CN115475603A - 一种柚子皮生物碳/MgFe-LDH复合材料的制备方法及其应用 - Google Patents
一种柚子皮生物碳/MgFe-LDH复合材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种柚子皮生物碳/MgFe‑LDH复合材料的制备方法及应用，属于环境功能材料制备和重金属水污染治理技术领域。以柚子皮生物质为前驱体制备生物碳，以生物碳为模板，加入含硝酸镁、硝酸铁的金属混合溶液，在室温条件下搅拌均匀并匀速缓慢滴加NaOH溶液，保持pH为10±0.1，滴加结束后继续剧烈搅拌1h，在80℃水浴陈化24h后，经过离心、洗涤、干燥、研磨后得到柚子皮生物碳/MgFe‑LDH复合材料。该制备方法制得的材料对于水中的Cd(Ⅱ)具有较强吸附锁定能力，可用于废水重金属离子的去除，工艺简单，材料易得，具有广泛的应用实用性和推广性。
Description
技术领域
本发明属于环境功能材料制备和重金属污染治理技术领域，特别涉及一种柚子皮生物碳/MgFe-LDH复合材料的制备方法及其应用于吸附锁定重金属Cd(Ⅱ)的技术。
背景技术
镉在自然界分布广泛，是最有毒的环境污染物之一，是一种慢性强效肾脏毒素，也是一种主要的致癌物。镉污染的主要来源是电镀、采矿、冶炼、染料、电池和化学工业的废水。即使是低浓度的镉污染废水，也会通过水-作物-人的接触途径，对人类健康构成重大威胁。水中的重金属主要以颗粒状态存在、迁移和转化，其过程复杂多样，几乎包括水中的各种物理、化学和生物过程。目前，镉污染废水的处理方法有吸附法、膜分离法、化学沉淀法、电化学法等。其中，膜分离法有节能、高效以及无二次污染的优点，但膜分离的膜组件难以设计且成本过高，需要大量的投资等；化学沉淀法工艺较成熟，具有去除范围广、效率高、经济简便的优点，但需要投加大量化学药剂，其沉淀会存在二次污染问题；大部分的生物吸附剂对低浓度重金属废水的处理效率高，但不适用于高金属含量的废水处理；在众多镉污染废水处理方法中，吸附法因具有操作简单、去除效率高、吸附材料具可再生性等优点而广泛应用。其核心在于吸附剂的选择，许多高效吸附剂都因昂贵的价格而被限制应用，因此寻找各种天然、廉价、高效的吸附材料成为国内外研究重点。
层状双氢氧化物(layered double hydroxide，LDH)是一类阴离子型层状功能材料，常被称为阴离子黏土、水滑石或类水滑石，是目前研究最多的粘土材料之一。由于其具有层间阴离子交换性、酸碱性、记忆效应以及良好的催化性能和热稳定性等特性，可以作为高性能催化材料、吸附材料、阻隔材料、生物材料、分离材料等应用于国民经济诸多行业。其通式为[M1-x 2+Mx 3+(OH-)2]x+(Ax/n)n-·mH2O，由二价金属离子M2+和三价金属离子M3+的羟基八面体构成主层结构，主层结构之间穿插阴离子，x代指层板电荷密度，为M3+/(M2++M3+)的摩尔比值，一般认为x在0.17～0.33内可得到单相LDH。经常用于合成LDH的二价和三价金属阳离子分别有Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Zn2+和Al3+、Mo3+、Fe3+、Co3+、Cr3+、Ga3+等。重金属Cd(II)可与LDHs层间大量的阴离子及羟基基团发生反应而得以去除，其作为吸附材料具有无毒特性对环境非常友好，并可以作为可再生吸附剂循环使用。有实验研究表明LDH-Cl对Cd(II)的最佳吸附量为61mg/g(Chem.Eng.J.2015,269,221-228)，MgAl-LDH对Cd(II)的最佳吸附量为108mg/g(Sep.Purif.Technol.2018,192,36-45)，NiAl-LDH对Cd(II)的最佳吸附量为10.67mg/g(J.Phys.Chem.Solids.2017,110,195-201)。然而重金属Cd(II)在LDH上的吸附锁定主要依靠沉淀作用，受到环境及材料表面pH值的影响较大，导致Cd(II)吸附稳定性差。此外，LDH表面通常带正电，会与阳离子型污染物Cd(II)发生静电排斥作用降低了对Cd(II)的吸附锁定作用，严重制约了LDH在重金属阳离子如Cd(II)上的吸附锁定作用。
为了进一步提高LDH对重金属阳离子Cd(II)的吸附性能，可通过与其他材料进行复合，使其表面物理化学性能得以改变来提高吸附性能。生物碳材料具有来源广泛、孔结构优良、活性中心多、表面电荷稳定等优点，可以作为LDHs表面功能化的理想材料。同时，与水滑石相结合，生物碳材料可以有效地减少LDH在成核过程中的团聚，还可以弥补LDHs的分散性，水力传导性及导电性差问题。然而许多高效的碳材料都因价格昂贵而被限制应用，针对这种现状，寻找各种天然、廉价、高效的碳源是开发研制生物碳/LDH复合材料的关键性问题之一。我国广西地区盛产柚子等水果，其农业废弃物柚子皮具有较大的比表面积，将其碳化后转化为柚子皮生物碳，可以达到资源充分利用及环境无危害的目的。将柚子皮生物碳与LDH复合在一起，制备出柚子皮生物碳/LDH复合材料，使其达到高效吸附含镉废水。因此，将生物碳材料与LDH结合成具有新颖结构和先进表面性能的复合材料具有实际工程利用意义。
发明内容
本发明的目的是提供一种柚子皮生物碳/MgFe-LDH复合材料的制备方法及其应用。以柚子皮生物碳为模板，以硝酸铁、硝酸镁为混合金属溶液，以氢氧化钠为碱溶液，采用共沉淀法，得到一种对水体中Cd(Ⅱ)具有高效去除能力的柚子皮生物碳/MgFe-LDH复合材料。对其物相与结构、成分组成以及形貌特征进行表征，并应用与水体中Cd(Ⅱ)的吸附处理，获得一种操作简单、廉价、可高效去除Cd(Ⅱ)的吸附材料。
本发明所提供的制备柚子皮生物碳/MgFe-LDH复合材料的具体步骤如下：
1.生物碳的制备
将柚子皮洗净切块，置于80℃的烘箱干燥24h，用破碎机破碎后过100目筛，然后置于氮气氛围的管式炉中以5℃/min的升温速率分别在600-800℃条件下煅烧4h，冷却至室温后的产物及柚子皮生物碳。
2.柚子皮生物碳/MgFe-LDH复合材料的制备
(1)将(n(Mg2+):n(Fe3+)＝(2～3：1)的金属硝酸盐溶液与5g的柚子皮生物碳(固液比1：100(g：ml))加到装有500ml的超纯水的烧杯中，混合均匀后放置在磁力搅拌器上，在室温下剧烈搅拌并缓慢匀速滴加NaOH碱溶液至pH为10±0.1，滴加结束后在80℃条件下水浴老化24h。
(2)将步骤2所得的沉淀物用超纯水洗涤5～6次，至pH不再变化，在80℃下干燥24h，最后将所得物研磨过200目筛，即制得柚子皮生物碳/MgFe-LDH复合材料。
本发明提供一种利用上述柚子皮生物碳/MgFe-LDH复合材料应用于对水中Cd(Ⅱ)的吸附锁定，其特征在于：所述步骤1中生物碳煅烧温度优选温度为800℃，所述步骤2中混合金属盐溶液优选n(Mg2+):n(Fe3+)比例为3:1。
本发明的优点在于：制备方法过程简单，操作方便，条件温和，使用试剂少，所制备的柚子皮生物碳/MgFe-LDH复合材料对于水中Cd(Ⅱ)具有很强的去除能力，可用于废水重金属的去除，且具有广泛的应用前景。
附图说明
图1为本发明实施例中不同煅烧温度制备的柚子皮生物碳材料对不同浓度Cd(Ⅱ)溶液吸附去除率变化图。
图2为本发明实施例中制备n(Mg2+):n(Fe3+)＝2～3：1的MgFe-LDH材料的X-射线衍射图谱。
图3为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料的X-射线衍射图谱。
图4为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料的扫描电镜图。
图5为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料的红外光谱图。
图6为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料的在不同投加量下对Cd(Ⅱ)吸附去除率变化图。
图7为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料在投加量为1.5g/L时，pH对Cd(Ⅱ)吸附去除率变化图。
具体实施方式
以下结合附图及实施例对本发明作进一步描述。
实施例1：
制备柚子皮生物碳
将柚子皮洗净切块，置于80℃的烘箱干燥24h，用破碎机破碎后过100目筛，然后置于氮气氛围的管式炉中以5℃/min的升温速600-800℃条件下煅烧4h，冷却至室温后的产物即柚子皮生物碳。
实施例2：
用本发明实施例中制备的不同煅烧温度柚子皮生物碳材料进行去除Cd(Ⅱ)的吸附实验。
(1)分别称取30mg实施例1中制得的柚子皮生物碳置于一系列50mL塑料离心管中，加入浓度分别为10，25，50，75，100，125，150，175，200mg/L的Cd(Ⅱ)溶液30mL，在温度为25℃，转速为220rpm的恒温振荡器中振荡至平衡后，用0.45μm的水系滤膜过滤，用电感耦合等离子体质谱仪测定Cd(Ⅱ)的浓度。结果如图1所示。
实施例3：
制备MgFe-LDH材料：
(1)将(n(Mg2+):n(Fe3+):＝2～3:1)的金属硝酸盐加到装有500ml的超纯水的烧杯中，混合均匀后放置在磁力搅拌器上，在室温下剧烈搅拌并缓慢匀速滴加NaOH碱溶液至pH为10±0.1，滴加结束后在80℃条件下水浴老化24h。
(2)将步骤1所得的沉淀物用超纯水洗涤5～6次，至pH不再变化，在80℃下干燥24h，最后将所得物研磨过200目筛，即制得MgFe-LDH材料。图2为(n(Mg2+):n(Fe3+):＝2～3:1)MgFe-LDH的XRD图。
实施例4：
制备柚子皮生物碳/MgFe-LDH复合材料：
(1)将总金属摩尔浓度为0.3mol/L的金属硝酸盐(n(Mg2+):n(Fe3+):＝3:1)与5g的柚子皮生物碳(固液比1：100(g：ml))加到装有500ml的超纯水的烧杯中，混合均匀后放置在磁力搅拌器上，在室温下剧烈搅拌并缓慢匀速滴加NaOH碱溶液至pH为10±0.1，滴加结束后在80℃条件下水浴老化24h。
(2)将步骤1所得的沉淀物用超纯水洗涤5～6次，至pH不再变化，在80℃下干燥24h，最后将所得物研磨过200目筛，即制得柚子皮生物碳/MgFe-LDH复合材料。
实施例5：
图3为本实施例所制备的柚子皮生物碳/MgFe-LDH复合材料的XRD图。
图4为本实施例所制备的柚子皮生物碳/MgFe-LDH复合材料的SEM图。
图5为本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料的FTIR图。
实施例6：
用本发明实施例中制备的柚子皮生物碳/MgFe-LDH复合材料进行去除Cd(Ⅱ)的吸附实验。
(1)分别称取30、45、60、75、90mg本实施例中制得的柚子皮生物碳/MgFe-LDH复合材料置于一系列50mL塑料离心管中，加入浓度为300mg/L的Cd(Ⅱ)溶液30mL，在温度为25℃，转速为220rpm的恒温振荡器中振荡至平衡后，用0.45μm的水系滤膜过滤，用电感耦合等离子体质谱仪测定Cd(Ⅱ)的浓度。结果如图6所示。
(2)称取45mg本实施例中制得的柚子皮生物碳/MgFe-LDH复合材料置于一系列50mL塑料离心管中，加入已调节好pH为＝2～7、浓度为300mg/L的Cd(Ⅱ)溶液30mL(0.1mol/L的HCl或NaOH溶液调节pH)，在温度为25℃，转速为160rpm的恒温振荡器中振荡至平衡后，用0.45μm的滤膜过滤，电感耦合等离子体质谱仪测定Cd(Ⅱ)的浓度。结果如图7所示。
Claims (3)
1.一种柚子皮生物碳/MgFe-LDH复合材料的制备方法，其特征在于具体步骤为：
1)柚子皮生物碳的制备
将柚子皮洗净切块，置于80℃的烘箱干燥24h，用破碎机破碎后过100目筛，然后置于氮气氛围的管式炉中以5℃/min的升温速率在600-800℃条件下煅烧4h，冷却至室温后得到柚子皮生物碳；
2)柚子皮生物碳/MgFe-LDH复合材料的制备
(1)将n(Mg2+):n(Fe3+)＝(2～3：1)的混合金属硝酸盐溶液与5g的柚子皮生物碳(固液比1：100(g：ml))加到装有500ml的超纯水的烧杯中，混合均匀后放置在磁力搅拌器上，在室温下剧烈搅拌并缓慢匀速滴加NaOH碱溶液至pH为10±0.1，滴加结束后在80℃条件下水浴老化24h；
(2)将步骤2所得的沉淀物用超纯水洗涤5～6次，至pH不再变化，在80℃下干燥24h，最后将所得物研磨过200目筛，即制得柚子皮生物碳/MgFe-LDH复合材料。
2.根据权利要求1所述的一种柚子皮生物碳/MgFe-LDH复合材料的制备方法，其特征在于：所述步骤1)中柚子皮生物碳煅烧温度为800℃；步骤2)中混合金属盐溶液Mg2+:Fe3+＝3:1。
3.一种如权利要求1或2所述制备方法制备的柚子皮生物碳/MgFe-LDH材料的应用，其特征在于该柚子皮生物碳/MgFe-LDH复合材料应用于水中Cd(Ⅱ)的吸附。
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