CN111644171B - 一种NaZnMo复合物催化剂材料的制备方法及其用途 - Google Patents
一种NaZnMo复合物催化剂材料的制备方法及其用途 Download PDFInfo
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Abstract
本发明公开了一种NaZnMo复合物催化剂材料的制备方法及其用途,本发明以醋酸锌和钼酸钠为原料,通过超声、调控pH值、溶液反应制备NaZnMo复合物,其作为超声催化剂催化降解有机染料效率高,结构稳定,应用前景广泛。本发明制备工艺简单,反应条件温和、成本低廉,设备投资少,适合批量生产。
Description
技术领域
本发明属于无机催化领域,具体涉及一种NaZnMo复合物催化剂材料的制备方法及其用途。
背景技术
近来,由于技术进步和工业发展引起的环境污染物已成为全球性问题。而氧化处理被认为是最有效的方法,其中光催化过程被认为是分解有机污染物的可持续的途径。然而,废水通常是半透明的,并且包含各种相对较高浓度的有机物,极大地阻碍了入射阳光的渗透和太阳能在催化剂颗粒表面的传输,从而极大地限制了光催化的去除效率。相反,超声催化能够克服上述缺点,并在废水处理和净化领域中具有潜在的应用价值。
纳米材料具有独特性能,其现有合成方法有多种,如高温固相法,溶胶-凝胶法,声化学法,水热法,共沉淀法等,但超声化学法(声化学法)因其具有高均匀性,良好的结晶性,简便性和可控参数等多种优势而被认为是最重要的方法之一,其可成功合成出不同的化合物。而且使用声化学法,它的高效合成技术可节省时间和能源,促进各种化学反应,有利于节能环保,且无需加热即可合成。在众多研究中,钼酸盐是一种性能良好的催化剂材料,应用广泛,如光催化剂、传感器、光子和激光设备构建材料等。NaZn2(OH)(MoO4)2·H2O这种钼酸盐研究的比较少。
发明内容
本发明所要解决的技术问题是针对现有技术,提供制备工艺简单、反应条件温和、无需添加表面活性剂、产率高的一种NaZnMo复合物催化剂材料的制备方法。
本发明为解决上述技术问题所采取的技术方案为:一种NaZnMo复合物催化剂材料的制备方法,该制备方法以醋酸锌和钼酸钠为原料,通过超声技术和调控酸碱度,在常温常压下,进行溶液反应,得到一种NaZnMo复合物催化剂材料,具体包括以下步骤:
(1)称取适量的醋酸锌Zn(Ac)2·2H2O加入到一定体积的蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A,其浓度为0.2mmol/mL;
(2)称取适量的钼酸钠Na2MoO4·2H2O加入到一定体积的蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B,其浓度为0.2mmol/mL;
(3)在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声,得到含有白色沉淀的浑浊液D;
(4)将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料;
所述步骤(1)、(2)和(3)中超声仪的超声功率为200W;
所述一种NaZnMo复合物的化学式为NaZn2(OH)(MoO4)2·H2O;
所述一种NaZnMo复合物的形貌为片状梭形。
进一步的,本发明还提供了所述NaZnMo复合物的用途,该复合物作为催化剂,在超声条件下能够高效快速催化降解亚甲基蓝及罗丹明B。
本文通过简单的声化学法,制备了一种NaZnMo复合物,其作为催化剂在超声条件下对亚甲基蓝及罗丹明B等有机染料具有很好的超声催化降解性能。
与现有技术相比,本发明具有如下特点:
(1)本发明所制备的NaZnMo复合物的形貌为片状梭形;
(2)本发明所制备NaZnMo复合物作为催化剂,能够在常温常压超声条件下,高效快速催化降解亚甲基蓝及罗丹明B有机染料。
附图说明
图1是不同时间所制备NaZnMo复合物催化剂的XRD图。
图2是反应时间40min所制备NaZnMo复合物催化剂的SEM图。
图3是不同时间所制备NaZnMo复合物催化剂在超声条件下催化降解亚甲基蓝浓度随着超声时间变化的关系图。
图4是不同时间所制备NaZnMo复合物催化剂在超声条件下催化降解罗丹明B浓度随着超声时间变化的关系图。
具体实施方式
以下结合实施例对本发明作进一步详细描述,本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合。
实施例1
称取2.0mmol(0.438g)的醋酸锌Zn(Ac)2·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A;称取2.0mmol(0.484g)的钼酸钠Na2MoO4·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B;在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声5分钟,得到含有白色沉淀的浑浊液D;将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料,其化学式为NaZn2(OH)(MoO4)2·H2O,并记为T5,并扫描电镜SEM观测其形貌。
实施例2
称取2.0mmol(0.438g)的醋酸锌Zn(Ac)2·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A;称取2.0mmol(0.484g)的钼酸钠Na2MoO4·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B;在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声10分钟,得到含有白色沉淀的浑浊液D;将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料,其化学式为NaZn2(OH)(MoO4)2·H2O,记为T10,并扫SEM观测其形貌。
实施例3
称取2.0mmol(0.438g)的醋酸锌Zn(Ac)2·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A;称取2.0mmol(0.484g)的钼酸钠Na2MoO4·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B;在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声15分钟,得到含有白色沉淀的浑浊液D;将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料,其化学式为NaZn2(OH)(MoO4)2·H2O,记为T15,并扫SEM观测其形貌。
实施例4
称取2.0mmol(0.438g)的醋酸锌Zn(Ac)2·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A;称取2.0mmol(0.484g)的钼酸钠Na2MoO4·2H2O加入到10mL蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B;在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声40分钟,得到含有白色沉淀的浑浊液D;将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料,其化学式为NaZn2(OH)(MoO4)2·H2O,记为T40,并扫SEM观测其形貌。
将上述实施例中所得到的T5、T10、T15和T40分别进行粉末X射线衍射分析,结果显示所获得的化合物为NaZn2(OH)(MoO4)2·H2O(图1)。
将上述实施例4所获得NaZnMo复合物催化剂材料用扫描电镜观测其形貌,结果显示材料的形貌为片状梭形(图2)。
将上述实施案例1-4中所制得的NaZnMo复合物作为催化剂,分别进行超声催化降解亚甲基蓝,结果表明所制备的复合物催化剂材料具有良好催化降解性能(图3),其中所用溶剂为水,催化剂用量为1.0g/L,亚甲基蓝染料溶液pH为7,亚甲基蓝染料溶液浓度10mg/L,超声功率为200W。从图3可以看到,所有样品对亚甲基蓝都有较好的催化降解效果,催化剂在前40分钟内降解速率很快,其中T40的降解率达63%,之后降解速率变慢。在120分钟后T5、T10、T15、T40催化降解率分别为82%,82%,86%,88%。表明超声时间越长,其催化降解效果越好。
将上述实施案例1-4中所制得的NaZnMo复合物作为催化剂,分别进行超声催化降解罗丹明B,结果表明所制备的复合物催化剂材料具有良好降解性能(图4),其中所用溶剂为水,催化剂用量为1.0g/L,罗丹明B染料溶液pH为7,罗丹明B染料溶液浓度10mg/L,超声功率为200W。从图4可以看到,所有样品对罗丹明B都有较好的催化降解效果。从图4可知,在前40分钟内降解速率比较慢,其T40的降解率达38%,之后降解速率变快。在120分钟后T5、T10、T15、T40降解率分别为82%,77%,90%,92%。表明超声时间越长,其催化降解效果越好。
Claims (2)
1.一种NaZnMo复合物催化剂材料的制备方法,其特征在于,所述制备方法包括如下步骤:
1)称取适量的醋酸锌加入到一定体积的蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液A,其浓度为0.2mmol/mL;
2)称取适量的钼酸钠加入到一定体积的蒸馏水中,用超声仪超声5分钟后,形成均匀透明的溶液B,其浓度为0.2mmol/mL;
3)在超声条件下,将溶液A缓慢的滴入到溶液B中,得到混合溶液C,用2M的NaOH调节溶液C的pH至6,再用超声仪超声5-40分钟,得到含有白色沉淀的浑浊液D;
4)将上述浑浊液D进行离心分离,得到白色沉淀物,将白色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到一种NaZnMo复合物催化剂材料;
所述醋酸锌的化学式为Zn(Ac)2·2H2O;所述钼酸钠化学式为Na2MoO4·2H2O;
所述NaZnMo复合物的化学式为NaZn2(OH)(MoO4)2·H2O;
所述步骤1)、2)和3)中用超声仪的超声的功率为200W;
所述NaZnMo复合物的形貌为片状梭形。
2.一种如权利要求1所述制备方法得到的NaZnMo复合物的用途,其特征在于,该复合物作为催化剂,在超声条件下能够高效快速催化降解亚甲基蓝及罗丹明B有机染料。
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