CN111036175B - 一种活性炭-Ag2O-CuO-Bi2O3吸附材料及其制备方法和应用 - Google Patents
一种活性炭-Ag2O-CuO-Bi2O3吸附材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种活性炭‑Ag2O‑CuO‑Bi2O3吸附材料及其制备方法和应用，其中制备方法包括以下步骤：S1、将银盐、铜盐、铋盐和活性炭加入稀硝酸溶液中，使银盐、铜盐、铋盐溶解，得到混合液；S2、将步骤S1所述混合液的pH调至8‑12，得到反应液；S3、将步骤S2所述反应液在搅拌、超声条件下加热反应，得到活性炭‑Ag2O‑CuO‑Bi2O3吸附材料。本发明制备的材料对含重金属废水具有很好的吸附去除效果，在含重金属的工业污水废水环境治理中具有很好的应用前景。
Description
技术领域
本发明涉及吸附材料技术领域，尤其涉及一种活性炭 -Ag2O-CuO-Bi2O3吸附材料及其制备方法和应用。
背景技术
多孔活性炭材料具有独特的骨架结构、较高的表面积、定向的孔道分布，具有较高的化学稳定性，是一种无污染、无害环境的吸附剂材料，在吸附分离、污水处理、气体净化等领域得到广泛应用。但是，单一多孔活性炭材料的吸附和催化性能有限，无法发挥很好的吸附效果，而复合多孔活性炭材料由于其独特的性能，比单一多孔碳材料具有更好的吸附和催化性能，成为当前研究的重点。
随着工业的发展，含重金属废水已经成为困扰人们的一大难题。重金属对人体、动植物具有显著的毒性，不能被微生物降解，易在生物体内富集，是对环境污染最大的污染物之一。以汞为例，长期食入低剂量无机汞，将会引起慢性肾炎，导致尿毒症，汞在环境中还会被细菌转化为有机汞，较为典型的是甲基汞，会损害大脑皮层、小脑和末梢神经，导致神经系统症状。开发高效净化含重金属废水的吸附剂，在含重金属废水的治理方面具有十分重要的意义。
发明内容
基于背景技术存在的技术问题，本发明提出了一种活性炭 -Ag2O-CuO-Bi2O3吸附材料及其制备方法和应用。
本发明提出的一种活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，包括以下步骤：
S1、将银盐、铜盐、铋盐和活性炭加入稀硝酸溶液中，使银盐、铜盐、铋盐溶解，得到混合液；
S2、将步骤S1所述混合液的pH调至8-12，得到反应液；
S3、将步骤S2所述反应液在搅拌、超声条件下加热反应，得到活性炭-Ag2O-CuO-Bi2O3吸附材料。
优选地，所述步骤S3中，反应的具体条件如下：超声频率为 15-30KHz；加热温度为90-140℃；反应时间为20-50min。
优选地，所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，所述活性炭 -Ag2O-CuO-Bi2O3吸附材料中，Ag2O、CuO和Bi2O3的摩尔比为(1-3)： (1-2)：(1-3)；优选地，Ag2O、CuO和Bi2O3的摩尔比为1:2:1。
优选地，所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，活性炭的质量占总质量的60-80％；更优选地，所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，活性炭的质量占总质量的70％。
优选地，所述银盐为硝酸银，所述铜盐为硝酸铜，所述铋盐为硝酸铋。
优选地，所述混合液中，银盐的摩尔浓度为0.10-0.80mol/L，铜盐的摩尔浓度为0.10-0.50mol/L，铋盐的摩尔浓度为0.10-0.80mol/L。
优选地，所述稀硝酸溶液的浓度为0.05-2.0mol/L。
优选地，所述步骤S2中，采用氨水溶液调节pH。
优选地，在所述步骤S3反应后，还包括干燥处理；更优选地，所述干燥处理的具体条件为：在100-140℃条件下干燥4-6h。
一种活性炭-Ag2O-CuO-Bi2O3吸附材料，由所述制备方法制得。
一种所述活性炭-Ag2O-CuO-Bi2O3吸附材料在处理含重金属废水中的应用。
本发明的有益效果如下：
本发明采用超声波搅拌组合法制备活性炭-Ag2O-CuO-Bi2O3吸附材料，利用强超声在液体中产生空化效应，对物质进行超声处理，同时使用恒温热源，磁力搅拌使混合溶液分散均匀，充分利用了两种场的优点，实现了均匀化合成活性炭-Ag2O-CuO-Bi2O3吸附材料，并且，通过对材料中活性炭含量和Ag2O、CuO和Bi2O3的摩尔比的选择，使得到的材料具有片形和棒状、球形状、多面体形状的混合结构，对废水中的重金属离子，尤其是汞离子、镉离子具有很强的吸附去除作用，在含重金属的工业污水废水环境治理中具有很好的应用前景。
附图说明
图1为实施例1中不同样品的XRD测试结果。
图2-图4为实施例1中的样品10的行SEM扫描电镜测试结果。
图5为为日光照条件下,实施例1中不同样品对含汞离子溶液吸附后的残余汞百分比曲线。
图6为日光照条件下,实施例1中不同样品对含汞离子溶液吸附量曲线。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
活性炭-Ag2O-CuO-Bi2O3吸附材料的制备
一种活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，包括以下步骤：
S1、将硝酸银、硝酸铜、硝酸铋和活性炭加入50mL浓度为 0.1mol/L的稀硝酸溶液中，使硝酸银、硝酸铜、硝酸铋溶解，得到混合液；
S2、用氨水溶液将步骤S1所述混合液的pH调至8-12，得到反应液；
S3、将步骤S2所述反应液在搅拌、超声条件下，在100℃加热反应30min，然后在120℃条件下干燥5h，得到活性炭 -Ag2O-CuO-Bi2O3吸附材料，其中超声频率为25KHz。
按上述制备方法制备Ag2O、CuO、Bi2O3的摩尔比不同的活性炭 -Ag2O-CuO-Bi2O3吸附材料，记为样品1-11。样品1-11中，活性炭的质量均占材料总质量的70％。样品1-11中Ag2O、CuO、Bi2O3的摩尔比如下：
样品1：1:1:1；样品2：2:1:3；样品3：3:1:2；样品4：1:1:2；样品5：1:2:2；样品6：1:2:3；样品7：2:1:2；样品8：2:2:1；样品9： 3:2:1；样品10：1:2:1；样品11：2:1:1。
实施例2
活性炭-Ag2O-CuO-Bi2O3吸附材料的表征
用SmartLab 9KM X射线衍射仪对实施例1制得的样品1-11进行 XRD测试，结果如图1所示(图1中从下到上依次为样品1-11)。
通过对样品1-11进行XRD分析可知，样品1-11的衍射强峰均能与C-Ag2O-CuO-Bi2O3物相基本相对应，且样品1-11的衍射峰强度有明显的差异。样品1-11的XRD衍射图均存在明显的Bi2O3，CuO， Ag2O的衍射峰，而且都比较尖锐，说明合成的复合吸附剂在物相上与实验设计目标物多孔活性炭-Ag2O-CuO-Bi2O3相吻合。
用SU8020冷场扫描电镜对实施例1中的样品10进行SEM扫描电镜测试，结果如图2-图4所示。
从图2-图4中可以看出，本发明在25KHz、100℃，30min的超声搅拌组合法条件下得到了具有片形和棒状、球形状、多面体形状的混合结构的Ag2O-CuO-Bi2O3改性多孔活性炭吸附复合材料，复合材料的孔道结构明显，其微结构尺寸范围为2-5μm。
实施例3
活性炭-Ag2O-CuO-Bi2O3吸附材料的吸附性能测试
在日光照条件下,分别将40mg样品1-11加入100mL含汞离子溶液(溶液中汞离子初始浓度C0为100mg/L)中进行吸附，吸附时间为60min，吸附结束后测定溶液中的汞离子终浓度Ct，计算残余汞百分比，计算公式为：残余汞百分比＝Ct/C0×100％，结果如图5所示。
如图5所示，本发明的活性炭-Ag2O-CuO-Bi2O3吸附材料对含汞离子废水有很好的吸附处理效果，其中样品10(样品中Ag2O、CuO、 Bi2O3的摩尔比为1:2:1)的吸附效果最好，去除率达到99.7％，且不同样品随着时间的延长，吸附去除效果越好。
在日光照条件下,分别将40mg样品1-11加入500mL含汞离子溶液(溶液中汞离子初始浓度为100mg/L)中进行吸附，吸附时间为 60min，吸附结束后测定溶液中的汞离子终浓度，计算吸附量，结果如图6所示。
如图6所示，样品10(样品中Ag2O、CuO、Bi2O3的摩尔比为1:2:1)的吸附效果最好，吸附量达到197mg/g，且不同样品随时间的延长，吸附去除效果越好,在吸附时间达到40min后，随着时间的增加，吸附量基本上达到稳定，说明吸附过程主要在40min内完成，而且吸附效果很好。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，包括以下步骤：
S1、将银盐、铜盐、铋盐和活性炭加入稀硝酸溶液中，使银盐、铜盐、铋盐溶解，得到混合液；
S2、将步骤S1所述混合液的pH调至8-12，得到反应液；
S3、将步骤S2所述反应液在搅拌、超声条件下加热反应，得到活性炭-Ag2O-CuO-Bi2O3吸附材料；
其中，所述步骤S3中，反应的具体条件如下：超声频率为15-30kHz ；加热温度为90-140℃；反应时间为20-50min；所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，Ag2O、CuO和Bi2O3的摩尔比为(1-3)：(1-2)：(1-3)。
2.根据权利要求1所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，Ag2O、CuO和Bi2O3的摩尔比为1:2:1。
3.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述活性炭-Ag2O-CuO-Bi2O3吸附材料中，活性炭的质量占总质量的60-80％。
4.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，活性炭的质量占总质量的70％。
5.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述银盐为硝酸银，所述铜盐为硝酸铜，所述铋盐为硝酸铋。
6.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述混合液中，银盐的摩尔浓度为0.10-0.80mol/L，铜盐的摩尔浓度为0.10-0.50mol/L，铋盐的摩尔浓度为0.10-0.80mol/L。
7.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述稀硝酸溶液的浓度为0.05-2.0mol/L。
8.根据权利要求1或2所述的活性炭-Ag2O-CuO-Bi2O3吸附材料的制备方法，其特征在于，所述步骤S2中，采用氨水溶液调节pH。
9.一种活性炭-Ag2O-CuO-Bi2O3吸附材料，其特征在于，由权利要求1-8任一项所述制备方法制得。
10.一种权利要求9所述活性炭-Ag2O-CuO-Bi2O3吸附材料在处理含重金属废水中的应用。
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