CN113145066A - 一种改性蛭石吸附剂的制备 - Google Patents

一种改性蛭石吸附剂的制备 Download PDF

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CN113145066A
CN113145066A CN202110330791.4A CN202110330791A CN113145066A CN 113145066 A CN113145066 A CN 113145066A CN 202110330791 A CN202110330791 A CN 202110330791A CN 113145066 A CN113145066 A CN 113145066A
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孟子霖
赵世凤
夏彩凤
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Shandong University of Technology
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Abstract

本发明提供了一种改性蛭石吸附剂的制备方法及其应用，所述改性蛭石吸附剂是通过共沉淀方法，以蛭石为负载材料，依靠两种物质层板的电荷性质将类水滑石负载在蛭石表面。该改性蛭石吸附剂主要用于对废水溶液中的铜离子、铅离子、锌离子三种重金属离子的去除。类水滑石改性蛭石吸附剂对铜离子、铅离子、锌离子的吸附量达到125 mg/g、85 mg/g、148 mg/g，蛭石对铜离子、铅离子、锌离子的吸附量达到19 mg/g、15 mg/g、20 mg/g。内扩散和二级动力学模型较好的描述了重金属离子吸附的动力学研究。类水滑石改性蛭石吸附剂对铜离子、铅离子、锌离子吸附等温线数据均与Freundlich模型吻合较好。该吸附剂具有良好的重金属吸附效果且操作过程简单，成本较低，无毒无害等特点。

Description

一种改性蛭石吸附剂的制备
技术领域
本发明涉及含重金属离子废水处理的技术领域，具体涉及采用类水滑石改性蛭石，用于处理废水中的铜离子、铅离子和锌离子的吸附剂。
背景技术
20世纪以来，科技的发展促进经济的发展的同时，造成了生态环境的污染。含重金属的污染废水主要来源于金属的冶炼、化工企业无节制排放和矿山的不规范开采。重金属污染具有长期性、不可逆性等特点，若含有重金属的废水未经处理而直接排放，会严重威胁到生态环境及人类健康。
鉴于重金属化学性质稳定的特点，一般只有通过将其转移或者改变其形态的方法去除其危害。目前处理重金属主要通过沉降法、氧化还原法、吸附法和生物处理法。
蛭石在自然界中主要以镁和硅形式存在的一类黏土。蛭石化学式为(Mg,Fe,Al)8(Si, Al)4O10(OH)2·4H2O。蛭石属于典型的2:1型层状硅铝酸盐,蛭石层板中硅氧四面体的的四价硅被三价铝取代，使层板带负电。由于阳离子交换性能，蛭石对金属离子具有一定的吸附效果，但蛭石层板的易团聚堆叠，严重影响其表面利用率。
类水滑石是一种阴离子型黏土，其层板主要成分为铝和镁,其结构通式为 [M2+1-xM3+x(OH)2]An-x/n·mH2O，其中M2+和M3+分别代表二价和三价金属阳离子，An-是层间阴离子，x是[M3+]/([M2+]+[M3+])的摩尔比。由于相似的离子半径，层板上镁离子会被铝离子取代，使得类水滑石层板带正电荷。类水滑石层板金属离子的可调变性使得类水滑石对重金属离子具有吸附效果，类水滑石层板也存在层板易团聚堆叠的缺点。
两种材料因其层板电荷性质的特点，使得蛭石容易被类水滑石改性。
综上所述，制备一种类水滑石改性蛭石吸附剂为废水溶液中重金属离子的去除提供了一种新的解决方法。
发明内容
本发明提供一种类水滑石改性蛭石吸附剂，并将其用于分离废水溶液中的铜离子、铅离子和锌离子。
本发明所提供的类水滑石改性蛭石吸附剂，其化学式为：(Mg,Fe,Al)8(Si, Al)4O10(OH)2·[Mg2+1-xAl3+x(OH)2]NO3-x·mH2O；x代表镁/铝摩尔比，x＝2，m＝8～10。
上述类水滑石改性蛭石吸附剂的制备方法通过以下技术方式实施：
将直径5～10mm的蛭石用去离子水清洗干净，干燥，置于马弗炉中于1000℃下煅烧240min，得膨胀蛭石，冷却至室温并研磨备用。
在200ml的去离子水中加入1g焙烧研磨好的蛭石，搅拌均匀后，超声4h。
向上述超声后的蛭石悬浊液中加入0.002mol九水硝酸铝、0.004mol六水硝酸镁，搅拌超声溶解均匀，并在搅拌状态下向其滴加1M氢氧化钠溶液，至pH为9.5±0.5。
陈化12h后，4000r/min离心10min、去离子水洗涤数次、70℃干燥一整夜后，得到类水滑石改性蛭石吸附剂。
上述类水滑石改性蛭石吸附剂用于吸附废水溶液中铜离子、铅离子和锌离子的具体动力学实验方法如下：
将25mL含有100mg/L重金属离子的溶液混合，然后加入50mg的类水滑石改性蛭石吸附剂，把密封的锥形瓶放到200rpm/min的摇床上，在不同的接触时间(1～200min)进行动力学研究。
上述类水滑石改性蛭石吸附剂用于吸附废水溶液中的铜离子、铅离子和锌离子的具体等温实验方法如下：
将25mL含有不同浓度重金属离子的溶液混合，然后加入50mg的复合吸附剂，把密封的锥形瓶放到200rpm/min的摇床上，统一在振荡4小时后离心(4000r/min)10min，取上清液过 0.45μm滤膜后供浓度分析。
使用元素分析仪对上述所得吸附后的溶液进行定量分析。铜离子、铅离子和锌离子的动力学部分的结果在中显示：类水滑石改性蛭石吸附剂对铜离子、铅离子和锌离子的吸附在 100～140min内达到平衡。铜离子、铅离子和锌离子的等温部分的结果在中显示，类水滑石改性蛭石吸附剂对铜离子、铅离子和锌离子的吸附量分别为125mg/g、85mg/g、148mg/g。
本发明的有益效果为：
与目前处理含重金属废水方法，如沉降法、氧化还原法和生物处理法等相比，本发明具有以下优点：操作简单，对操作技能要求不高且不易引入二次污染。
本发明对铜离子、铅离子和锌离子有较高的去除率，达到平衡的时间较短。
本发明制备的类水滑石改性蛭石吸附剂，制作成本低，为处理含铜离子、铅离子和锌离子的废水溶液提供了一种高效的分离材料。
附图说明
图1为类水滑石改性蛭石吸附剂的制备过程。
图2是类水滑石改性蛭石吸附剂、蛭石和类水滑石的XRD图。
图3为蛭石(a)与类水滑石改性蛭石吸附剂(b)的SEM图。
图4为蛭石和类水滑石改性蛭石吸附剂对铜离子吸附的动力学曲线图。
图5为蛭石和类水滑石改性蛭石吸附剂对铅离子吸附的动力学曲线图。
图6为蛭石和类水滑石改性蛭石吸附剂对锌离子吸附的动力学曲线图。
图7为蛭石和类水滑石改性蛭石吸附剂对铜离子吸附的等温曲线图。
图8为蛭石和类水滑石改性蛭石吸附剂对铅离子吸附的等温曲线图。
图9为蛭石和类水滑石改性蛭石吸附剂对锌离子吸附的等温曲线图。
具体实施方式
下面将结合附图和实施例对本发明作进一步的详细说明。
实施例1
A.将直径5～10mm的蛭石用去离子水清洗干净，干燥，置于马弗炉中于1000℃下煅烧240 min，得膨胀蛭石，冷却至室温并研磨备用。
B.在200ml的去离子水中加入1g焙烧研磨好的蛭石，搅拌均匀后，超声4h。
C.向上述超声后的蛭石悬浊液中加入0.002mol九水硝酸铝、0.004mol六水硝酸镁，搅拌超声溶解均匀，并在搅拌状态下向其滴加1M氢氧化钠溶液，至pH为9.5±0.5。
D.陈化12h后，4000r/min离心10min、去离子水洗涤数次、70℃干燥一整夜后，得到类水滑石改性蛭石吸附剂。
应用例1
将25mL含有不同浓度重金属离子的溶液混合，然后加入50mg的复合吸附剂，把密封的锥形瓶放到200rpm/min的摇床上，统一在振荡4小时后离心(4000r/min)10min，取上清液过 0.45μm滤膜后供浓度分析。
将25mL含有100mg/L重金属离子的溶液混合，然后加入50mg的类水滑石改性蛭石吸附剂，把密封的锥形瓶放到200rpm/min的摇床上，在不同的接触时间(1-200min)进行动力学研究。
使用元素分析仪对上述所得吸附后的溶液进行定量分析。铜离子、铅离子和锌离子的动力学部分的结果在图4，图5，图6中显示：类水滑石改性蛭石吸附剂对铜离子、铅离子和锌离子的吸附在100～140min内达到平衡。铜离子、铅离子和锌离子的等温部分的结果在图 7，图8和图9中显示，类水滑石改性蛭石吸附剂对铜离子、铅离子和锌离子的吸附量分别为 125mg/g、85mg/g、148mg/g。

Claims (3)

1.一种类水滑石改性蛭石吸附剂，具有三维结构，上述复合吸附剂的制备方法为：将蛭石用去离子水清洗干净，干燥备用，取适量清洗过的蛭石在马弗炉中于1000 ℃下煅烧120min，得膨胀蛭石，并研磨备用，在200 ml的去离子水中加入1 g焙烧研磨好的蛭石，搅拌均匀后，超声4 h，向上述超声后的蛭石悬浊液中加入0.002 mol九水硝酸铝、0.004 mol六水硝酸镁，搅拌超声溶解均匀，向其滴加1 M 氢氧化钠溶液，至 pH为9.5±0.5，陈化12 h后，经离心、洗涤、干燥后，得到类水滑石改性蛭石吸附剂。
2.一种权利要求1所述的类水滑石改性蛭石吸附剂对废水溶液中铜离子、铅离子和锌离子的吸附。
3.一种根据权利要求2所述的类水滑石改性蛭石吸附剂的应用，其具体应用方法是将25 mL含有不同浓度重金属离子的溶液混合，然后加入50 mg的类水滑石改性蛭石吸附剂，把密封的锥形瓶放到200 rpm/min的摇床上，统一在振荡24小时后离心(4000 r/min)10min，取上清液过0.45 µm滤膜后供浓度分析。
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CN113877519A (zh) * 2021-09-18 2022-01-04 北京化工大学 一种水滑石/蛭石复合材料及其制备方法和应用
CN116371352A (zh) * 2023-03-31 2023-07-04 北京化工大学 一种含钙水滑石-蛭石复合材料及其制备方法和应用

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