CN113304728B - 一种二次改性碳基磷吸附复合材料及其制备方法和应用 - Google Patents
一种二次改性碳基磷吸附复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种二次改性碳基磷吸附复合材料及其制备方法和应用,用铁镧双金属和阳离子表面活性剂先后二次改性多壁碳纳米管,吸附材料的制备方法。该方法包括以下步骤。该方法制备得到材料作为磷酸根吸附复合材料,在较广泛的pH(3~9)条件下对磷酸根有较高吸附量,常温下最大磷酸根吸附量约80mg/g(以P计可达约27mg/g),并且受其他阴阳离子的影响较小,1mol/L的NaOH作为最佳解吸液浓度,五次解吸循环后材料仍有较强对磷吸附能力,材料具备循环再生对磷吸附的能力,可用于去除废水和富营养化水体中的磷。
Description
技术领域
本发明涉及污水处理技术领域,具体为一种二次改性碳基磷吸附复合材料及其制备方法,以及该材料在水中吸附除磷的应用。
背景技术
传统的碳基吸附剂较便宜但对磷的吸附能力十分有限,而纳米金属类吸附剂磷吸附能力强,但易团聚导致吸附位点和比表面积降低,吸附能力不能充分发挥,且价格昂贵。利用碳基材料的大比表面积,把纳米金属负载于炭基材料上,可以达到优势互补的效果。纳米金属负载改性后的复合材料对磷的吸附能力可增大为原炭基材料的数十倍。选择合适的碳基材料和纳米金属,以及用合理的比例和方法制备出高效的磷吸附复合材料,是亟待解决的吸附除磷技术难题。
发明内容
针对上述技术问题,本发明提供一种二次改性碳基磷吸附复合材料及其制备方法和应用。
具体技术方案为:
一种二次改性碳基磷吸附复合材料的制备方法,包括以下步骤:
S1.Fe/La双金属对多壁碳纳米管进行改性
多壁碳纳米管,投加到FeCl3和LaCl3·7H2O混合液中,待其均匀混合后将溶液pH调为7,密封锥形瓶置于恒温水浴振荡器中振荡,然后在烘箱中反应,静置、过滤、洗涤,最后烘干,所得样品是一次改性碳纳米管材料;
S2.阳离子表面活性剂对Fe/La双金属改性的碳纳米管材料进行二次改性
一次改性碳纳米管材料投加到阳离子表面活性剂(十六烷基三甲基氯化铵)溶液中,密封锥形瓶置于恒温水浴振荡器振荡,然后在烘箱中反应,静置、过滤、洗涤,最后烘干,所得样品是二次改性碳纳米管磷吸附复合材料。
进一步的,S1中,多壁碳管用量分别是0.125~0.5g,投加到100mL金属总摩尔浓度为21mmol/L的FeCl3和LaCl3·7H2O混合液中,其中Fe3+和La3+的浓度比分别为7:3~9:1,溶液pH调为7~10;S2中,一次改性碳纳米管材料0.75g,阳离子表面活性剂溶液100mL,浓度为21mmol/L。
S1和S2中:
振荡条件均为,25℃,200r/min振荡24h;
烘箱中反应条件均为,80℃,反应6h。
烘干条件均为,105℃。
本发明还要求保护一种二次改性碳基磷吸附复合材料,根据上述的的制备方法所得。
该二次改性碳基磷吸附复合材料的应用,用于去除废水和富营养化水体中的磷。
本发明具有的技术效果:
该方法制备得到材料作为磷酸根吸附复合材料,在较广泛的pH(3~9)条件下对磷酸根有较高吸附量,常温下最大吸附量以P计可达约27mg/g,并且受其他阴阳离子的影响较小,在1mol/L的NaOH最佳解吸液浓度,五次解吸循环后材料仍有较强对磷吸附能力,材料具备循环再生对磷吸附的能力,可用于去除废水和富营养化水体中的磷。
附图说明
图1为实施例1中三种双金属改性的碳纳米管对P的吸附动力学;
图2为实施例2中改性CNTs质量不同对磷的吸附动力学;
图3为实施例2中不同Fe/La摩尔浓度比改性碳纳米管对磷的吸附动力学;
图4为实施例3中不同温度下优选材料C-CNTs-7Fe/3La的磷吸附等温线;
图5为实施例4中C-CNTs-7Fe/3La的pH吸附影响;
图6为实施例4中C-CNTs-7Fe/3La不同pH下金属溶出率;
图7(a)为实施例4中C-CNTs-7Fe/3La的共存阳离子吸附影响;
图7(b)为实施例4中C-CNTs-7Fe/3La的共存阴离子吸附影响;
图8(a)为实施例5中解吸液浓度对磷吸附饱和C-CNTs-7Fe/3La的解吸影响;
图8(b)为实施例5中在1mol/L NaOH解吸液下对磷吸附饱和C-CNTs-7Fe/3La的五次循环再生。
具体实施方式
结合实施例说明本发明的具体技术方案。
除图4优选材料C-CNTs-7Fe/3La的磷吸附等温线,其他图3中吸附条件均为,初始浓度均为10mg/L的KH2PO4溶液100mL,复合材料投加量0.5g/L,磷吸附量q(mg/g)以磷酸根计。
实施例1
双金属种类对比案例:称取1g多壁碳纳米管,分别投加到100mL金属总摩尔浓度为21mmol/L的Fe/La、Mg/La、Fe/Mg双金属离子溶液中,金属离子以1:1的摩尔比,待其均匀混合后将溶液pH调为7,密封锥形瓶置于恒温水浴振荡器中以25℃、200r/min振荡24h,然后在80℃烘箱中反应6h,静置、过滤、洗涤,最后在105℃下烘干,所得样品是三种一次改性碳纳米管材料。
如图1所示,以未双金属改性的碳纳米管为参照,对比了三种经双金属改性的碳纳米管对P的吸附量。可见双金属改性碳纳米管材料中,Fe/La改性的碳纳米管P吸附效果最好。
实施例2
复合材料的制备方法,包括以下步骤:
S1.Fe/La双金属对多壁碳纳米管进行改性
分别称取0、0.125、0.25、0.5g多壁碳纳米管,分别投加到100mL金属总摩尔浓度为21mmol/L的FeCl3和LaCl3·7H2O混合液中,其中Fe3+和La3+的浓度比为0:10、1:9、3:7、5:5、7:3、9:1、10:0;待其均匀混合后将溶液pH调为7,密封锥形瓶置于恒温水浴振荡器中以25℃、200r/min振荡24h,然后在80℃烘箱中反应6h,静置、过滤、洗涤,最后在105℃下烘干,所得样品是一次改性碳纳米管材料CNTs-Fe/La。
S2.阳离子表面活性剂对Fe/La双金属改性的碳纳米管材料进行二次改性
称取0.75g已Fe/La双金属改性的碳纳米管材料,分别投加到100mL浓度为21mmol/L的十六烷基三甲基氯化铵溶液,密封锥形瓶置于恒温水浴振荡器中以25℃、200r/min振荡24h,在80℃烘箱中反应6h,静置、过滤、洗涤,最后在105℃下烘干,所得样品是二次改性碳基磷吸附复合材料。
用CTAC对一次改性碳纳米管材料CNTs-Fe/La进行二次改性,复合材料的P吸附能力提高进一步提高约15%。
如图2和图3,制备条件中碳管用量和Fe/La双金属摩尔浓度比对复合材料P吸附能力的比较。可见多壁碳管用量0.25~0.5g,Fe/La双金属摩尔浓度比例7:3~9:1时,材料效果好。
实施例3
二次改性碳管制得复合材料制备方法:
当0.25g的碳管,Fe/La为7:3,在中性条件下制备,其他条件同实施例2,得到的复合材料C-CNTs-7Fe/3La。
对磷酸根的吸附等温线具体做法:
100mL浓度梯度为1、5、8、10、15、20、30、50、80、100、150mg/L的KH2PO4溶液,C-CNTs-7Fe/3La的投加量为0.5g/L,分别加入各个聚乙烯塑料瓶中,每个浓度三组平行试验。在15℃、25℃、35℃条件下,150r/min的摇床中震荡反应,密封振荡待其达到吸附平衡,取上清液过0.45μm水系微孔滤膜,测定并计算磷浓度及其吸附平衡量。
由图4可见,常温下该材料最大吸附量以磷酸根计可达80mg/g,若以P计约27mg/g。
实施例4
实施案例3中所得的复合材料C-CNTs-7Fe/3La在不同环境条件下的应用效果,以及材料稳定性。实验条件保持为0.05g复合材料,加入100mL质量浓度为10mg/L的KH2PO4溶液。酸碱适应性实验中,调节反应液的pH为3、5、7、9、11。离子共存实验中,加入0、1、10mmol/L阳离子或阴离子与磷酸根共存。密封振荡待其达到吸附平衡。
如图5和图6结果显示:在pH3~9,材料对P的吸附效果较好,中性pH吸附效果尤佳;材料能适用于10mmol/L以下常见阳离子或阴离子与P共存的情况下。如图7(a)和图7(b),材料在较广泛的酸碱度溶液中比较稳定,Fe3+和La3+溶出率均低于7%。
实施例5
实施案例3中所得的复合材料C-CNTs-7Fe/3La的再生和可循环利用性。使复合材料在中性条件下对磷吸附达到饱和,记为第一次吸附饱和的单位材料吸附量q0(mg/g),用浓度分别为0.01、0.1、1mol/L的NaOH溶液为解吸液,对吸附后的复合材料进行磷酸根解吸,计算解吸率d(%),见公式(1);将解吸后的复合材料滤出、洗净、重新烘干,再次在同样吸附条件下对磷酸根吸附达到饱和,计算再生吸附率r(%),见公式(2)。结果见图8(a)。其中,用1mol/L的NaOH解吸液解吸再生的样品组,重复5次上述吸附解吸过程,结果见图8(b)。
其中,md是解吸掉的吸附质质量,m0是当次解吸前复合材料上的吸附质质量,qn(mg/g)是吸附剂再生后的单位材料吸附量(n为再生次数)。q0(mg/g)是第一次饱和单位材料吸附量。
如图8(b),吸附后的复合材料能在碱溶液中解吸再生。其中1mol/L NaOH解吸液解吸再生性能最好,随着再生次数增加,材料的解吸率d和再生吸附率r皆呈降低趋势,但5次吸附解吸循环后仍有较强的磷吸附能力,约为第一次饱和单位材料吸附量的一半。
Claims (4)
1.一种二次改性碳基磷吸附复合材料的制备方法,其特征在于,包括以下步骤:
S1. Fe/La双金属对多壁碳纳米管进行改性
多壁碳纳米管,投加到FeCl3和LaCl3·7H2O混合液中,待其均匀混合后将溶液pH调为7,密封锥形瓶置于恒温水浴振荡器中振荡,然后在烘箱中反应,静置、过滤、洗涤,最后烘干,烘箱中反应条件为, 80 ℃,反应6 h;所得样品是一次改性碳纳米管材料;
S1中,多壁碳管用量是0.125~0.5 g,投加到100 mL金属总摩尔浓度为21 mmol/L的FeCl3和LaCl3·7H2O混合液中,其中 Fe3+和La3+的浓度比分别为7:3~9:1;
S2.阳离子表面活性剂对Fe/La双金属改性的碳纳米管材料进行二次改性
一次改性碳纳米管材料投加到十六烷基三甲基氯化铵阳离子表面活性剂溶液中,密封锥形瓶置于恒温水浴振荡器振荡,然后在烘箱中反应,烘箱中反应条件为, 80 ℃,反应6h;静置、过滤、洗涤,最后烘干,所得样品是二次改性碳基磷吸附复合材料;
S2中,一次改性碳纳米管材料0.75 g,阳离子表面活性剂溶液100 mL,浓度为 21mmol/L。
2.根据权利要求1所述的一种二次改性碳基磷吸附复合材料的制备方法,其特征在于,S1和S2中:
振荡条件均为,25 ℃,200 r/min 振荡 24 h;
烘干条件均为,105 ℃。
3.一种二次改性碳基磷吸附复合材料,其特征在于,根据权利要求1或2所述的制备方法所得。
4.根据权利要求3所述的一种二次改性碳基磷吸附复合材料的应用,其特征在于,用于去除废水和富营养化水体中的磷。
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