CN106475038A - 激光诱导单分散Ag‑Ag2S纳米粒子光催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种激光诱导单分散Ag‑Ag2S纳米粒子光催化剂的制备方法，包括如下步骤：(1)在旋转容器中加入含有硫代乙酰胺和十六烷基三甲基溴化铵的水溶液为反应液；(2)Ag片抛光后浸没于反应液中，旋转；(3)通过石英透镜将激光束聚焦在位于旋转容器中Ag片上；(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，离心，沉积产物烘干，即得。本发明的方法简单，本发明制备的Ag‑Ag2S纳米粒子光催化剂表现出去除废水中甲基蓝(MB)的优越性能，可见光下，5min之内MB的去除率可达99.83％；吸附降解有机物后实现了纳米材料不需借助外力的沉降分离。
Description
技术领域
本发明属于水体净化领域，涉及一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂及制备方法。
背景技术
地下水中的一些有机污染物具有很高的毒性甚至会对水生生物和包括人类和其他陆生生物产生致死作用。越来越多的证据表明，电镀、纺织工业、化妆品、药品等行业向水体中排放的有机污染物是人肾脏、肝脏及膀胱癌等发病率升高的主要原因。甲基蓝(MB)和甲基橙(MO)是比较常见的有机污染物，具有复杂的芳香族分子结构，通常对光、热或氧化剂具有稳定性，非常难从废水中分离、降解。常规的去除废水中染料有机物的处理技术包括化学沉淀、生物氧化、臭氧氧化及光催化。因为常规技术都具有程序复杂且去除效率低的缺陷，所以现今大多数研究者都致力于开发环保吸附剂以求通过简单的吸附作用去除水体中的有机污染物。例如，Das等人合成负载羟基(-OH)的氧化铁纳米颗粒获得较高的吸附性能。最近的研究中，一些新兴的纳米材料表现出良好的吸附性能，如已有研究表明过渡金属氧化物(Fe、Co和Ni)纳米颗粒可以有效的从废水中去除MB。但是，水处理后的净化程序仍旧是一个亟待解决的问题，这些吸附材料或者催化还原剂只能通过离心或外部磁场协助才能够除去，这成为了应用于实际污水处理厂的一大限制。
在溶液中进行的激光诱导合成技术由于高温、高压及非平衡的处理条件，而成为一种新兴的用于合成金属稳定材料的绿色合成法。电子重建α-Ag2WO4纳米棒、碳纳米管及微米管bbc结构的制造、硅纳米球低聚物的MIT效应、新相纳米晶体的形成、Ag/AgCl异质结构立方体的制备等均为液体激光制造领域获得的最新研究进展。
但目前尚未有用激光诱导单分散Ag-Ag2S纳米粒子光催化剂的报道。
发明内容
本发明的目的是克服现有技术的不足，提供一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法。
本发明的技术方案概述如下：
一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法，包括如下步骤：
(1)在旋转容器中加入反应液，所述反应液为含有硫代乙酰胺和十六烷基三甲基溴化铵的水溶液，所述硫代乙酰胺的浓度为0.2M，十六烷基三甲基溴化铵的浓度为0.05M；
(2)Ag片抛光后浸没于反应液中，在300-400rpm条件下，旋转20-40min；
(3)在发射激光波长1064nm，脉冲持续时间10ns，频率为10Hz的条件下，通过具有65mm焦距的石英透镜将激光束聚焦在位于旋转容器中Ag片上30min，使Ag片表面的激光束平均直径为370μm，激光功率密度为6～9GW/cm2；
(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，将冲洗液在10000rpm离心5-15min，沉积产物，在烘箱中在室温干燥，得到激光诱导单分散Ag-Ag2S纳米粒子光催化剂。
本发明的优点：
1.本发明的方法简单，本发明制备的Ag-Ag2S纳米粒子光催化剂表现出去除废水中甲基蓝(MB)和甲基橙(MO)的优越性能，将9mgAg-Ag2S纳米粒子光催化剂加入30mL甲基蓝(MB)浓度为10mg/L的废水中，可见光下，5min之内MB的去除率可达99.83％；
2.相比较传统的纳米材料催化剂，本发明的方法制备的Ag-Ag2S纳米粒子光催化剂，由于SO3Na官能团的存在，在吸附降解污染物后可以自行聚集沉降于反应容器底部，通过过滤即可除去，去除率99.999％(图2)，对于其在实际中的应用具有重大意义。
3.本发明的方法制备的Ag-Ag2S纳米颗粒表现出卓越的吸附性能，且在吸附降解有机物后突破性地实现了纳米材料不需借助外力的沉降分离。
附图说明
图1为激光诱导单分散Ag-Ag2S纳米粒子光催化剂在可见光下对水溶液中MB的降解。
图2 MB降解过程颜色变化。
图3 MB的降解浓度与Ag-Ag2S中Ag、Ag2S质量比的响应曲线。
图4 Ag-Ag2S混合纳米颗粒吸附MB分子的示意图。
具体实施方式
本发明激光所采用的激光器为Q-switched Nd:YAG(Yttrium Aluminum Garnet)laser(Quanta Ray,Spectra Physics)，这种激光器的公开是为了使本领域技术人员能够更好地理解本发明，但并不对本发明作任何限制。
本发明各实施例中所示的TAA为硫代乙酰胺的简写；CTAB为十六烷基三甲基溴化铵的简写，MB为甲基蓝的简写。
实施例1
一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法，包括如下步骤：
(1)在旋转容器中加入反应液，所述反应液为含有TAA和CTAB的水溶液，所述TAA的浓度为0.2M，CTAB的浓度为0.05M；
(2)Ag片抛光后浸没于反应液中，在350rpm条件下，旋转30min；
(3)在发射激光波长1064nm，脉冲持续时间10ns，频率为10Hz的条件下，通过具有65mm焦距的石英透镜将激光束聚焦在位于旋转容器中Ag片上30min，使Ag片表面的激光束平均直径为370μm，激光功率密度为6～9GW/cm2；
(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，将冲洗液在10000rpm离心10min，沉积产物，在烘箱中在室温干燥，得到激光诱导单分散Ag-Ag2S纳米粒子光催化剂。
实施例2
一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法，包括如下步骤：
(1)在旋转容器中加入反应液，所述反应液为含有TAA和CTAB的水溶液，所述TAA的浓度为0.2M，CTAB的浓度为0.05M；
(2)Ag片抛光后浸没于反应液中，在300rpm条件下，旋转40min；
(3)在发射激光波长1064nm，脉冲持续时间10ns，频率为10Hz的条件下，通过具有65mm焦距的石英透镜将激光束聚焦在位于旋转容器中Ag片上30min，使Ag片表面的激光束平均直径为370μm，激光功率密度为6～9GW/cm2；
(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，将冲洗液在10000rpm离心5min，沉积产物，在烘箱中在室温干燥，得到激光诱导单分散Ag-Ag2S纳米粒子光催化剂。
实施例3
一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法，包括如下步骤：
(1)在旋转容器中加入反应液，所述反应液为含有TAA和CTAB的水溶液，所述TAA的浓度为0.2M，CTAB的浓度为0.05M；
(2)Ag片抛光后浸没于反应液中，在400rpm条件下，旋转20min；
(3)在发射激光波长1064nm，脉冲持续时间10ns，频率为10Hz的条件下，通过具有65mm焦距的石英透镜将激光束聚焦在位于旋转容器中Ag片上30min，使Ag片表面的激光束平均直径为370μm，激光功率密度为6～9GW/cm2；
(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，将冲洗液在10000rpm离心15min，沉积产物，在烘箱中在室温干燥，得到激光诱导单分散Ag-Ag2S纳米粒子光催化剂。
实施例4
实施例1制备的激光诱导单分散Ag-Ag2S纳米粒子光催化剂用于MB光催化降解，具体步骤如下：
(1)配置浓度为10mg/L的MB溶液，取样3mL标记为M0
(2)精确称取9mg激光诱导单分散Ag-Ag2S纳米粒子光催化剂置于烧杯中，加入30mL浓度为10mg/L的MB水溶液，黑暗中搅拌60min，将样品溶液分成两份，一份3mL，在6000rpm离心后，取上清标记为M60；
(3)在步骤(2)剩余的另一份样品溶液放置在300W汞灯下，汞灯垂直于杯底，距液面8.5cm照射，5min后取样3mL，在6000rpm离心后，取上清液标记为M5；
(4)停止照射，烧杯内剩余的液体(悬浮液)发生自然沉降，以0.22μm滤膜过滤，取滤液3mL，标记为M6，M0与M6的对比如图2，(图2MB降解过程颜色变化(左图为降解前的M0，右图为降解、过滤后的M6)
(5)用紫外-可见分光光度计分别检测M0、M60、M5于190～1100nm处吸收光谱，如图1所示,从图1中可以看出：激光诱导单分散Ag-Ag2S纳米粒子光催化剂在可见光下对水溶液中MB的降解率可在5min内达到99.83％，664nm处的吸光度由初始的2.474Abs降至5min时的0.004Abs。
实施例5不同Ag、Ag2S比率的激光诱导单分散Ag-Ag2S纳米粒子光催化剂对MB吸附容量曲线
按照实施例1的激光诱导单分散Ag-Ag2S纳米粒子光催化剂制备方法，仅将步骤(3)的激光束聚焦在位于旋转容器中Ag片上的时间分别用10min、15min、20min、30min、40min、50min，得到6种激光诱导单分散Ag-Ag2S纳米粒子光催化剂。分别对应0.4、0.6、0.8、1.0、1.2、1.4的Ag/Ag2S质量比，按照下述步骤测试其各自对于MB的处理能力：
(1)配制浓度为10mg/L的MB水溶液，取样3mL标记为M0
(2)精确称取9mg激光诱导单分散Ag-Ag2S纳米粒子光催化剂置于烧杯中，加入30mL浓度为10mg/L的MB水溶液，黑暗中搅拌60min；
(3)将上述溶液置于300W汞灯下，汞灯垂直于杯底，距液面8.5cm照射，5min后取样3mL，6000rpm离心后分别标记为M5；
M0、M5分别对比MB标准曲线，得到C0、C5(mg/L)，以C5-C0的差值为纵坐标，以所用的催化剂中Ag与Ag2S的质量比为横坐标作图(图3)。可以看出Ag与Ag2S的质量比小于1.0时，制得的纳米颗粒对于MB处理能力随着质量比升高而升高；Ag与Ag2S的质量比大于1.0时，制得的纳米颗粒对于MB处理能力随着质量比升高而降低；Ag与Ag2S的质量比为1.0时，达到最大处理能力，即前例所用的纳米颗粒，降解率可达99.83％。
实施例6
激光诱导单分散Ag-Ag2S纳米粒子光催化剂对水体中有机染料分子的吸附机理
通过上面的讨论我们可以分析得出激光诱导单分散Ag-Ag2S纳米粒子光催化剂吸附水体中有机染料分子的机理。即激光诱导单分散Ag-Ag2S纳米粒子光催化剂的正活性位点与MB分子的负电荷之间强大的电子-静电作用使得MB分子吸附于纳米颗粒表面，之后维持凝聚体的能力来自于带正电荷的Ag-Ag2S与MB带负电荷的-SO3 -官能团之间形成的离子键。因此，染料分子是否携带-SO3 -官能团将影响光催化降解效率。另外，由实施例5可知，Ag2S表面Ag的沉积量直接影响正活性位点的数量，因此Ag沉积过多或者过少均不利于纳米粒子对染料分子的降解能力。
图4为激光诱导单分散Ag-Ag2S纳米粒子光催化剂对水体中有机染料分子MB的吸附机理示意图。
Claims (1)
1.一种激光诱导单分散Ag-Ag2S纳米粒子光催化剂的制备方法，其特征是包括如下步骤：
(1)在旋转容器中加入反应液，所述反应液为含有硫代乙酰胺和十六烷基三甲基溴化铵的水溶液，所述硫代乙酰胺的浓度为0.2M，十六烷基三甲基溴化铵的浓度为0.05M；
(2)Ag片抛光后浸没于反应液中，在300-400rpm条件下，旋转20-40min；
(3)在发射激光波长1064nm，脉冲持续时间10ns，频率为10Hz的条件下，通过具有65mm焦距的石英透镜将激光束聚焦在位于旋转容器中Ag片上30min，使Ag片表面的激光束平均直径为370μm，激光功率密度为6～9GW/cm2；
(4)从旋转容器中取出激光照射后的Ag片，用蒸馏水冲洗激光照射后的Ag片表面收集的产物，将冲洗液在10000rpm离心5-15min，沉积产物，在烘箱中在室温干燥，得到激光诱导单分散Ag-Ag2S纳米粒子光催化剂。
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