CN106732376B - 一种用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法 - Google Patents
一种用于含铬废水处理的高效磁性碳纳米纤维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含铬废水处理的高效磁性碳纳米复合材料的制备方法。本发明结合静电纺丝技术与高温煅烧技术，制备出一种用于含铬废水处理的高效磁性碳纳米纤维复合材料，能够快速而且高效地处理含铬废水，达到含铬废水无害化，保护环境，节约水资源的目的，所制备的磁性碳纳米纤维复合材料可以利用磁性有效地回收再利用，经脱附后吸附效率仍保持在较高水平，节约了成本。首先用0.5‑1.5ml/g聚苯乙烯的环氧氯丙烷作为接枝剂，采用0.5‑2g/g聚苯乙烯的氧化铝或者三氯化铝作为催化剂，对聚苯乙烯进行接枝改性，然后利用静电纺丝技术制备改性聚苯乙烯纤维，纤维直径0.5‑2微米。经过浓度为3‑10%的九水硝酸铁/无水乙醇溶液完全浸润，30‑60℃烘箱干燥至完全后，冷冻干燥10‑20小时后400‑600℃煅烧0‑3小时，得到用于含铬废水处理的高效磁性碳纳米纤维复合材料。
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纤维复合材料的制备方法。
背景技术
水是生命之源，是人类赖以生存和发展的物质基础。目前在我国，约有82%的江河湖泊受到了不同程度的污染，其中难降解有机污染物和重金属离子的污染，已经对人类的生存环境构成了严重威胁。含铬废水是其中污染性和对人体危害性巨大的一类废水。铬及其化台物在工业上应用广泛，冶金、化工、矿物工程、电镀、颜料、制药、轻工纺织、铬盐及铬化物的生产等一系列行业，都会产生大量的含铬废水。铬化物可以通过消化道、呼吸道、皮肤和粘膜侵人人体，主要积聚在肝、肾、内分泌系统和肺部。毒理作用是影响体内物质氧化、还原和水解过程，与核酸、核蛋白结合影响组织中的磷含量。并且铬化合物具有致癌作用。如何高效地对含铬废水进行净化处理成为研究学者们密切关注的一个问题。吸附法因其操作费用低、去除效率高等优点，成为一种非常有前景的废水处理方法，可以有效地去除废水中的重金属离子。其他用于废水中污染物去除的方法，如膜分离法、氧化还原法、光催化降解法等都有各自的局限性。如膜分离法是一种较方便的处理重金属的方法，但是操作费用相对较高；氧化还原法、光催化降解法等处理过程有的过于复杂、处理费用普遍偏高、氧化剂消耗大，碳酸根离子及悬浮固体对反应有干扰。普通的吸附材料如由椰子树、木质素以及焦炭制备的活性炭已广泛用作吸附剂去除水中难降解重金属污染物，但这些材料的吸附容量和吸附速率极其有限。
发明内容
本发明要解决普通吸附材料的吸附速率极其有限的问题，提供一种用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法。
为了实现上述目的，本发明采用一下技术方案：
一种用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，具体步骤如下：
使用改性剂和催化剂对聚苯乙烯进行接枝改性，利用静电纺丝技术制备改性聚苯乙烯纤维，控制改性聚苯乙烯纤维直径在0.2-2微米之间。经过浓度为3-10%的九水硝酸铁/无水乙醇溶液完全浸润，30-60℃烘箱干燥至完全后，冷冻干燥10-20小时后，在400-600℃温度下煅烧0.1-3小时；即得用于含铬废水处理的高效磁性碳纳米纤维复合材料。
本发明中，所述聚苯乙烯接枝改性采用的改性剂为环氧氯丙烷，每克聚苯乙烯中加入0.5-1.5ml的环氧氯丙烷，催化剂为氧化铝或者三氯化铝，每克聚苯乙烯中加入0.5-2g的氧化铝或者三氯化铝。
本发明中，所述改性聚苯乙烯纤维直径为0.8-1.5微米。
本发明中，所述九水硝酸铁/无水乙醇溶液浓度为4-7%。
本发明中，所述的烘箱干燥温度为30-40℃。
本发明中，所述的冷冻干燥时间为12-18小时。
本发明中，所述的煅烧温度为350-550℃。
本发明中，所述的煅烧时间为0.5-3小时。
本发明具有以下有益效果：
本发明结合静电纺丝技术与高温煅烧技术，制备出一种用于含铬废水处理的高效磁性碳纳米纤维复合材料，能够快速而且高效地处理含铬废水，达到含铬废水无害化，保护环境，节约水资源的目的.而且，所制备的磁性碳纳米纤维复合材料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。
附图说明
图１为实施例１的磁性碳纳米复合材料SEM图像，(a) 为相同图样，50000放大倍数，(b)为100000放大倍数。
具体实施方式
下面结合具体含铬溶液的铬去除实验进一步说明本发明。
为提高含铬废水的铬去除速率，本发明经过多次反复实验，发现采用下述发明，结合静电纺丝技术与高温煅烧技术，制备出一种用于含铬废水处理的磁性碳纳米纤维复合材料，能够快速而且高效地处理含铬废水。
实施例１：
本发明探索了不同纤维直径，不同九水硝酸铁/无水乙醇溶液浓度，不同干燥方式，不同煅烧温度以及不同煅烧时间对铬去除效率的影响，通过实验发现，本发明首先采用改性剂和催化剂对聚苯乙烯进行接枝改性，所述聚苯乙烯接枝改性采用的改性剂为环氧氯丙烷，每克聚苯乙烯中加入0.5-1.5ml的环氧氯丙烷，催化剂为氧化铝或者三氯化铝，每克聚苯乙烯中加入0.5-2g的氧化铝或者三氯化铝。然后利用静电纺丝技术制备改性聚苯乙烯纤维，控制纤维直径0.8-1.5微米。经过浓度为4-7%的九水硝酸铁/无水乙醇溶液完全浸润，30-40℃烘箱干燥至完全后，冷冻干燥12-18小时后350-550℃煅烧0.5-3小时，得到用于高效处理含铬废水的磁性碳纳米纤维复合材料，该材料的场发射电子扫描显微镜图像如图1所示。
实施例２
将1.125 g 实施例１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1.5 L，内径10 cm，高26 cm，呈圆柱形），向其中加入1.5L铬浓度为2mg/L的含铬废水，处理温度为25℃，pH为3，超声处理15s，铬去除率达77%。
实施例３
将1.5 g实施例１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1.5 L，内径10 cm，高26 cm，呈圆柱形），向其中加入1.5L铬浓度为2mg/L的含铬废水，处理温度为25℃，pH为3，超声处理15s，铬去除率达95%。用永磁体回收并经过脱附处理后，重复上述过程，铬去除率为94.2%。
实施例４
将1.875 g实施例１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1.5 L，内径10 cm，高26 cm，呈圆柱形），向其中加入1.5L铬浓度为2mg/L的含铬废水，处理温度为25℃，pH为3，超声处理15s，铬去除率达100%。
上述的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 (7)
1.一种用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于具体步骤如下：
使用改性剂和催化剂对聚苯乙烯进行接枝改性，利用静电纺丝技术制备改性聚苯乙烯纤维，控制改性聚苯乙烯纤维直径在0.2-2微米之间；经过浓度为3-10%的九水硝酸铁/无水乙醇溶液完全浸润，30-60℃烘箱干燥至完全后，冷冻干燥10-20小时后，在400-600℃温度下煅烧0.1-3小时；即得用于含铬废水处理的高效磁性碳纳米纤维复合材料；所述聚苯乙烯接枝改性采用的改性剂为环氧氯丙烷，每克聚苯乙烯中加入0.5-1.5ml的环氧氯丙烷，催化剂为氧化铝或者三氯化铝，每克聚苯乙烯中加入0.5-2g的氧化铝或者三氯化铝。
2.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所得改性聚苯乙烯纤维直径为0.8-1.5微米。
3.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所述九水硝酸铁/无水乙醇溶液浓度为4-7%。
4.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所述的烘箱干燥温度为30-40℃。
5.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所述的冷冻干燥时间为12-18小时。
6.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所述的煅烧温度为350-550℃。
7.根据权利要求1所述的用于含铬废水处理的高效磁性碳纳米纤维复合材料的制备方法，其特征在于：所述的煅烧时间为0.5-3小时。
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