然后在恒温水浴锅中加热至50-100℃回流0.5-3 h，控制机械搅拌速度为100-500 r min-1；反应完成后将混合溶液用无水乙醇洗涤5次，并置于30-90℃真空烘箱中干燥8-15 h；将干燥后的样品研磨成粉末状后置于管式炉中，在氮气气氛和300-800℃、5-60 min煅烧时间条件下煅烧，得到磁性碳纳米复合材料。
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