CN103762371B - 一种耦合mbr与mfc的碳泡沫催化电极系统 - Google Patents
一种耦合mbr与mfc的碳泡沫催化电极系统 Download PDFInfo
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Abstract
一种耦合MBR与MFC的碳泡沫催化电极系统，属于污水处理与能源回收利用技术领域。其特征是应用碳泡沫与含有过渡金属的前驱体混合，煅烧，制得催化性能优于含贵金属的催化剂；碳泡沫与催化剂混合于有机溶剂，Nafion与PVDF作为粘结剂，涂于苯胺植酸滤布电极上催化MFC-MBR氧化还原；碳泡沫作为MFC-MBR阳极，孔隙多利于微生物附着于表面或孔道内，电池电势输出0.4v；碳泡沫含有氮，具有氧化还原性，作为MFC-MBR阴极。本发明的效果和益处是MFC-MBR在高效处理污水的同时实现电能输出，达到能源回收利用的目标，且反应器中的微电场有效地减缓了膜污染。
Description
技术领域
本发明属于污水处理与能源回收利用技术领域，涉及应用碳泡沫制备催化剂、碳泡沫作为微生物燃料电池与膜生物反应器耦合系统电极，利用微生物直接将污水中化学能转化为电能。
背景技术
微生物燃料电池（MFC）是微生物技术与电池技术相结合的产物，产生电能或H2O2等有益物质，但其出水水质差；膜生物反应器（MBR）出水水质好，但膜容易污染、能耗高；将两者耦合MFC-MBR，MBR可以克服MFC出水水质差，MFC产生的能量，可降低MBR曝气、出水、去除COD所需的部分能耗，降低运行成本、出水水质好。MFC-MBR多应用碳纤维布、碳纸、碳毡等作为电极材料，虽导电性能好，但其比表面积和孔隙度较小，微生物只能在其表面生长，因而产生的电流密度受到限制，应用碳泡沫作为污水处理中的电极材料还很少。
Guo Ping Sheng.et al.以石墨颗粒作为阳极，功率密度与电流密度分别为4.35W/m3和18.32A/m3（Guo Ping Sheng.et al.Environ Sci Technol2011;45:9256–61）；Yong Peng Wang.et al.应用碳纤维作为阳极，无纺布外层包裹碳毡作为阴极（YongPeng Wang.et al.Applied Energy98(2012)230–235）；以上关于MFC-MBR的实例中，虽出水水质好，但均未应用催化剂，产电量较低。
目前多应用贵金属与碳黑制备催化剂，催化效果虽好，但成本高；碳泡沫是一种新型碳材料，具有高比表面积，多用于夹层电极的中间层、超级电容器等，仍无研究者将其应用于MFC阴极催化剂的制备。
发明内容
本发明的目的是提供一种耦合MBR与MFC的碳泡沫催化电极系统，解决了催化剂成本高、产电量低、膜污染的问题。
本发明的技术方案是：
1）反应器1阴极催化剂制备：将碳泡沫用研钵磨碎至120目，加入含酸苯胺溶液，10℃以下，加入摩尔质量比3：1的铁、钴催化剂前驱体、过硫酸铵溶液，搅拌24h后60℃烘干，800～1000℃煅烧；
2）反应器1阴极组件制作：首先，苯胺、植酸与过硫酸铵溶液分别涂于滤布表面；其次，催化剂PANI-FeCo-C掺杂于苯胺、植酸中，与过硫酸铵溶液分别涂于上述滤布；再次，将PANI-FeCo-C，磨碎的碳泡沫，分别加入N-N-二甲基乙酰胺溶剂中，加入Nafion与PVDF粘结剂，搅拌、超声，涂于含苯胺、植酸凝胶滤布上；最后，滤布外层加碳纤维丝；
3）反应器1构型：将碳泡沫置于阳极室内，阳极室底部与四周密闭，顶端出水，悬挂于反应器上方，阳极为厌氧环境，阴极膜组件置于阳极室外侧，阴极顶端由泵抽吸出水，反应器下方曝气；
4）置于阳极室内碳泡沫接种产电希瓦式菌；
5）反应器1运行：阳极产电菌降解污水中有机物产生电子，电子通过外电路到达阴极，与带负电荷污染物排斥减缓阴极膜污染，反应器运行整个周期，未进行膜组件清洗；
6）检验碳泡沫氧化还原性：扫描速率50mv/s,于0.1mol/L H2SO4中测定不完全碳化碳泡沫与未煅烧三聚氰胺甲醛树脂泡沫循环伏安曲线进行对比；
7）反应器2构型：阳极组件为封闭长方体，内保持细长而狭窄的空间，用玻璃胶将聚苯胺改性滤布粘于阳极外侧，碳泡沫与阳极相邻作为阴极，反应器底端曝气；
8）反应器2运行：水流由阳极底部进入，顶部出水，碳纤维丝将阳极产生电子传导至阴极，电子与质子和氧气在阴极泡沫的催化作用下形成水。
本发明的效果和益处是利用碳泡沫制得成本低廉且高效地催化剂，催化氧化还原反应，提高MFC-MBR产电量；碳泡沫作为MFC-MBR电极，在高效处理污水的同时实现电能输出，达到能源回收利用的目标，且反应器中的微电场有效地减缓了膜污染。
附图说明
附图1是碳泡沫作为阳极改性滤布作为阴极电势图。
图中：横坐标表示时间，单位d，纵坐标表示电压，单位v，圆点、正方形、三角形分别代表电池电压、阳极电势、阴极电势；阳极电势虽高，却得到0.4v电池电势，说明碳泡沫作为MFC-MBR阳极，更有利于阳极产的电子传导至阴极，更高效地产生电能。
附图2是磨碎碳泡沫制得催化剂循环伏安图。
图中：横坐标表示电压，单位v，纵坐标表示电流，单位A，扫描速率50mv/s,于0.1mol/L H2SO4中扫描循环伏安图，由循环伏安曲线得到两对明显且对称的氧化还原峰，说明催化剂具有良好的催化氧化还原性能，可取代碳黑等催化剂载体。
附图3是碳泡沫作为阴极改性滤布作为阳极电势图。
图中：以苯胺植酸凝胶改性滤布作为阳极，不完全碳化碳泡沫作为阴极，甘汞电极为参比电极，测得阳极、阴极与电池电势图；横坐标表示时间，单位min，纵坐标表示电压，单位v，圆点代表电池电压，正方形代表阳极电势，三角形代表阴极电势，得到电池电势0.2v，优于同等条件下其他阴极组件。
附图4是550℃制得碳泡沫循环伏安图。
图4以不完全碳化的碳泡沫作为工作电极，铂片为对电极，甘汞电极为参比电极，扫描速率50mv/s,于0.1mol/L H2SO4中扫描循环伏安，横坐标表示电压，单位v，纵坐标表示电流，单位A，由图可以看出，在±0.4v左右具有明显且相对对称的氧化还原峰，说明不完全碳化碳泡沫本身具有优异的氧化还原性。
附图5是未煅烧三聚氰胺甲醛树脂泡沫循环伏安图。
图5未经煅烧的三聚氰胺甲醛树脂泡沫在与图4相同的条件下，扫描循环伏安，横坐标表示电压，单位v，纵坐标表示电流，单位A，目的是为了与煅烧后的碳泡沫进行对比；
具体实施方式
以下结合技术方案和附图详细叙述本发明的具体实施方式。
实施例1
在惰性气氛下，以三聚氰胺甲醛树脂泡沫为原料，升温速率10℃/min，升温至1000℃，碳化30min，自然冷却至室温，制得5cm×1cm×1cm碳泡沫1。
催化剂制作：溶液A：6mL苯胺与1g碳泡沫混合；溶液B：1.43g过硫酸铵、0.5g Co(NO3)2·6H2O、1.61g FeCl3·6H2O加入10mL去离子水中，于10℃下混合，搅拌24h氮气气氛在，800℃煅烧3h。
阴极组件制作：首先，4.58mL苯胺与9.21mL植酸加入10mL去离子水中，2.86g过硫酸铵加入10mL去离子水中，分别用刷子涂于乙醇清洗过的6cm×6cm滤布表面；其次，0.2g催化剂PANI-FeCo-C掺杂于4.58mL苯胺、9.21mL植酸与10mL去离子水的溶液中，与10mL含有2.86g过硫酸铵溶液分别涂于上述滤布上；再次，将0.2g PANI-FeCo-C，0.2g磨碎的碳泡沫，分别加入10ml N-N-二甲基乙酰胺溶剂中，加入220μLNafion与0.2g PVDF粘结剂，搅拌、超声，涂于含苯胺植酸凝胶滤布上；最后，滤布外层包裹碳纤维丝作为导线与外电路连接。
将碳泡沫1置于φ5cm×6cm阳极室内，阳极室侧面开孔用于传递质子，将阳极室悬挂于反应器φ9cm×20cm上方，改性滤布阴极膜组件放于阳极室外侧，反应器下方曝气；阳极接种希瓦式菌，挂膜一个星期后，反应器开始运行；污水由阳极室底部进入，部分水从阳极侧壁流出，部分由阳极顶部流入反应器，经阴极组件过滤出水；利用气体流量计调节曝气量大小，使好氧区的阴极溶解氧保持正常水平；运行期间，电池电势0.4v,COD去除率99％。
实施例2
在惰性气氛下，以三聚氰胺甲醛树脂泡沫为原料，升温速率10℃/min，升温至550℃，碳化30min，自然冷却至室温，制得5cm×3cm×0.5cm碳泡沫2。
由循环伏安图可知，未完全碳化碳泡沫具有氧化还原性，将碳化碳泡沫2置于平板式膜组件反应器内作为阴极，阳极采用苯胺植酸凝胶改性滤布，将其用玻璃胶黏在每个膜组件两侧，穿插碳纤维丝作为导线，接种希瓦式菌运行。
Claims (1)
1.一种耦合膜生物反应器与微生物燃料电池的碳泡沫催化电极系统，是将孔隙度96％、电导率5s/cm的碳泡沫用于制备催化剂；将制得催化剂与含植酸苯胺溶液混合后与过硫酸铵溶液分别涂于聚苯胺滤布表面，再将碳泡沫与催化剂混合均匀涂于含催化剂聚苯胺滤布表面制备电极；将制得的电极应用于膜生物反应器与微生物燃料电池的碳泡沫催化电极系统，其特征在于：
a)将磨碎的碳泡沫与含酸苯胺溶液、过硫酸铵溶液和过渡金属催化剂前驱体混合、搅拌24h，60℃烘箱烘干，800℃氮气中煅烧，制得催化剂；
b)a)中制得催化剂掺杂于含植酸苯胺溶液中，与过硫酸铵溶液分别涂于负载聚苯胺滤布表面；
c)将磨碎的碳泡沫与a)中制得催化剂混合，溶于N-N-二甲基乙酰胺溶剂，加入Nafion与PVDF作为粘结剂，搅拌、超声，均匀涂于b)中所得滤布表面；
d)微生物附着于碳泡沫表面与内部孔道，作为阳极，c)中制得电极作为阴极，运行膜生物反应器与微生物燃料电池。
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