CN110860271B - 一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用 - Google Patents

一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用 Download PDF

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CN110860271B
CN110860271B CN201911381247.1A CN201911381247A CN110860271B CN 110860271 B CN110860271 B CN 110860271B CN 201911381247 A CN201911381247 A CN 201911381247A CN 110860271 B CN110860271 B CN 110860271B
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徐泽忠
曹显志
王志阳
马兰兰
韩成良
谢劲松
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Abstract

一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用，涉及纳米复合粉体在脱除有机染料中的应用技术领域。SiO2/Ag2S纳米复合粉体的比表面积为5～80m2/g，是以链状Ag2S纳米颗粒为基体，通过纳米SiO2微球包覆在其表面或者嵌入到其颗粒内部而形成，吸附亚甲基蓝的吸附动力学曲线符合准一阶动力学方程，脱除亚甲基蓝规律满足Freundlich等温吸附模型。本发明采用室温共沉淀法成功制备出了SiO2/Ag2S纳米复合材料，随着SiO2胶体溶液含量的增加，SiO2/Ag2S纳米复合材料的比表面积也相应增大，SiO2/Ag2S纳米复合材料的形貌和吸附性能会发生相应改变。

Description

一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用
技术领域
本发明涉及纳米复合粉体在脱除有机染料中的应用技术领域，特别涉及一种SiO2/Ag2S 纳米复合粉体在脱除亚甲基蓝中的应用。
背景技术
众所周知，工业废水中含有大量有毒物质，如染料、重金属、持续存在的污染物等。不仅污染水体环境，还可以通过食物链危害水体中的生物及人类身体健康。亚甲基蓝(MB)是一种应用比较广泛的有机染料，也是印染废水中典型的有机污染物之一。亚甲基蓝不易降解，在流动的水中长时间存在，延缓光合活性，利用遮光抑制水生生物的生长，抗氧化和抗光解能力强，同时亚甲基蓝的致癌性、致突变性、毒性已得到证实。因此如何能够高效去除水体中的亚甲基蓝等有机染料成为人们共同关注的焦点。
目前去除废水中的有机染料主要是通过吸附法、化学沉淀法、膜分离法、电化学法等来实现，其中吸附法具有回收效率高、操作简便、多功能性、成本效益较高、适应能力强等优点而被广泛应用于废水中有机染料和重金属离子的去除等方面。而吸附剂的种类能够在一定程度上决定吸附效果，纳米SiO2微球由于特殊的结构尺寸和表面特性，较大的比表面积使其能有效吸附杂质和颗粒，常用作吸附剂和污水处理剂。而单分散的SiO2纳米微球的吸附能力有限，故制备出SiO2/Ag2S粉体能够有效提高对有机染料的吸附能力。
发明内容
为了克服现有技术中存在的技术问题，本发明的目的是提出一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用，为废水中的有机染料的去除提供一种新的替代方案。
为实现该目的，本发明采用了以下技术方案：一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用，所述SiO2/Ag2S纳米复合粉体是以链状Ag2S纳米颗粒为基体，通过纳米SiO2微球包覆在其表面或者嵌入到其颗粒内部而形成，所述SiO2/Ag2S纳米复合粉体的比表面积为5～80m2/g，所述SiO2/Ag2S纳米复合材料吸附亚甲基蓝的吸附动力学曲线符合准一阶动力学方程，脱除亚甲基蓝规律满足Freundlich等温吸附模型。
作为本发明SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用的优选技术方案，所述 SiO2/Ag2S纳米复合粉体采用室温共沉淀法法制备，具体方法为：
1)、准确称取0.1902g的硫脲和0.4245g的AgNO3固体分别溶解于25mL和50mL的去离子水中，配制成浓度分别为0.01mol/L和0.005mol/L的硫脲水溶液和AgNO3溶液；
2)、将AgNO3溶液利用微量移液器在磁性搅拌下逐滴滴加到硫脲水溶液中，形成硫脲银配合物溶液，然后往硫脲银配合物溶液中滴加6～24mL的SiO2胶体溶液，室温下反应出现黑色沉淀后停止搅拌，用去离子水和无水乙醇分离和清洗若干次，经过烘干得到SiO2/Ag2S 纳米复合粉体。
优选地，制备方法步骤2)中烘干温度为160℃。
与现有技术相比，本发明的有益效果表现在：
本发明采用室温共沉淀法成功制备出了SiO2/Ag2S纳米复合材料，并通过XRD，SEM和BET等手段对复合产物的物相、结构和吸附性能进行了表征与分析，结果表明，SiO2/Ag2S纳米复合材料是以链状Ag2S纳米颗粒为基体，通过纳米SiO2微球包覆在表面或者嵌入到颗粒内部而形成。比表面积测试结果表明，随着SiO2胶体溶液含量的增加，SiO2/Ag2S纳米复合材料的比表面积也相应增大，SiO2/Ag2S纳米复合材料的形貌和吸附性能会发生相应改变。对制备的SiO2/Ag2S纳米复合材料进行吸附动力学和热力学实验。吸附研究实验表明，SiO2/Ag2S纳米复合材料吸附亚甲基蓝的吸附动力学曲线符合准一阶动力学方程，并且SiO2/Ag2S复合材料脱除亚甲基蓝规律满足Freundlich等温吸附模型。
附图说明
图1是纯的Ag2S的XRD谱图(a)和实施例3制备的SiO2/Ag2S的XRD谱图(b)。
图2是不同含量SiO2胶体溶液所制备的SiO2/Ag2S粉体的扫描电镜图片(a、b、c)与能谱分析图片(d)。
图3是三种吸附剂的吸附-脱附等温曲线及孔径分布。
图4是三种吸附剂吸附亚甲基蓝的的吸附动力学曲线(a)和等温吸附曲线的线性拟合 (b)。
图5是三种吸附剂吸附亚甲基蓝的吸附热力学等温曲线(a、c、e)和吸附热力学等温曲线的线性拟合(b、d、f)。
具体实施方式
以下通过具体实施例进一步详细说明本发明的SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用。产物分别用X射线衍射仪(XRD)，扫描电子显微镜(SEM，SU-8010)，比表面积测试仪(BET)等进行表征。
实施例1
SiO2/Ag2S纳米复合粉体采用室温共沉淀法法制备，具体方法为：
1)、准确称取0.1902g的硫脲和0.4245g的AgNO3固体分别溶解于25mL和50mL的去离子水中，配制成浓度分别为0.01mol/L和0.005mol/L的硫脲水溶液和AgNO3溶液。
2)、将AgNO3溶液利用微量移液器在磁性搅拌下逐滴滴加到硫脲水溶液中，形成硫脲银配合物溶液，然后往硫脲银配合物溶液中滴加6mL的SiO2胶体溶液，室温下反应出现黑色沉淀后停止搅拌，用去离子水和无水乙醇分离和清洗若干次，160℃烘干，得到SiO2/Ag2S纳米复合粉体。
实施例2和3
制备步骤同实施例1，区别仅在于，SiO2胶体溶液的添加量分别为12mL、24mL。
实施例1-3制备的SiO2/Ag2S纳米复合粉体依次标记为A类吸附剂、B类吸附剂、C类吸附剂。
实施例3制备的C类吸附剂的XRD谱图如图1b所示，作为对比，图1a是纯的Ag2S 的XRD谱图。从图中可以看出复合产物的谱图与Ag2S的XRD谱图在2θ＝23°左右多了一个特征吸收峰，这段特征吸收峰与SiO2的标准谱图刚好一致，因此，制备的SiO2/Ag2S纳米复合粉体的纯度较高，无其他杂质。
图2是不同含量SiO2胶体溶液所制备的SiO2/Ag2S粉体的扫描电镜图片，从图中可以看出，在相同的实验条件下，随着SiO2胶体溶液含量的增加，SiO2纳米微球的数量也逐渐增多，并且大量纳米SiO2微球嵌入链状Ag2S纳米晶的内部(见图2c)，而SiO2胶体溶液含量较低时，纳米SiO2微球主要是附着在链状Ag2S纳米颗粒的表面(见图2a和2b)。并且通过能谱分析可知SiO2/Ag2S复合粉体的主要元素为Si、O、S、Ag，其中Si元素的含量最高(见图2d)。由上述分析与测试表明，SiO2胶体溶液的含量能在一定程度上影响SiO2/Ag2S 复合粉体的形态。
批量吸附实验
在等温吸附动力学实验中，在25℃下，将实施例1-3制备的三种不同比例的SiO2/Ag2S 粉体都取0.1g加入到初始浓度为10mg/L、50mL的亚甲基蓝溶液中，形成三组对照实验，经过超声分散之后避光处理1h进行吸附实验，以20min为时间间隔进行离心取样。在等温吸附热力学实验中，首先配制浓度分别为2mg/L、4mg/L、6mg/L、8mg/L(各50mL) 的亚甲基蓝溶液，分别往四组不同浓度的亚甲基蓝溶液中加入0.1g的A、B、C类吸附剂。超声分散避光处理进行吸附实验，等待吸附达到平衡之后取上清液进行离心处理。并依据下列式子进行平衡吸附量的计算：
Figure GDA0003675161370000031
C0(mg/L)代表亚甲基蓝初始浓度，V(L)是吸附液的体积，m(g)是吸附剂的质量。
图3是三种吸附剂的吸附-脱附等温曲线及孔径分布。从图中可以看出H2对应的A类吸附剂的比表面积最小为6m2/g(见图3a)，在20nm处的吸附量最大(见图3b)，随着SiO2胶体溶液含量的增大，对应的吸附剂的比表面积也急剧增大，B类和C类吸附剂的比表面积分别为60m2/g和73m2/g(见图3c和3e)，而孔径越大，相应的吸附量也呈逐渐上升的趋势(见图3d和3f)。由以上分析与测试可知三种吸附剂均属于多级孔结构，其中SiO2微球既存在介孔也有大孔结构，而Ag2S链状颗粒主要以大孔结构存在。
为了探究时间对吸附过程的影响，分别以20min为一个时间间隔进行吸附液的取样，测定不同时间间隔内吸附液的浓度变化。结果如图4a所示，在吸附的起始阶段，B、C两类吸附剂表现出很强的吸附能力，在60min左右吸附容量趋于稳定，而A类吸附剂仍然具有一定的吸附能力。通过动力学模型对数据的拟合分析，得到三种不同比例的吸附剂对亚甲基蓝的吸附动力学曲线符合准一阶动力学方程。
等温吸附研究可以提供一些关于吸附容量和表面性质的信息以及所使用的吸附剂的亲和力，从而更好地理解吸附过程如何进行。为此，在相同条件下，本发明对比研究了不同 SiO2胶体溶液添加量制备的SiO2/Ag2S复合粉体对亚甲基蓝的吸附情况。结果如图5所示，可以发现B类吸附剂能够较大容量去除亚甲基蓝。将Freundlich(qe＝KFCe 1/n模型线性化后分别对三种吸附等温线进行拟合处理，结果分别如图5中b、d、f所示。由此可知，SiO2/Ag2S复合材料吸附亚甲基蓝模型符合Freundlich模型。
需要指出的是，本发明不仅仅限于以上列举的实施例，凡是能从本发明内容直接导出或启示联想得到的相关技术均应属于本发明涵盖保护的范围。

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1.一种SiO2/Ag2S纳米复合粉体在脱除亚甲基蓝中的应用，其特征在于：所述SiO2/Ag2S纳米复合粉体是以链状Ag2S纳米颗粒为基体，大量纳米SiO2微球嵌入链状Ag2S纳米晶的内部形成，所述SiO2/Ag2S纳米复合粉体属于多级孔结构，其中SiO2微球既存在介孔也有大孔结构，而Ag2S链状颗粒主要以大孔结构存在；所述SiO2/Ag2S纳米复合材料吸附亚甲基蓝的吸附动力学曲线符合准一阶动力学方程，脱除亚甲基蓝规律满足Freundlich等温吸附模型。
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