CN103208666B - 一种提高微生物燃料电池浸取钴酸锂中Co(III)的方法 - Google Patents
一种提高微生物燃料电池浸取钴酸锂中Co(III)的方法 Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
一种提高微生物燃料电池浸取钴酸锂中Co(III)的方法,微生物燃料电池的阴极和阳极电极均为石墨材料;阳极室装有电化学活性微生物以及阳极液;阴极室装有阴极液和钴酸锂颗粒;阳极室接种污水处理厂的澄清池污泥作为电化学活性微生物;阴极液为含有少量CuCl2的无机酸溶液。与不加CuCl2的对照相比,催化剂Cu(II)的加入不仅提高钴酸锂中Co(III)的浸取,而且增加无机酸的有效利用率。Cu(II)经过间歇使用后可沉积在电极表面,实现与Co(II)的分离。本发明过程清洁高效、副产电能、方法简单、成本低,对于处理废旧锂离子电池并浸出其中的钴金属具有很好的应用前景。
Description
技术领域
本发明涉及微生物燃料电池浸取钴酸锂,具体地说是一种提高微生物燃料电池浸取钴酸锂中Co(III)的有效方法。
背景技术
微生物燃料电池(Microbial Fuel Cells, MFCs)是以微生物为催化剂,将环境中污染物转化为电能和有价产品的新技术。这种兼具环境污染治理与废物资源化的革新技术正引起人们的广泛关注。
钴是生产锂离子电池的重要稀有金属,以LiCoO2存在于电池中,含量达15-20%。随着锂离子电池的大量生产和广泛使用,其带来的环境问题也日益引起关注。同时,我国又是锂离子电池最大消费、生产和出口国(占全球份额33%以上),而来自于钴矿的含量仅为0.01-0.2%。因此,若能清洁、高效地回收废旧锂离子电池中钴金属,不仅有效解决电池污染,而且资源化利用废弃物,具有显著的环境和生态效益、社会效益和经济效益。
与传统的物理的、化学的、以及生物的浸取钴酸锂方法不同,化学阴极MFCs能利用阳极有机底物提供的电子,浸取钴酸锂中Co(III),具有清洁、流程短、副产物少、污泥量少、产品易分离,且副产电能等优点。然而,有效提高钴浸取速率和酸利用率,仍是MFCs与传统钴浸取技术竞争所面临的关键挑战。
发明内容
本发明提供了一种有效提高MFCs浸出钴酸锂中Co(III)的新方法。
本发明采用的技术方案如下:
一种提高MFCs浸出钴酸锂中Co(III)的方法。
在MFCs的阳极室,装有电化学活性微生物以及阳极液,在MFCs的阴极室,装有阴极液和钴酸锂颗粒。
所述阳极室接种污水处理厂澄清池污泥作为电化学活性微生物。
所述澄清池污泥的pH: 6.8-7.0;电导率: 0.80-0.93 mS/cm;悬浮性固形物: 30-35 g/L;化学需氧量(COD): 150-300 mg/L。
阳极液成分为:12.0 mM乙酸钠;5.8 mM NH4Cl;1.7 mM KCl;17.8 mM NaH2PO4?H2O;32.3 mM Na2HPO4;矿质元素:12.5 mL/L (组成为MgSO4: 3.0 g/L;MnSO4?H2O: 0.5 g/L;NaCl:1.0 g/L;FeSO4?7H2O: 0.1 g/L;CaCl2?2H2O: 0.1 g/L;CoCl2?6H2O: 0.1 g/L;ZnCl2: 0.13 g/L;CuSO4?5H2O: 0.01g/L;KAl(SO4)2?12H2O: 0.01 g/L;H3BO3: 0.01 g/L;Na2MoO4: 0.025 g/L;NiCl2?6H2O: 0.024 g/L;Na2WO4?2H2O: 0.024 g/L);维生素: 12.5 mL/L (组成为维生素B1: 5.0 g/L;维生素B2: 5.0 g/L;维生素B3: 5.0 g/L;维生素B5: 5.0 g/L;维生素B6: 10.0 g/L;维生素B11: 2.0 g/L;维生素H: 2.0 g/L;对氨基苯甲酸: 5.0 g/L;硫辛酸: 5.0 g/L;氨基三乙酸:1.5 g/L)。
阴极液为含有一定量CuCl2的无机酸溶液,阴极和阳极电极均为石墨材料,钴酸锂颗粒附着在阴极石墨材料表面。
本发明的MFCs阳极室和阴极室初始时需通入氮气并密封以保持厌氧环境。
本发明的MFCs运行流程为:阳极液中的有机物在阳极室内被微生物氧化,过程产生的质子穿过质子交换膜进入阴极室,产生的电子经外电路导入阴电极。在阴电极表面,钴酸锂颗粒中的Co(III)在Cu(II)催化下,获得阴电极提供的电子,被还原为Co(II),从固相浸入到液相。
本发明中含催化剂Cu(II)和产物Co(II)的母液在调整酸度后可重复使用。
本发明中Cu(II)的作用不仅有效提高MFCs对钴酸锂中Co(III)的浸出效率,而且提高无机酸的有效利用率,同时系统电能也得到提高。
附图说明
图1是实施本发明的MFCs浸出钴酸锂中Co(III)的示意图。
图2是实施本发明的MFCs浸出钴酸锂中Co(III)的时间变化图。
图3是实施本发明的MFCs阴极库仑效率的时间变化图。
图4是实施本发明的MFCs电能输出图。
图5是实施本发明的MFCs阴极液pH的时间变化图。
图6是实施本发明的MFCs阴极的无机酸有效利用率。
具体实施方式
以下是对本发明的进一步说明,而不是对本发明的限制。
实施例1:
步骤一:构建微生物燃料电池(图1),阳极室和阴极室均为有机玻璃材质,总容积分别为125 mL,有效工作体积为100 mL,以质子交换膜(CMI-7000)隔开。
步骤二:分别将阳极电极和阴极电极置于阳极室和阴极室中,阳极电极和阴极电极的电极材料均为石墨毡(北京三业碳材料公司) (表观尺寸:3 cm × 2 cm × 1 cm),在外电路导线3中接入200欧外阻和参比电极,通过数据采集系统收集产电数据和电极电势。
步骤三:将20 mg 钴酸锂粉末(粒度8~9 μm)、阴极电极置于100mL去离子水中,100 rpm磁力搅拌20 min,钴酸锂颗粒完全吸附在碳毡上,从而制得以钴酸锂中Co(III)为电子受体的MFCs阴电极。
步骤四:在阳极室加入100 mL培养液,其组成为12.0 mM乙酸钠;5.8 mM NH4Cl;1.7 mM KCl;17.8 mM NaH2PO4?H2O;32.3 mM Na2HPO4;矿质元素:12.5 mL/L (MgSO4: 3.0 g/L;MnSO4?H2O: 0.5 g/L;NaCl: 1.0 g/L;FeSO4?7H2O: 0.1 g/L;CaCl2?2H2O: 0.1 g/L;CoCl2?6H2O: 0.1 g/L;ZnCl2: 0.13 g/L;CuSO4?5H2O: 0.01g/L;KAl(SO4)2?12H2O: 0.01 g/L;H3BO3: 0.01 g/L;Na2MoO4: 0.025 g/L;NiCl2?6H2O: 0.024 g/L;Na2WO4?2H2O: 0.024 g/L);维生素: 12.5 mL/L (维生素B1: 5.0 g/L;维生素B2: 5.0 g/L;维生素B3: 5.0 g/L;维生素B5: 5.0 g/L;维生素B6: 10.0 g/L;维生素B11: 2.0 g/L;维生素H: 2.0 g/L;对氨基苯甲酸: 5.0 g/L;硫辛酸: 5.0 g/L;氨基三乙酸: 1.5g/L)。阳极室接种污水处理厂澄清池污泥10 g(大连凌水河污水处理厂)。阴极室加入100 mL含50 mM铁氰化钾缓冲溶液驯化阳极。阳极液曝氮气20 min后密封。将装置置于15 oC环境避光运行。当电压下降至20 mV以下时,即完成一个周期,并补加上述培养基成分。待连续三个周期输出电压稳定在相似值时,表明阳极电化学活性菌驯化和启动成功。
步骤五:将步骤四的铁氰化钾溶液替换为100 mL的0.01 M HCl溶液,加入CuCl2,使其浓度达到10 mg/L,曝氮气20 min,将步骤三的阴极电极组装并密封。同时,将步骤四的阳极液进行更新。
步骤六:定期取样,分析液相中Co(II)和Cu(II)浓度。
步骤七:设置对照,即:MFCs反应器、阳极液组成与前述过程完全相同,阴极液中除不含有10 mg/L的CuCl2外,其它均与上述MFCs一致。该条件下的Co(III)浸出归因于无Cu(II)催化的MFCs浸取钴酸锂过程。
本实施事例的MFCs的浸出钴酸锂中Co(III)发生的反应如式(1)所示,钴浸出率的时间变化过程如图2所示;阴极库仑效率随时间变化如图3所示;系统电能输出如图4所示;系统pH的时间变化如图5所示;系统对酸的有效利用率如图6所示。钴浸出率、阴极库仑效率、酸的有效利用率的计算方法如式(2)-(4)所示。
Ct,Co(II):反应器运行t时刻的阴极液中Co(II)浓度(mmol/L);C0,H+:初始阴极液中氢离子浓度(mmol/L);Ct,H+:反应器运行t时刻的阴极液中氢离子浓度(mmol/L);200:初始钴酸锂浓度(mg/L);98:钴酸锂的摩尔质量(mg/mmol);0.1:阴极液体积(L);0.001:量纲换算(mol/mmol); 1:每摩尔Co(III)还原为Co(II)需要的电子数(mol/mol);4: 每毫摩尔Co(III)所需消耗的氢离子的物质的量(mmol/mmol);96485:每摩尔库仑量(C/mol);i:第i个时间间隔;Ui:第i个时间间隔下的系统输出电压(V);R:系统外阻,200 Ω;ti:间隔时间,30 min;60:量纲换算(s/min)。
结果:随着反应时间的延长,有Cu(II)存在的MFCs与对照组的Co(II)浓度均逐渐升高(图2),但前者的钴浸出率显著高于后者。在时间为12 h时,Cu(II)催化的钴浸出率已达47.7 ± 1.6%,而无铜催化的钴仅浸出15.5 ± 0.2%,提高208%(图2),表明MFCs阴极中Cu(II)加快和促进了Co(III)的浸出和还原。相应地,前者的阴极库仑效率由3h时的81.9 ± 2.8%逐渐降低为12 h时的62.6 ± 2.6%(图3);而后者的阴极库仑效率则由3 h时的38.3 ± 8.2%降低为12 h时的36.1 ± 5.3%(图3),表明Cu(II)提高MFCs阴极库仑效率。Cu(II)还提高MFCs开路电压和电能输出(图4):与无Cu(II)存在的对照相比(开路电压0.87 V;最大功率0.32 W/m3),Cu(II)的存在使开路电压达1.02 V,最大功率0.74 W/m3,电能输出提高131%。随着钴的不断浸出,有Cu(II)或无Cu(II)的MFCs系统pH均逐渐升高,但至12 h时,前者增长幅度低于后者(图5)。Cu(II)存在的MFCs的较高钴浸出速率、较小pH变化,使其酸的有效利用率比无Cu(II)存在MFCs提高70.7%(图6)。MFCs运行12 h时,阴极液中Cu(II)由初始的10 mg/L降低为9.2mg/L,归因于电极的吸附和对Cu(II)的还原。将此“母液”滴入HCl调整pH至2.0,浸取负载200 mg/L钴酸锂颗粒的新电极,5个间歇运行周期后Cu(II)浓度降低至5.4 mg/L,钴酸锂浸取率由第1周期的47.7 ± 1.6%降低至第5周期的40.3 ± 1.8%。因此,催化剂铜最终附着于阴极电极,而钴以Co(II)存留于液相,避免了铜对钴的污染。
Claims (6)
1.一种提高微生物燃料电池浸出钴酸锂中Co(III)的方法,其特征在于,微生物燃料电池的阳极室,装有电化学活性微生物以及阳极液;微生物燃料电池的阴极室,装有阴极液和钴酸锂颗粒;阳极室接种污水处理厂的澄清池污泥作为电化学活性微生物;阴极液为含有CuCl2的无机酸溶液;阴极和阳极电极均为石墨材料。
2.根据权利要求1所述的方法,其特征在于,所述的澄清池污泥的pH: 6.8-7.0;电导率: 0.80-0.93 mS/cm;悬浮性固形物: 30-35 g/L;化学需氧量(COD): 150-300 mg/L。
3.根据权利要求1或2所述的方法,其特征在于,所述的阳极液成分为:12.0 mM乙酸钠;5.8 mM NH4Cl;1.7 mM KCl;17.8 mM NaH2PO4?H2O;32.3 mM Na2HPO4;矿质元素:12.5 mL/L ,其组成为MgSO4: 3.0 g/L;MnSO4?H2O: 0.5 g/L;NaCl: 1.0 g/L;FeSO4?7H2O: 0.1 g/L;CaCl2?2H2O: 0.1 g/L;CoCl2?6H2O: 0.1 g/L;ZnCl2: 0.13 g/L;CuSO4?5H2O: 0.01 g/L;KAl(SO4)2?12H2O: 0.01 g/L;H3BO3: 0.01 g/L;Na2MoO4: 0.025 g/L;NiCl2?6H2O: 0.024 g/L;Na2WO4?2H2O: 0.024 g/L;维生素: 12.5 mL/L ,其组成为维生素B1: 5.0 g/L;维生素B2: 5.0 g/L;维生素B3: 5.0 g/L;维生素B5: 5.0 g/L;维生素B6: 10.0 g/L;维生素B11: 2.0 g/L;维生素H: 2.0 g/L;对氨基苯甲酸: 5.0 g/L;硫辛酸: 5.0 g/L;氨基三乙酸: 1.5 g/L。
4.根据权利要求1或2所述的方法,其特征在于,所述的无机酸溶液为盐酸溶液。
5.根据权利要求3所述的方法,其特征在于,所述的无机酸溶液为盐酸溶液。
6.根据权利要求1或2或5所述的方法,其特征在于,所述的石墨材料为碳毡;钴酸锂颗粒为8~9 μm。
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