CN113385169A - 一种高效降解有机污染物的新型压电光催化剂、制备方法及应用 - Google Patents
一种高效降解有机污染物的新型压电光催化剂、制备方法及应用 Download PDFInfo
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Abstract
本发明提供了一种高效降解有机污染物的新型压电光催化剂、制备方法及应用,属于液相污染物净化处理、新型材料制备技术领域。在不锈钢网上用硅溶胶固定涂覆纳米催化剂BaTiO3/Bi2WO6,作为导电阳极,阴极是碳棒,两极经鳄鱼夹及导线和外电阻构成闭合电路回路,可见光源由灯提供,构成的系统可实现对典型有机污染物罗丹明B的高效去除。
Description
技术领域
本发明属于液相污染物净化处理、新型材料制备技术领域。涉及BaTiO3/Bi2WO6新型纳米压电光催化剂,并用新型催化剂实现了有机污染物的高效降解,且效果稳定,为进一步开发其他压电光催化剂提供了参考,为有机染料废水的净化处理提供科学基础。
背景技术
罗丹明B(Rhodamine B)是一种典型的有机染料,又称若丹明B、玫瑰红B、玫瑰精B、碱性玫瑰精,分子式为C28H31ClN2O3,是一种具有鲜桃红色的人工合成的染料。我国是染料制造和消费的主力军,印染废水的排放量也很大,经统计,由于染色过程效率低下,每年的年染料产量有超过3%(高达20万吨)通过染色和处理操作释放到自然环境中。首先,染料废水会降低水体透明度、消耗大量的氧气、影响水体自净能力、并影响生物生长,对水体造成不同程度的污染。其次,很多染料还具有致癌和致畸性,威胁饮用水源,对人体危害很大。
目前,去除水中有机污染物的各种技术包括吸附法、生物法、光催化氧化法和膜分离等。但是这些技术都有一定局限性,例如吸附法和膜分离法成本高、难再生、某些有机染料在再生之前易产生二次污染,生物降解法和光催化处理效率低、过程缓慢等。
压电光催化技术继承了光催化材料的化学反应优势,结合了压电材料的压电效应,成为当前水污染治理领域的研究热点之一。压电光催化材料通过改变机械能或超声波能量触发压电效应而产生交变电场,促进光催化材料的光生载流子的分离,抑制电子和空穴的复合,从而提高复合材料的光催化效率。钙钛矿是一种典型的具有钙钛矿结构的压电催化材料,广泛用于压电催化剂的研制。钙钛矿结构的BaTiO3具有良好的压电系数(D33)~200pc/n和较高的结构稳定性,是目前研究最多的材料,具有广阔的应用前景。但是目前将BaTiO3/Bi2WO6压电光催化材料应用于去除有机染料废水的报道还未出现。
本申请以BaTiO3/Bi2WO6为压电光催化剂,选择典型的有机污染物罗丹明B作为目标污染物,以此催化剂快速降解去除罗丹明B。
发明内容
本发明制备了一种去除有机污染物效率高、制备过程简单、稳定性高的新型半导体催化材料。BaTiO3/Bi2WO6对罗丹明B处理净化效率高、能耗低。
本发明的技术方案:
一种高效降解有机污染物的新型压电光催化剂的制备方法,步骤如下:
(1)将Ba(OH)2、钛酸四丁酯溶于去离子水中,其中Ba(OH)2与钛酸四丁酯的摩尔比为1:1,然后用NaOH溶液将pH调节为13,接着搅拌均匀后将溶液转入聚四氟乙烯内衬高压釜中,反应结束后,用乙醇和去离子水洗涤多次后烘干得到纯BaTiO3粉末。
(2)五水合硝酸铋溶于乙二醇后再加入二水钨酸钠,完全溶解得到混合溶液,将已溶于乙醇并超声至分散均匀的BaTiO3溶液加入到上述混合溶液中并继续搅拌,五水合硝酸铋、二水钨酸钠、BaTiO3摩尔比是2:1:0.25~1,接着将溶液转入聚四氟乙烯内衬高压釜中进行水热反应。反应后产物用乙醇和去离子水洗涤,干燥得到最终的催化剂BaTiO3/Bi2WO6。
进一步地,所述步骤(1)中,聚四氟乙烯内衬高压釜反应温度为180~200℃,反应时间为20~24h;烘干温度为60℃-80℃,烘干时间为10~12h。
进一步地,所述步骤(2)中,水热反应温度为100℃~160℃,水热反应时间为8~10h。
进一步地,所述步骤(2)中,干燥温度为60℃-80℃,干燥时间为10~12h。
一种高效降解有机污染物的新型压电光催化剂的应用,上述的制备方法制得的BaTiO3/Bi2WO6应用在压电催化耦合光电催化系统。
压电催化耦合光电催化系统的构建:用硅溶胶将BaTiO3/Bi2WO6固定在不锈钢网表面作为系统阳极,阴极使用碳棒,系统内部为污染物和电解质,外电路由导线和外电阻连接阴阳两极构成闭合回路。
压电催化耦合光电催化系统的所需的机械能由曝气提供。机械能可由但不仅限于由曝气提供,在以上所述的压电催化耦合光电催化系统基础上进行的任何形式的变动或衍生都应属于本专利的保护范围内。
本发明的有益效果:该反应系统集成了电催化、光催化以及压电催化,降解去除罗丹明B:新型纳米压电光催化剂可以对罗丹明B进行快速吸附和催化降解,该系统在催化体系中,净化效果显著,而且稳定性好,为今后催化降解有机染料提供了科学依据。
附图说明:
图1是光电催化体系(PFC)、压电耦合电催化体系(PZ-FC)、压电耦合光电催化体系(PZ-PFC)三种不同体系下罗丹明B的去除率对比图。图中,横坐标表示时间(min),纵坐标表示降解率(Ct/C0)。
图2是不同外电阻下体系降解罗丹明B效果对比图。图中,横坐标表示时间(min),纵坐标表示降解率(Ct/C0)。
图3(1)是不同比例掺杂得到的降解效果动力学拟合图。
图3(2)是不同比例掺杂得到的速率常数K值图。
图4是多次重复利用去除效果图。图中,横坐标表示时间(min),纵坐标表示降解率(Ct/C0)。
具体实施方式
以下结合技术方案和附图,进一步说明本发明的具体实施方式:
实施例1
首先将0.15773gBa(OH)2、0.17016g钛酸四丁酯溶于25ml去离子水中,然后用1MNaOH将溶液pH调节为13,接着搅拌30min后将溶液转入聚四氟乙烯内衬高压釜中,200℃反应24h后,用乙醇和去离子水洗涤多次后60℃烘干12h得到纯BaTiO3粉末,将0.46638gBaTiO3粉末溶于40ml乙醇中超声6h。1.8721g五水合硝酸铋溶于40ml乙二醇后再加入0.63643g二水钨酸钠,完全溶解得到混合溶液,将超声6h的溶液加入到上述混合溶液中并继续搅拌,接着将溶液转入聚四氟乙烯内衬高压釜中,在160℃下水热反应10h。反应后产物用乙醇和去离子水洗涤3次,60℃干燥12h得到最终的催化剂BaTiO3/Bi2WO6。
实施例2
将BaTiO3/Bi2WO6用硅溶胶涂覆到不锈钢网作为系统的阳极,阴极使用碳棒,阴阳两极放在同一反应容器中,反应容器内装有混合了一定量电解质的罗丹明B溶液,浓度为20mg/L。外电路由鳄鱼夹、导线和电阻形成闭合的回路,光源是由20~50W的普通灯泡提供。
实施例3:不同体系下去除罗丹明B
将阴阳电极和混有电解质的罗丹明B污染物溶液加入到反应器中,先暗反应30min,之后根据各个体系的特点设置相应的反应条件,每隔10min取样一次进行测量。反应时长60min。
光电催化体系:加光照,外电路用导线和外电阻连通,不曝气;压电耦合电催化体系:加曝气,外电路用导线和外电阻连通,不加光照;压电耦合光电催化体系:加光照,加曝气,外电路用导线和外电阻连通。
图1中,PZ-PFC效果最好,50min就可达到98.68%,远比PFC和P-EC的处理效果好。证明了压电催化和光电催化具有良好的耦合作用。
实施例4:不同外电阻下体系降解罗丹明B
实验同实施例3,将外电阻分别设为10Ω、100Ω和1000Ω。图2结果显示当外电阻为100Ω时的罗丹明B去除率最高,50min达到98.68%。
实施例5:不同掺杂比例对降解的影响
实验同实施例3,通过调节BaTiO3与Bi2WO6之间的掺杂摩尔比探究其对降解效果的影响。图中H0、H5、H11、H12、H14、H21、H41分别代表:纯BaTiO3、纯Bi2WO6、BaTiO3/Bi2WO6(1:1)、BaTiO3/Bi2WO6(1:2)、BaTiO3/Bi2WO6(1:4)、BaTiO3/Bi2WO6(2:1)、BaTiO3/Bi2WO6(4:1)。从图3(1)和图3(2)中可以看到当掺杂摩尔比为1:1时速率常数最大,且分别是纯BaTiO3和纯Bi2WO6的7.13和5.26倍。
实施例6:压电光催化剂的稳定性探究
实验同实施例3。每次实验结束后将催化阳极在60℃下烘干2h后用于下一次实验。图3显示4次重复利用后该催化剂活性基本不变,第5次活性稍有下降,表明该催化剂具有良好的稳定性。
Claims (9)
1.一种高效降解有机污染物的新型压电光催化剂的制备方法,其特征在于,步骤如下:
(1)将Ba(OH)2、钛酸四丁酯溶于去离子水中,其中Ba(OH)2与钛酸四丁酯的摩尔比为1:1,然后用NaOH溶液将pH调节为13,接着搅拌均匀后将溶液转入聚四氟乙烯内衬高压釜中,反应结束后,用乙醇和去离子水洗涤多次后烘干得到纯BaTiO3粉末;
(2)五水合硝酸铋溶于乙二醇后再加入二水钨酸钠,完全溶解得到混合溶液,将已溶于乙醇并超声至分散均匀的BaTiO3溶液加入到上述混合溶液中并继续搅拌,五水合硝酸铋、二水钨酸钠、BaTiO3摩尔比是2:1:0.25~1,接着将溶液转入聚四氟乙烯内衬高压釜中进行水热反应;反应后产物用乙醇和去离子水洗涤,干燥得到最终的催化剂BaTiO3/Bi2WO6。
2.根据权利要求1所述的一种高效降解有机污染物的新型压电光催化剂的制备方法,其特征在于,所述步骤(1)中,聚四氟乙烯内衬高压釜反应温度为180~200℃,反应时间为20~24h;所述步骤(1)中,烘干温度为60℃-80℃,烘干时间为10~12h。
3.根据权利要求1或2所述的一种高效降解有机污染物的新型压电光催化剂的制备方法,其特征在于,所述步骤(2)中,水热反应温度为100℃~160℃,水热反应时间为8~10h。
4.根据权利要求1或2所述的一种高效降解有机污染物的新型压电光催化剂的制备方法,其特征在于,所述步骤(2)中,干燥温度为60℃-80℃,干燥时间为10~12h。
5.根据权利要求3所述的一种高效降解有机污染物的新型压电光催化剂的制备方法,其特征在于,所述步骤(2)中,干燥温度为60℃-80℃,干燥时间为10~12h。
6.一种高效降解有机污染物的新型压电光催化剂,其特征在于,所述的新型压电光催化剂是由权利要求1-8任一所述的制备方法制得的。
7.一种高效降解有机污染物的新型压电光催化剂的应用,其特征在于,权利要求1-8任一所述的制备方法制得的BaTiO3/Bi2WO6应用在压电催化耦合光电催化系统。
8.根据权利要求7所述的应用,其特征在于,压电催化耦合光电催化系统的构建:用硅溶胶将BaTiO3/Bi2WO6固定在不锈钢网表面作为系统阳极,阴极使用碳棒,系统内部为污染物和电解质,外电路由导线和外电阻连接阴阳两极构成闭合回路。
9.根据权利要求7或8所述的应用,其特征在于,压电催化耦合光电催化系统的所需的机械能由曝气提供。
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