CN110182906B - 一种导电有机膜耦合过滤***降解有机废水的处理工艺 - Google Patents
一种导电有机膜耦合过滤***降解有机废水的处理工艺 Download PDFInfo
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Abstract
本发明涉及一种导电有机膜耦合过滤***降解有机废水的处理工艺，其特征在于，该处理工艺是利用导电有机膜耦合过滤***对有机废水进行处理，所述导电有机膜耦合过滤***包括相连通的水泵和反应器；反应器上端设置有进水口，下端设置有出水口，进水口与出水口之间的反应器内固定有对电极和膜电极；所述膜电极和对电极构成两电极体系，通过金属导线分别连接到外置的恒电位仪上。本发明中膜电极为碳基聚偏氟乙烯膜，可与电化学耦合，增强了分离小分子物质的能力，达到强化去除污染物的目的。本发明的导电有机膜耦合过滤***能耗低，工艺简单，运行稳定，出水水质高，占地面积小且易实现自动控制，具有广阔的应用前景。
Description
技术领域
本发明涉及一种导电有机膜耦合过滤***降解有机废水的处理工艺，属于废水处理及资源化技术领域。
背景技术
21世纪以来全人类面临的主要生存挑战大多数与水质和水量问题密切相关。在全球范围内，饮用水安全和卫生条件的限制导致每年有高达160万人口的死亡。膜过滤技术作为一种高效的分离纯化技术，由于其能耗低、运行稳定、占地面积小、出水水质高等优势，常应用于废水处理和资源化领域中。如中国专利文献CN105060617A公开了一种低浓度有机废水的双膜内循环生物处理工艺，经格栅和格网除渣后的有机污水进入双膜内循环生物反应器，经布水装置均匀分配到填料生物膜反应区，通过气流的作用在填料生物膜反应区与微滤膜过滤区之间形成内循环，间隙开启填料生物膜反应区和微滤膜过滤区的进气电动阀，交替形成厌氧-缺氧-好氧的环境，完成微生物好氧硝化吸磷、缺氧脱氮反应和厌氧放磷反应，达到净化水质的目的。脱落的生物膜和颗粒物被微滤膜截留，清水透过微滤膜经自吸泵抽吸出来，再经紫外线消毒后即可达标排放。但是该方法过滤的颗粒等污染物被微滤膜截留，易造成膜污染，并且对浓度较高的有机废水的处理效果不理想。
由于大分子、胶体颗粒和微生物引起的膜污染以及膜过滤期间产生的浓缩废水的处理限制了膜过滤技术的应用范围。然而耦合膜过滤和电化学技术的结合可以解决或缓解膜污染问题、直接处理产生地浓缩污染物，是一个废水处理领域的新兴研究方向。目前对导电有机膜制备方法的研究主要有对基底膜的导电改性，导电纳米材料的负载等，如中国专利文献CN104857866A公开了一种制备亲水改性聚偏氟乙烯膜的方法，包括如下步骤：1)含有引发剂的聚偏氟乙烯膜的制备；2)KH570接枝聚偏氟乙烯膜的制备；3)将KH570接枝的聚偏氟乙烯膜浸入到二氧化钛水溶液中进行反应制备亲水改性聚偏氟乙烯膜。但该方法具有修饰过程复杂、膜稳定性差、易造成二次污染和制备成本高等缺点阻碍了导电有机膜的工业规模化应用。
发明内容
针对现有技术的不足，本发明提供一种导电有机膜耦合过滤***降解有机废水的处理工艺。本发明将电化学与膜过滤技术结合起来，实现了有机废水处理中有机物降解和污水消毒的同时应用了新型导电有机膜，避免了传统膜改性工艺的缺陷，解决了膜污染问题。
本发明是通过以下技术方案实现的：
一种导电有机膜耦合过滤***降解有机废水的处理工艺，其特征在于，该处理工艺是利用导电有机膜耦合过滤***对有机废水进行处理，所述导电有机膜耦合过滤***包括相连通的水泵和反应器；反应器上端设置有进水口，下端设置有出水口，进水口与出水口之间的反应器内固定有对电极和膜电极；所述对电极和膜电极构成两电极体系，通过金属导线分别连接到外置的恒电位仪上；
所述膜电极为碳基聚偏氟乙烯膜，是按以下方法制备得到：将聚偏氟乙烯铸膜液以刮膜的方式涂覆在预处理后的干燥碳纤维上，涂层厚度为300～400μm，空气静中置1～5min，浸入去离子水中过夜，制得聚偏氟乙烯涂层基底膜；再将基底膜真空干燥后，经相转化法制得光滑均匀的碳基聚偏氟乙烯膜(CC/PVDF膜)；
降解有机废水的处理工艺：将纯水通过反应器，对反应器预处理20～30min，使膜电极处于稳定状态，预处理后开启恒电位仪给对电极和膜电极施加稳定电压；再将有机废水持续泵入反应器，依次通过对电极和膜电极，净化后的废水从出水口自然流出。
根据本发明优选的，所述金属导线为钛丝；所述对电极和膜电极分别嵌入反应器的电极卡槽中，通过防水胶、凡士林和硅胶垫片固定。
根据本发明优选的，所述对电极位于膜电极的正上方；进一步优选的，所述膜电极和对电极垂直距离为1～3cm。
根据本发明优选的，所述对电极为铂网、钛网或不锈钢网。
根据本发明优选的，所述恒电位仪提供稳定电压范围为0～30V。
根据本发明优选的，所述碳纤维为聚丙烯腈基碳纤维；所述碳纤维预处理为将碳纤维依次在丙酮、乙醇和去离子水溶液中分别超声60～80min去除碳纤维附着的有机物及其它杂质，然后在50～80℃条件下干燥4～5小时。
根据本发明优选的，所述聚偏氟乙烯铸膜液的制备方法具体为：将聚偏氟乙烯粉末和造孔剂聚乙烯吡咯烷酮溶解在N，N-二甲基甲酰胺中，磁力搅拌10～12小时，再经50～80℃真空脱气3～5h后制得聚偏氟乙烯铸膜液；其中，聚偏氟乙烯粉末、造孔剂聚乙烯吡咯烷酮与N，N-二甲基甲酰胺的质量比为12:2:86。
根据本发明优选的，所述真空干燥的条件为50～80℃，50～70min。
根据本发明优选的，所述相转化法具体为：将聚偏氟乙烯铸膜液以刮膜的方式涂覆在聚偏氟乙烯涂层基底膜的涂层表面，所述的基底膜固定于玻璃板上，涂层厚度为200～400μm，空气中静置1～3min，将玻璃板整体缓慢浸入25～28℃恒温去离子水凝固浴中，经相转化后转变成一个三维大分子网络式的凝胶结构固化成膜。
其中，相转化是指聚偏氟乙烯铸膜液和去离子水通过溶剂和非溶剂两相界面进行溶剂和非溶剂的传质交换，相互扩散、相间流动、发生膜孔的凝聚和聚偏氟乙烯富相固化。
根据本发明优选的，所述有机废水以3～5mL/min的流速通过对电极和膜电极。
本发明中所述刮膜使用常规技术即可。
本发明过滤有机废水的原理：当有机废水通过反应器时发生静电排斥、电增强润湿、直接电子转移和羟基自由基高级氧化等作用。静电排斥作用是指在导电有机膜耦合过滤***中，给膜电极施加负电位，当有机废水中的污染物带负电荷时，由于静电排斥作用，与膜电极带同种电荷地污染物会被排斥到远离膜表面的另一端，减少了污染物在膜上的沉积从而缓解膜污染。电增强润湿作用是指给膜电极施加恒定电位后，通过连接固液界面的外电位可以降低固液表面的界面张力而不改变膜表面的化学组成，起到降低膜表面水接触角，提高膜表面的润湿性，提高膜水通量。直接电子转移和羟基自由基高级氧化作用是指有机废水进入***后，当膜施加的电位大于有机物的氧化电位时，膜电极发生直接电子转移，促进有机废水发生氧化还原作用，从而达到降解有机废水的目的，而在膜被极化时，溶解氧通过氧的双电子还原产生过氧化氢，通过碳纤维上的活性位点或对电极表面的二氧化钛等催化作用发生类芬顿反应产生羟基自由基，同时通过对水的直接氧化产生羟基自由基，产生的羟基自由基进一步对污染物进行高级氧化甚至矿化。
本发明的技术特点与有益效果：
1、本发明中通过在碳纤维上涂覆两次聚偏氟乙烯铸膜液，采用操作简单的两步相转换法制备得到CC/PVDF导电有机膜。第一次刮膜涂覆聚偏氟乙烯铸膜液改善了碳纤维的粗糙织物结构制得平整的基底膜，同时浸入碳纤维大孔的铸膜液与孔壁碳纤维紧密结合可以提高膜的机械稳定性，第二次刮膜涂覆聚偏氟乙烯铸膜液是为了制备光滑致密的膜选择层，两次涂覆使CC/PVDF膜具有优异的导电性和机械稳定性以及光滑均匀的表面形貌，克服了传统导电膜改性工艺修饰过程复杂、膜稳定性差、制备成本高和易造成二次污染等缺点。本发明制备的碳基聚偏氟乙烯膜可与电化学耦合，增强了分离小分子物质的能力，克服传统膜过滤工艺的膜孔截留的局限性，使去除小于膜孔的污染物成为可能，达到强化去除污染物的目的，同时具有高效经济的特点，将其应用于导电有机膜过滤***具有潜在优势。
2、本发明中导电有机膜耦合过滤***通过恒电位仪对两电极体系施加恒电位，在有机废水通过对电极和膜电极期间发生静电排斥、电增强润湿、直接电子转移和羟基自由基高级氧化等作用，可达到控制膜污染和降解有机废水的目的，解决传统膜过滤工艺存在的浓缩液处理问题，同时解决阻碍膜应用的膜污染问题。
3、本发明的导电有机膜耦合过滤***能耗低，工艺简单，运行稳定，出水水质高，占地面积小且易实现自动控制，具有广阔的应用前景。
附图说明
图1为本发明中实施例1导电有机膜耦合过滤***工作示意图；
图中：1、水泵，2、进水口，3、对电极，4、膜电极，5、出水口，6、恒电位仪，7、反应器。
图2为碳纤维、基底膜和CC/PVDF膜的扫描电子显微镜图像。
图3为碳纤维的共聚焦激光扫描显微镜图像。
图4为基底膜的共聚焦激光扫描显微镜图像。
图5为CC/PVDF膜的共聚焦激光扫描显微镜图像。
图6为实施例1通过有机废水30min后CC/PVDF膜的扫描电子显微镜图像。
图7为实施例1通过有机废水30min后CC/PVDF膜的傅里叶变换衰减全反射红外光谱图。
图8为不同浓度的甲基橙溶液通过CC/PVDF膜的伏安曲线图。
图9为实施例3施加0V电压通过有机废水30min后CC/PVDF膜表面扫描电子显微镜图像。
图10为实施例3施加1V电压通过有机废水30min后CC/PVDF膜表面扫描电子显微镜图像。
图11为实施例3施加2V电压通过有机废水30min后CC/PVDF膜表面扫描电子显微镜图像。
图12为实施例3施加3V电压通过有机废水30min后CC/PVDF膜表面扫描电子显微镜图像。
具体实施方式
下面结合附图和具体实施例对本发明做进一步描述，但本发明保护范围不限于此。
同时下述实施例中所述实验方法，如无特殊说明，均为常规方法；所述试剂、材料和设备，如无特殊说明，均可从商业途径获得。
实施例中恒电位仪采用CHI1030C多通道恒电位仪，上海辰华仪器有限公司有售；所用钛网，60目，沧州康威金属制品有限公司有售；实施例中碳纤维采用聚丙烯腈基碳纤维，上海河森电气有限公司有售；导电胶、钛丝、防水胶、凡士林、硅胶垫片、聚偏氟乙烯，甲基橙、腐殖酸均为市售产品。
实施例1
一种导电有机膜耦合过滤***降解有机废水的处理工艺，该处理工艺是利用导电有机膜耦合过滤***对有机废水进行处理，所述导电有机膜耦合过滤***包括相连通的水泵1和反应器7(反应器7为封闭的有机玻璃柱，有效容积为12L)，反应器7上端设置有进水口2，下端设置有出水口5，进水口2与水泵1相连通，进水口2与出水口5之间的反应器7内将对电极3和膜电4极嵌入反应器的电极卡槽中，然后用防水胶、凡士林和硅胶垫片固定；对电极3采用材料为60目钛网，膜电极4采用材料为碳基聚偏氟乙烯膜(CC/PVDF膜)，所述对电极3位于膜电极4的上方，垂直距离为1cm，膜电极4的截留作用使有机废水中的污染物富集在两电极间，延长***中污染物的停留时间进行氧化还原反应，使污染物更大程度被降解；膜电极4和对电极3构成两电极体系，通过导电胶与钛丝连接到外置的恒电位仪6上；
所述膜电极为碳基聚偏氟乙烯膜，是按以下方法制备得到：首先将聚偏氟乙烯粉末和造孔剂聚乙烯吡咯烷酮溶解在N，N-二甲基甲酰胺中，磁力搅拌12小时后完全溶解，再经50℃真空脱气4小时后制得聚偏氟乙烯铸膜液；然后将聚偏氟乙烯铸膜液以刮膜的方式涂覆在预处理后的干燥碳纤维上，涂层厚度为300μm，空气静中置3min，浸入去离子水中过夜制得聚偏氟乙烯涂层基底膜，基底膜经过80℃真空干燥70min后，将聚偏氟乙烯铸膜液以刮膜的方式涂覆在聚偏氟乙烯涂层基底膜的涂层表面，所述的基底膜固定于玻璃板上，涂层厚度为200μm,空气中静置2min，将玻璃板整体缓慢浸入25℃恒温去离子水凝固浴中，经相转化制得光滑均匀的碳基聚偏氟乙烯膜(CC/PVDF膜)。如图2-5所示，从碳纤维到基底膜到CC/PVDF膜，其表面形貌越来越光滑，表面粗糙度明显降低，提高了CC/PVDF膜的机械稳定性。
上述聚偏氟乙烯粉末、造孔剂聚乙烯吡咯烷酮与N，N-二甲基甲酰胺的质量比为12:2:86。
降解有机废水的处理工艺：将纯水通过反应器，对反应器预处理20min，使膜电极处于稳定状态，预处理后开启恒电位仪给钛网和CC/PVDF膜分别施加1V，2V和3V的稳定电压；再将有机废水持续泵入反应器，以4mL/min的流速依次通过钛网和CC/PVDF膜，净化后的废水从出水口自然流出。
采用10mg/L甲基橙、10mM NaCl水溶液作为有机废水。
取本实施例运行30min净化后的水，检测有机废水处理效果为：分别施加1V，2V和3V的稳定电压下甲基橙去除率为21％、88％和92％，膜水通量分别为70％、86％和92％。如图6和图7所示，通过有机废水30min后的CC/PVDF膜表面与未通过有机废水的CC/PVDF膜表面形貌和化学组成无明显区别，说明甲基橙在膜上几乎无附着或被降解，有效的抑制了膜污染。如图8所示，在有机废水通过CC/PVDF膜时氧化电位产生了变化，说明CC/PVDF膜发生了直接电子转移。
实施例2
一种导电有机膜耦合过滤***降解有机废水的处理工艺，其结构与具体处理工艺步骤如实施例1所述，不同之处在于采用20mg/L腐殖酸水溶液作为有机废水。
取本实施例运行30min净化后的水，检测有机废水处理效果为：分别施加1V，2V和3V的稳定电压下腐殖酸去除率为71％、76％和82％，膜水通量分别为65％、81％和85％。
实施例3
一种导电有机膜耦合过滤***降解有机废水的处理工艺，其结构与具体处理工艺步骤如实施例1所述，不同之处在于采用105CFU/mL的大肠杆菌菌液作为有机废水。
取本实施例运行30min净化后的水，检测污染物去除效果为：分别施加1V，2V和3V的稳定电压下出水细菌死亡率均达到100％，膜水通量分别为71％、80％和85％。如图9-12所示，可以发现大肠杆菌细胞破裂及死亡，且随电压增大，细胞破裂越严重，表明导电有机膜耦合过滤***具有高效的杀菌能力。
对比例1
一种常见超滤***去除有机废水的处理工艺，其结构与具体处理工艺步骤如实施例1所述，不同之处在于采用Sterlitech公司的PVDF超滤膜作为导电有机膜，恒电位仪施加的电压为3V，30min后取过滤后的水，其有机废水处理效果为甲基橙去除率为36％，膜水通量为55％。
对比例2
一种导电有机膜耦合过滤***降解有机废水的处理工艺，其结构与具体处理工艺步骤如实施例1所述，不同之处在于，恒电位仪施加的电压为0V，30min后取过滤后的水，其有机废水处理效果为甲基橙去除率小于20％，膜水通量为60％。
对比例3
一种导电有机膜耦合过滤***降解有机废水的处理工艺，其结构与具体处理工艺步骤如实施例1所述，不同之处在于，恒电位仪施加的电压为0V，30min后取过滤后的水，其有机废水处理效果为腐殖酸去除率为65％，膜水通量为40％。
Claims (9)
1.一种导电有机膜耦合过滤***降解有机废水的处理工艺，其特征在于，该处理工艺是利用导电有机膜耦合过滤***对有机废水进行处理，所述导电有机膜耦合过滤***包括相连通的水泵和反应器；反应器上端设置有进水口，下端设置有出水口，进水口与出水口之间的反应器内固定有对电极和膜电极；所述对电极和膜电极构成两电极体系，通过金属导线分别连接到外置的恒电位仪上；
所述膜电极为碳基聚偏氟乙烯膜，是按以下方法制备得到：将聚偏氟乙烯铸膜液以刮膜的方式涂覆在预处理后的干燥碳纤维上，涂层厚度为300～400μm，空气中静 置1～5min，浸入去离子水中过夜，制得聚偏氟乙烯涂层基底膜；再将基底膜真空干燥后，经相转化法制得光滑均匀的碳基聚偏氟乙烯膜；所述对电极为铂网、钛网或不锈钢网；
所述相转化法为：将聚偏氟乙烯铸膜液以刮膜的方式涂覆在聚偏氟乙烯涂层基底膜的涂层表面，所述的基底膜固定于玻璃板上，涂层厚度为200～400μm，空气中静置1～3min，将玻璃板整体缓慢浸入25～28℃恒温去离子水凝固浴中，经相转化后转变成一个三维大分子网络式的凝胶结构固化成膜；
降解有机废水的处理工艺：将纯水通过反应器，对反应器预处理20～30min，使膜电极处于稳定状态，预处理后开启恒电位仪给对电极和膜电极施加稳定电压；再将有机废水持续泵入反应器，依次通过对电极和膜电极，净化后的废水从出水口自然流出。
2.如权利要求1所述的处理工艺，其特征在于，所述金属导线为钛丝；所述对电极和膜电极嵌入反应器的电极卡槽中，通过防水胶、凡士林和硅胶垫片固定。
3.如权利要求1所述的处理工艺，其特征在于，所述对电极位于膜电极的正上方。
4.如权利要求3所述的处理工艺，其特征在于，所述膜电极和对电极垂直距离为1～3cm。
5.如权利要求1所述的处理工艺，其特征在于，所述恒电位仪提供稳定电压范围为0～30V。
6.如权利要求1所述的处理工艺，其特征在于，所述碳纤维为聚丙烯腈基碳纤维；所述预处理为将碳纤维依次在丙酮、乙醇和去离子水溶液中分别超声60～80min去除碳纤维附着的有机物及其它杂质，然后在50～80℃条件下干燥4～5小时。
7.如权利要求1所述的处理工艺，其特征在于，所述聚偏氟乙烯铸膜液的制备方法具体为：将聚偏氟乙烯粉末和造孔剂聚乙烯吡咯烷酮溶解在N，N-二甲基甲酰胺中，磁力搅拌10～12小时，再经50～80℃真空脱气3～5h后制得聚偏氟乙烯铸膜液；其中聚偏氟乙烯粉末、造孔剂聚乙烯吡咯烷酮与N，N-二甲基甲酰胺的质量比为12:2:86。
8.如权利要求1所述的处理工艺，其特征在于，所述真空干燥的条件为50～80℃，50～70min。
9.如权利要求1所述的处理工艺，其特征在于，所述有机废水以3～5mL/min的流速通过对电极和膜电极。
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