CN108212127B - 一种功能纳米复合水凝胶的制备方法及应用 - Google Patents

一种功能纳米复合水凝胶的制备方法及应用 Download PDF

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CN108212127B
CN108212127B CN201810047197.2A CN201810047197A CN108212127B CN 108212127 B CN108212127 B CN 108212127B CN 201810047197 A CN201810047197 A CN 201810047197A CN 108212127 B CN108212127 B CN 108212127B
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许明
张璐璐
操家顺
薛朝霞
方芳
李超
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Abstract

本发明公开了一种功能纳米复合水凝胶的制备方法及其应用。本发明利用Fe3O4纳米颗粒,少量氧化石墨烯(RGO)和聚丙烯酰胺(PAM)，通过两步化学合成方法获得功能纳米复合水凝胶材料。其制备过程如下：将RGO‑乙醇溶液与乙腈在超声波浴中混合，依次加入氨水和乙酰丙酮铁/乙醇溶液，搅拌，静置后制得Fe3O4/RGO纳米复合材料；将复合材料洗涤离心分散，再加入硝酸钙、PAM单体、一溴乙酸和过硫酸铵，经脱气后干燥，得到Fe3O4/RGO/PAM水凝胶。本发明制备的功能纳米复合水凝胶材料具有机械强度高,高光芬顿活性，吸附性能好的优点。

Description

一种功能纳米复合水凝胶的制备方法及应用
技术领域
本发明属于环保材料和水处理领域，涉及一种功能纳米复合水凝胶材料的方法及其在高效降解有机污染物的应用。
背景技术
电解、电镀、农药、医药、涂料、造纸、印染、纺织等化工行业对生态环境造成了很大的危害，因为工业废水中常含有有机污染物，难以被自然降解。一些传统的方法，如Fenton反应、生物处理、膜技术、萃取、电渗析过程等都对有机污染物有一定的处理效果。聚合物水凝胶是在药物递送和组织中具有广泛潜在应用的典型的多用途的软材料，可以释放矩阵的药物，作为细胞调节物质，以及重金属的吸附。水凝胶的网络结构提供的3D环境具有高保水性，可调节机械性能和营养物质，在环境中有很大的应用潜力。
发明内容
发明目的：为解决现有技术中存在的技术问题，本发明提出了一种功能纳米复合水凝胶的制备方法，通过利用Fe3O4纳米颗粒、少量氧化石墨烯(RGO)和聚丙烯酰胺(PAM)，采用两步化学合成方法制得纳米复合水凝胶，并将制备得到的水凝胶材料用于降解有机污染物。
为实现上述技术目的，本发明提供的纳米复合水凝胶材料的制备方法包括如下步骤：
(1)将氧化石墨烯的醇溶液与乙腈混合得到悬浮液，在室温下向悬浮液中加入NH3·H2O搅拌；优选地，将氧化石墨烯的醇溶液与乙腈混合90～100分钟，加入NH3·H2O后搅拌20～30min；
(2)向上述溶液中缓慢加入乙酰丙酮铁的醇溶液，搅拌；优选地，搅拌30～40min；
(3)将步骤(2)得到的悬浮液在50-80℃下维持10-12h，使无定形Fe3O4纳米颗粒预生长在氧化石墨烯表面上；
(4)将步骤(3)得到的材料用乙醇洗涤后，离心，将得到的沉淀物重新分散在10毫升蒸馏水中，得到氧化石墨烯分散系；
(5)将Ca(NO3)2、丙烯酰胺单体、一溴乙酸和过硫酸铵溶解在前述氧化石墨烯分散系中；
(6)将步骤(5)得到的混合物脱气20-30分钟后，放入容器中，在烘箱中干燥，得到Fe3O4/氧化石墨烯/PAM水凝胶。
其中，步骤(1)中，氧化石墨烯的醇溶液、NH3·H2O、乙酰丙酮铁的醇溶液的浓度分别为5-10mg/ml、25-30wt％和0.3-0.5mol/L；氧化石墨烯的醇溶液、乙腈、NH3·H2O、乙酰丙酮铁的醇溶液的体积分别为100-110ml、20-30ml、0.1-0.5ml和10-20mL。
步骤(1)或(2)中的醇溶液为乙醇溶液、甲醇溶液或异丙醇溶液中的任意一种。
步骤(2)乙酰丙酮铁的醇溶液的加入速度不超过30ml/min。
步骤(5)中Ca(NO3)2、丙烯酰胺单体、一溴乙酸和过硫酸铵的量分别为5-10mmol、30-40mmol、0.01-0.02mmol和30-35mmol。
步骤(5)中，溶解操作需在N2气保护和冰浴下。
步骤(6)中，烘箱的条件为在50-80℃烘箱中烘2-5小时。
将步骤(6)制备的水凝胶在-60℃、0.12mbar冷冻干燥10-15小时以利储存。
通过上述制备方法制备得到的功能纳米复合水凝胶也在本发明的保护范围之内。
本发明进一步提出了上述功能纳米复合水凝胶在降解有机污染物中的应用。
在一种实施例中，所述有机污染物为有机染料。
有益效果：与现有技术相比，本发明制备出的功能纳米复合水凝胶材料，可以实现高效降解有机污染物，制备简单，吸附效率高。
附图说明
图1为实施例1制备的3种材料降解速率图；
图2为不同pH条件下材料的降解速率。
具体实施方式
根据下述实施例，可以更好地理解本发明。
其中，光-芬顿反应试验采用如下步骤进行：
配制20mg/l的有机染料罗丹明B(RhB)溶液，并取50ml于反应器中，向反应溶液中加入1.0mL H2O2。再加入制得的水凝胶，并用氙灯照射反应器，启动反应。以不同的时间间隔从反应池中取出一定量溶液。经过充分的显色，用紫外可见分光光度计在550nm测量RhB溶液的吸光度。
降解率：β＝[(A0-A)/A0]×100％
式中：A0表示RhB的起始吸光度，A表示不同时刻RhB的吸光度。
实施例1
100mLRGO的乙醇溶液(5mg/ml)与25mL乙腈在超声波浴中混合90分钟，然后在室温下向悬浮液中加入0.1mL的NH3·H2O(25wt％)。搅拌30分钟后，加入10mL乙酰丙酮铁的乙醇溶液(调节乙酰丙酮铁的乙醇溶液的浓度为0.1mol/L，0.2mol/L，0.4mol/L)慢加入上述溶液中，再搅拌30分钟。悬浮液在60℃下维持12h，使无定形Fe3O4纳米颗粒预生长在RGO表面上，得到Fe3O4/RGO纳米复合材料。
将上述Fe3O4/RGO纳米复合材料用乙醇洗涤2次，2000g离心10min，倒去上清液，将得到的沉淀物重新分散在10毫升蒸馏水中，得到RGO分散体。将一定量的Ca(NO3)2(8mmol)，AM单体(40mmol)，MBAA(0.013mmol)和过硫酸铵(31mmol)在N2气保护和冰浴下溶解在RGO分散体中。将混合物脱气15分钟后，放入一个50ml的容器中，在70℃烘箱中烘4小时。制得0.1Fe/RGO/PAM，0.2Fe/RGO/PAM和0.4Fe/RGO/PAM 3种水凝胶。
实施例2
将实施例1中获得的三种水凝胶样品进行降解RhB实验研究，考察不同浓度乙酰丙酮铁/乙醇溶液条件下所合成的对比材料对有机染料RhB的降解效果率。实验结果如图1所示，结果表明，最佳水凝胶为0.2Fe/RGO/PAM，其降解率在15min内即达到90％。0.4Fe/RGO/PAM次之，15min降解率为98％。0.1Fe/RGO/PAM效果最差，反应时间到45min时，RhB的降解率也仅为60％。
常见的Fenton反应机理如下：
Fe2++H2O2→Fe3++OH·+OH-
Fe3++H2O2→Fe2++HO2·+H+
在太阳光照射下，像RhB这样的染料分子会被光子敏化释放出来电子还原Fe3+。染料可能水解或与一些氧化剂反应，如溶液中的溶解氧分子。与此同时，通过施加太阳光或紫外线的芬顿过程，另外产生羟基自由基，并且铁离子被氧化成亚铁。Fe2+的再循环导致OH的进一步生成。羟基的总量显着增加自由基导致太阳光驱动的芬顿反应加速有机染料的降解。
实施例3
将实施例1中获得的水凝胶材料0.2Fe/RGO/PAM用于光-芬顿反应过程。在光-芬顿反应过程中调节RhB溶液pH分别为3.5、4.5、5.5、6.5。
实施例4
将实施例3中获得的样品进行光-芬顿反应实验研究，考察光-芬顿反应过程中，RhB溶液不同pH对降解效果的影响。实验结果如图2所示，结果表明，不同pH的实验效果相似，降解率随反应时间增长都呈现持续升高，最终都能达到90％左右。其中，相较于其他反应条件，pH为4.5时反应较快。众所周知，pH值对于确定Fenton氧化的效率具有重要的作用。通常，pH值限制在2.0-4.0的范围内，但在本实验中，当pH值继续增加到6.5时，0.2Fe/RGO/PAM的降解率仍然很高RhB的降解率。而且，总结出pH值芬顿反应的区域可以从3.5扩大到6.5，这表明水凝胶因此具有良好的工业应用前景。

Claims (9)

1.一种功能纳米复合水凝胶的制备方法，其特征在于，包括如下步骤：
（1）将还原氧化石墨烯的醇溶液与乙腈混合得到悬浮液，在室温下向悬浮液中加入NH3·H2O搅拌；
（2）向步骤（1）得到的溶液中缓慢加入乙酰丙酮铁的醇溶液，搅拌；
（3）将步骤（2）得到的悬浮液在50-80°C下维持10-12h，使无定形Fe3O4纳米颗粒预生长在还原氧化石墨烯表面上；
（4）将步骤（3）得到的材料用乙醇洗涤后，离心，将得到的沉淀物重新分散在蒸馏水中，得到还原氧化石墨烯分散系；
（5）将Ca(NO3)2、丙烯酰胺单体、一溴乙酸和过硫酸铵溶解在前述还原氧化石墨烯分散系中；
（6）将步骤（5）得到的混合物脱气，放入容器中，在烘箱中干燥，得到Fe3O4/还原氧化石墨烯/PAM水凝胶，其中，还原氧化石墨烯的醇溶液、NH3·H2O、乙酰丙酮铁的醇溶液的浓度分别为5-10mg/ml、25-30 wt%和0.3-0.5 mol /L；还原氧化石墨烯的醇溶液、乙腈、NH3·H2O、乙酰丙酮铁的醇溶液的体积分别为100-110ml、20-30ml、0.1-0.5ml和10-20mL。
2.根据权利要求1所述的制备方法，其特征在于，步骤（1）或（2）中的醇溶液为乙醇溶液、甲醇溶液或异丙醇溶液中的任意一种。
3.根据权利要求1所述的制备方法，其特征在于，步骤（2）中，乙酰丙酮铁的醇溶液的加入速度不超过30ml/min。
4.根据权利要求1所述的制备方法，其特征在于，步骤（5）中Ca(NO 3)2、丙烯酰胺单体、一溴乙酸和过硫酸铵的量分别为5-10mmol、30-40 mmol、0.01-0.02 mmol和30-35mmol。
5.根据权利要求1所述的制备方法，其特征在于，步骤（5）中，溶解操作需在N2气保护和冰浴下。
6.根据权利要求1所述的制备方法，其特征在于，步骤（6）中，烘箱的条件为在50-80℃烘箱中烘2-5小时。
7.根据权利要求1所述的制备方法，其特征在于，将步骤（6）制备的水凝胶在-60℃、0.12mbar冷冻干燥10-15小时以利储存。
8.权利要求1~7任一项所述的制备方法制备得到的功能纳米复合水凝胶。
9.权利要求8所述的功能纳米复合水凝胶在降解有机污染物中的应用，其中，所述有机污染物为有机染料。
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