CN113351153A - 一种MgFe-LDO-MnO2复合材料的制备方法及其应用 - Google Patents
一种MgFe-LDO-MnO2复合材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种MgFe‑LDO‑MnO2复合材料的制备方法及其应用,属于环境功能材料制备和重金属离子治理技术领域。即利用一定量Mg(NO3)2·6H2O和Fe(NO3)3·9H2O配置的金属混合溶液,在60℃、搅拌条件下滴加NaOH碱液,保持pH为10~12,滴加结束后继续剧烈搅拌4h,再70~80℃水浴陈化24~48h后,室温搅拌条件下滴加KMnO4后继续剧烈搅拌4h,滴加MnCl2·4H2O后剧烈搅拌2h,室温下老化12h,经过离心、洗涤、干燥、研磨后得到MgFe‑LDH‑MnO2复合材料,不同温度下煅烧后得到具有超强吸附锁定性能的MgFe‑LDO‑MnO2复合材料。该制备方法过程简单,操作方便,条件温和,制得的复合材料对于水中的As(Ⅲ)和Pb2+吸附能力强,可分别应用于废水中阴离子和阳离子的去除,且具有广泛的应用前景。
Description
技术领域
本发明属于环境功能材料制备和重金属离子治理技术领域,特别涉及一种 MgFe-LDO-MnO2复合材料的制备方法及其应用。
背景技术
水体重金属离子污染一直是人们密切关注的对象,且重金属在自然界中很难被降解,他们会随着人类的活动和食物链,进入人体和动物体内,即使在微量水平下也能对其健康造成危害。其中铅是工业废水中典型的有毒重金属阳离子,主要通过皮肤、消化道和呼吸道进入体内,导致贫血、神经功能障碍、肾脏损害和其他疾病。而类金属砷则是一种具有剧毒性和致癌性的环境污染物,已被国际癌症研究中心列为一类致癌物。据世界卫生组织官员公布,全球至少有5000多万人口正面临着地方性砷中毒的威胁。
目前,对于含重金属废水的处理方法主要有化学沉淀法、离子交换法、吸附法、生物法等,其中吸附法因成本低、操作简单、效率高等优点而被广泛应用于重金属废水处理中。选择合适的吸附剂对于快速、高效去除重金属离子非常重要,常见的吸附剂有活性炭、硅胶材料、粘土矿物等无机吸附材料,纤维素基、壳聚糖基、木质素基、淀粉基等天然高分子吸附材料,还包括细菌、藻类在内的生物吸附材料,此外飞灰、炉渣等工业废弃物也作为吸附材料应用于含重金属废水的处理中。但许多吸附剂都因吸附容量低,且吸附效果受环境条件影响明显、易受其他离子竞争吸附抑制、再生效果差等,从而不能满足实际需求。针对上述现状,研发廉价、高效的吸附材料已成为国内外学者研究的重点之一。
层状双氢氧化物(Layered double hydroxides,LDHs),是一种具有巨大比表面积和较高阴离子交换容量的、易于人工合成的、具有层状结构的多金属化合物,其通式可表示为M=metal,A=anion,其中 M2+、M3+分别代表二价(Ca2 +、Mg2+、Zn2+、Mn2+和Ni2+等)以及三价(Al3+、Fe3+和Cr3+等)金属阳离子,An-表示可交换的层间阴离子(如Cl-、NO3-、CO3 2-等), x代指层板电荷密度,为M3+/(M2++M3+)的摩尔比值,其范围是0.17-0.33, m为层间结晶水的摩尔数,其值可由m=1-Nx/n得到,式中N为阴离子占据的位置数目,n为阴离子的电荷数。大量实验证明,层状金属氢氧化物及其复合材料能作为吸附剂去除水中的重金属离子,且吸附效果显著,同时通过煅烧手段得到双金属氧化物(Layered double oxides,LDOs),从而提高其对重金属的吸附性能。利用LDHs层间阴离子交换作用对复合材料合成过程中元素进行固定的研究报道较为少见。此外,MnO2是含锰元素材料中最重要的化合物之一,在土壤和环境沉淀物中最常见的锰化合物为δ型的MnO2,这种形态存在的MnO2因其具有细小的颗粒,晶化度不高,而氧化吸附性能强,能够影响着环境中污染物的迁移转化作用,常被用于污染废水的修复。将锰氧化物与LDHs复合能有效的提高对重金属离子的吸附能力,可作为吸附剂去除废水中重金属离子,是一类理想的吸附材料。因此,针对重金属污染问题,本研究以MgFe-LDH为前驱体,将其负载上二氧化锰研制出MgFe-LDH-MnO2复合材料,在400~600℃条件下煅烧4~6h得到具有超强吸附锁定性能MgFe-LDO-MnO2复合材料。以上材料的制备及其在重金属污染水体中的应用为实际重金属污染应急处理提供了新的思路和技术支持,对环境可持续发展具有非常重要的现实意义。
发明内容
本发明的目的是提供一种MgFe-LDO-MnO2复合材料的制备方法及其应用。以硝酸镁和硝酸铁为混合金属盐溶液,以氢氧化钠碱溶液,采用共沉淀法制备 MgFe-LDH材料,将其负载上锰化合物后,400~600℃煅烧4~6h后得到一种对水体中As(Ⅲ)和Pb2+具有高效去除能力的MgFe-LDO-MnO2复合材料。
本发明所提供的制备MgFe-LDO-MnO2复合材料的具体步骤如下:
(1)将总金属摩尔浓度为0.06~0.1mol/L的混合金属盐加到盛有200ml超纯水的烧杯中,混合均匀后放到磁力搅拌器上,在60℃、剧烈搅拌条件下滴加碱液NaOH,滴加结束后保持pH为10~12继续在60℃条件下剧烈搅拌4h后,所得混合物在70~80℃条件下水浴老化24~48h;
(2)将步骤(1)中所得沉淀物冷却到室温后,在剧烈搅拌条件下缓慢滴入200mLKMnO4,再剧烈搅拌4h;
(3)室温、搅拌条件下向步骤(2)混合溶液中缓慢滴入200mL MnCl2,剧烈搅拌2h后,室温下水浴老化12~24h;
(4)将步骤(3)所得沉淀物用超纯水洗涤3~6次,在75℃条件下干燥24~48 小时,最后研磨并过200目筛,即制得MgFe-LDH-MnO2复合材料;
(5)将步骤(4)中MgFe-LDH-MnO2复合材料在400~600℃条件下煅烧4~6 小时,即得MgFe-LDO-MnO2复合材料。
本发明提供一种利用上述MgFe-LDO-MnO2复合材料分别应用于对水中 As(Ⅲ)和Pb2+的吸附锁定,其特征为:所述步骤(1)中混合金属盐溶液Mg2+/Fe3+=(2~4):1,(Mg2++Fe3 +)/Mn=(6~10):1。
步骤(1)所述混合金属盐溶液和碱溶液的滴加方式为共沉淀法。其中碱液 NaOH摩尔浓度为0.3~0.5mol/L。
本发明的优点在于:制备方法过程简单,操作方便,条件温和,所制得的 MgFe-LDO-MnO2复合材料对于水中As(Ⅲ)和Pb2+具有超强的去除能力,可用于废水重金属离子的去除,且具有广泛的应用前景。
附图说明
图1为本发明实施例中制备的MgFe-LDO-MnO2(400℃)复合材料的扫描电镜图。
图2为本发明实施例中制备的MgFe-LDO-MnO2(400℃)复合材料的X- 射线衍射图谱。
图3为本发明实施例中制备的MgFe-LDO-MnO2复合材料(400~600℃煅烧)对As(Ⅲ)吸附去除率变化图。
图4为本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料在不同初始pH值下对As(Ⅲ)吸附去除率变化图。
图5为本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料在pH=5时,投加量对As(Ⅲ)吸附去除率变化图。
图6为本发明实施例中制备的MgFe-LDO-MnO2复合材料(400~600℃煅烧)对Pb2+吸附去除率变化图。
图7为本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料在不同初始pH值下对Pb2+吸附去除率变化图。
图8为本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料在pH=5时,投加量对Pb2+吸附去除率变化图。
具体实施方式
实施例1:
制备MgFe-LDH-MnO2、MgFe-LDO-MnO2复合材料:
(1)将总金属摩尔浓度为0.08mol/L的混合金属盐(Mg2+/Fe3+=3:1)加到盛有200ml超纯水的烧杯中,混合均匀后放到磁力搅拌器上,在60℃、剧烈搅拌条件下滴加0.4mol/L的NaOH碱液,保持pH为10.5,继续在60℃条件下剧烈搅拌4h后,所得混合物在80℃条件下水浴老化48h;
(2)将步骤(1)中所得沉淀物冷却到30℃后,在剧烈搅拌条件下缓慢滴入 200mL浓度为4mmol/L的KMnO4,再保持30℃剧烈搅拌4h;
(3)30℃、搅拌条件下向步骤(2)混合溶液中缓慢滴入200mL浓度为6mmol/L的MnCl2,剧烈搅拌2h后,室温下水浴老化12h;
(4)将步骤(3)所得沉淀物用超纯水洗涤3~6次,在75℃条件下干燥24小时,最后研磨并过200目筛,即制得MgFe-LDH-MnO2复合材料;
(5)将步骤(4)中MgFe-LDH-MnO2复合材料在400~600℃条件下煅烧5小时,即得MgFe-LDO-MnO2复合材料。
实施例2:
图1为本实施例所制备的MgFe-LDO-MnO2(400℃煅烧)复合材料的SEM 图(采用场发射扫描电子显微镜(SEM,JGM-1900-F)表征)。
图2为本实施例所制备的MgFe-LDO-MnO2(400℃煅烧)复合材料的XRD 图(采用X射线衍射仪(XRD,X’Pert3 Powder)表征)。
实施例3:
用本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2复合材料进行去除As(Ⅲ)的吸附实验。
(1)分别称取0.03g本实施例中制得的MgFe-LDO-MnO2(400~600℃煅烧) 复合材料置于一系列50mL塑料离心管中,加入30mL浓度为50mg/L的As(Ⅲ) 溶液(原pH),在温度为25℃,转速为160rpm的恒温振荡器中震荡至平衡后,用0.22μm的滤膜过滤,用电感耦合等离子体质谱仪测定As(Ⅲ)的浓度。结果如图3所示。
(2)分别称取0.03g本实施例中制得的MgFe-LDH-MnO2、MgFe-LDO-MnO2 (400℃煅烧)复合材料置于一系列50mL塑料离心管中,加入30mL浓度为 50mg/L的As(Ⅲ)溶液,用0.1mol/L的HCl或NaOH溶液调节pH到设定值(2 ~12),在温度为25℃,转速为160rpm的恒温振荡器中震荡至平衡后,用0.22 μm的滤膜过滤,用电感耦合等离子体质谱仪测定As(Ⅲ)的浓度。结果如图4所示。
(3)分别称取150、300、450、600、750、900mg本实施例中制得的 MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料置于一系列50mL 塑料离心管中,加入30mL已调节好的pH=5.0、浓度为50mg/L的As(Ⅲ)溶液 (0.1mol/L的HCl或NaOH溶液调节pH),在温度为25℃,转速为160rpm 的恒温振荡器中震荡至平衡后,用0.22μm的滤膜过滤,电感耦合等离子体质谱仪测定As(Ⅲ)的浓度。结果如图5所示。
实施例4:
用本发明实施例中制备的MgFe-LDH-MnO2、MgFe-LDO-MnO2复合材料进行去除Pb2+的吸附实验。
(1)分别称取0.03g本实施例中制得的MgFe-LDO-MnO2(400~600℃煅烧) 复合材料置于一系列50mL塑料离心管中,加入30mL浓度为500mg/L的Pb2+原pH溶液,在温度为25℃,转速为160rpm的恒温振荡器中震荡至平衡后,用0.22μm的滤膜过滤,用电感耦合等离子体质谱仪测定Pb2+的浓度。结果如图 6所示。
(2)分别称取0.03g本实施例中制得的MgFe-LDH-MnO2、MgFe-LDO-MnO2 (400℃煅烧)复合材料置于一系列50mL塑料离心管中,加入30mL浓度为 500mg/L的Pb2+溶液,用0.1mol/L的HCl或NaOH溶液调节pH到设定值(2~ 8),在温度为25℃,转速为160rpm的恒温振荡器中震荡至平衡后,用0.22μm 的滤膜过滤,用电感耦合等离子体质谱仪测Pb2+的浓度。结果如图7所示。
(3)分别称取150、300、450、600、750、900mg本实施例中制得的 MgFe-LDH-MnO2、MgFe-LDO-MnO2(400℃煅烧)复合材料置于一系列50mL 塑料离心管中,加入30mL已调节好的pH=5.0、浓度为500mg/L的pb2+溶液(0.1 mol/L的HCl或NaOH溶液调节pH),在温度为25℃,转速为160rpm的恒温振荡器中震荡至平衡后,用0.22μm的滤膜过滤,电感耦合等离子体质谱仪测定 Pb2+的浓度。结果如图8所示。
Claims (5)
1.一种MgFe-LDO-MnO2复合材料的制备方法,其特征在于具体步骤为:
(1)将总金属摩尔浓度为0.06~0.1mol/L的混合金属盐加到盛有200ml超纯水的烧杯中,混合均匀后放到磁力搅拌器上,在60℃、剧烈搅拌条件下滴加碱液NaOH,滴加结束后保持pH为10~12继续在60℃条件下剧烈搅拌4h后,所得混合物在70~80℃条件下水浴老化24~48h;
(2)将步骤(1)中所得沉淀物冷却到室温后,在剧烈搅拌条件下缓慢滴入200mLKMnO4,再剧烈搅拌4h;
(3)室温、搅拌条件下向步骤(2)混合溶液中缓慢滴入200mL MnCl2,剧烈搅拌2h后,室温下水浴老化12~24h;
(4)将步骤(3)所得沉淀物用超纯水洗涤3~6次,在75℃条件下干燥24~48小时,最后研磨并过200目筛,即制得MgFe-LDH-MnO2复合材料;
(5)将步骤(4)中MgFe-LDH-MnO2复合材料在400~600℃条件下煅烧4~6小时,即得MgFe-LDO-MnO2复合材料。
2.根据权利要求1所述的一种MgFe-LDO-MnO2复合材料的制备方法,其特征在于:所述步骤(1)中混合金属盐溶液Mg2+/Fe3+=(2~4):1,(Mg2++Fe3+)/Mn=(6~10):1。
3.根据权利要求1或2所述的一种MgFe-LDO-MnO2复合材料的制备方法,其特征在于:步骤(1)所述混合金属盐溶液和碱溶液的滴加方式为共沉淀法;其中碱液NaOH浓度为0.3~0.5mol/L。
4.根据权利要求1或2或3所述的一种MgFe-LDO-MnO2复合材料的制备方法,其特征在于:煅烧温度为400~600℃,煅烧时间为4~6小时。
5.一种如权利要求1或2或3或4所述制备方法制备的MgFe-LDO-MnO2复合材料的应用,其特征在于该MgFe-LDO-MnO2复合材料应用于对水中As(Ⅲ)和Pb2+的吸附。
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