CN111804318A - 一种吸附光催化剂及其制备方法和应用 - Google Patents
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Abstract
本发明公开一种吸附光催化剂及其制备方法和应用,首先分别通过水热法制备磷酸铋和通过水热法制备二硫化钼,再将磷酸铋和二硫化钼研磨混合后进行煅烧后得到吸附光催化剂,将光催化材料用于降解亚甲基蓝模拟染料废水,表现出吸附能力和光催化降解效果。本发明吸附光催化剂制备工艺简单,不需要大型设备,合成条件简易。
Description
技术领域
本发明属于环境功能光催化材料技术领域,更加具体地说,具体涉及一种MoS2/MoO3/BiPO4吸附光催化剂及其制备方法。
背景技术
根据世界卫生组织的统计数据显示,每年至少有500万人因为饮用了不安全的水以及缺乏卫生用水而得病死去;有248万人因为长期吸入微尘颗粒而引发中风、心血管疾病、呼吸道病变或肺癌等疾病。环境污染治理问题已然成为人们亟待解决的难题。自1972年Fujishima等人首次报道光解水制氢以来,光催化技术以其充分利用太阳能、能矿化污水中的大部分有机污染物等优点,为人们处理环境污染物提供了新思路,降解效率高、稳定性好、成本低、无毒的光催化材料成为人们的研究热点。
2010年,潘成思首次报道了磷酸铋(BiPO4)用于光催化降解有机物,并发现其具有优异的紫外光光催化活性,同时磷酸铋(BiPO4)具有廉价、无毒、易制备、易分离等优点,在光催化领域具有潜在的应用价值,但因可见光利用率不够高、量子效率低和光生载流子复合等缺点又限制了其进一步的发展和应用。从实际意义上来讲,对磷酸铋(BiPO4)进行改性以提高效率,对工业应用具有重要意义。
为解决上述问题,一方面,可以通过调控光催化剂本身的微观形貌及结构来提高光催化活性;另一方面,可以通过掺杂或复合扩展光催化剂的光响应范围,并提高量子效率。其中,不同半导体之间的复合,不仅可以扩展光吸收范围,还能通过形成异质结从而提高光生空穴和电子的分离与迁移效率,进而提高光催化活性。然而,二硫化钼作为半导体助催化剂且具有一定的比表面积,目前尚未有文献关于MoS2/MoO3/BiPO4吸附光催化剂的报道。
发明内容
本发明的目的在于克服现有技术的不足,提供一种具有吸附和光催化双重功能的MoS2/MoO3/BiPO4复合催化剂及其制备方法和应用,制备方法工艺简单易行,不需要大型设备,合成条件简易。
本发明技术目的通过下述技术方案予以实现:
一种吸附光催化剂及其制备方法,按照下述步骤进行制备:将磷酸铋和二硫化钼进行研磨并混合均匀,置于空气氛围中自室温以每分钟5—10摄氏度的速度升温至280—300摄氏度并保温1—5小时,自然冷却至室温后研磨得到吸附光催化剂;二硫化钼和磷酸铋的质量比为(0.05—0.3):1。
而且,二硫化钼和磷酸铋的质量比为(0.1—0.2):1。
而且,将磷酸铋和二硫化钼混合均匀后,自室温以每分钟8—10摄氏度的速度升温至290—300摄氏度并保温1—2小时。
对本发明制备的吸附光催化剂进行表征,样品的晶型采用德国布鲁克D8Advance型X射线衍射仪进行测试。采用CuKa射线(λ=0.154nm)进行分析,电压为40kv,电流为40mA。扫描步长为0.01°。XRD用于探测制备的BiPO4/MoO3/MoS2异质结光催化剂的晶体结构和相信息。图1中,由下至上依次是MoO3(JCPDS 05-0508)和BiPO4(JCPDS No.15-0767)XRD标准图谱。由于MoO3的低结晶度而显示出弱峰强度,然而,MoO3的XRD图仍然有归因于MoO3的(110),(040)和(021)晶面的特征峰。BiPO4在2θ值为27.07°,29.02°,31.15°处出现三强峰,分别指向(200),(120),(012)晶面,说明BiPO4的有效合成且具有高结晶度。由于MoS2掺杂量较低,且在煅烧过程中氧化生产了MoO3,所以在XRD衍射图中为发现明显的MoS2衍射峰,但是鉴于催化剂颜色为深灰色,所以存在少量的MoS2掺杂。XRD图像表现出混合相(磷酸铋、二硫化钼和MoO3),说明了异质结的成功制备;从SEM来看,以磷酸铋和二硫化钼为原料制备的催化剂虽然出现些许团聚现象,但整体形貌匀称。
在本发明中,磷酸铋为磷酸铋纳米棒,通过水热法制备磷酸铋纳米棒,具体可以参考文献(磷酸铋纳米棒的可控合成及其光催化性能,刘艳芳,马新国,易欣,朱永法,物理化学学报(Wuli Huaxue Xuebao)Acta Phys.-Chim.Sin.2012,28(3),654-660):将2-4mmol/L五水硝酸铋加入到120mL去离子水中配置五水硝酸铋水溶液,加入10-12mmol磷酸二氢钠,搅拌1h,转入到以聚四氟乙烯为内衬的高压反应釜中,160℃水热18-24小时,待反应釜冷却至室温后,以转速8000-9000r/min离心将产物用去离子水和无水乙醇交替洗涤3-4次,120℃干燥10-13小时。
在本发明中,二硫化钼为二硫化钼纳米微球,通过水热法制备二硫化钼,具体参考文献(水热法合成球花状二硫化钼及其电化学性能,李美娟,沈舒宜,罗国强,张联盟,无机化学学报,2017年9月,第33卷第9期,1521-1526):将0.4-0.5g钼酸铵加入到40ml去离子水中配置成钼酸铵溶液,加入0.5-0.6g硫脲,搅拌溶解后超声处理30min,转入到50ml以聚四氟乙烯为内衬的高压反应釜中,200℃反应18-24小时,待反应釜冷却至室温后,以转速8500-9500r/min离心将产物用去离子水和无水乙醇交替洗涤3-4次,45℃干燥10-13小时。
与现有技术相比,本发明的有益效果如下:(1)本发明中MoS2/MoO3/BiPO4吸附光催化剂制备工艺简单,不需要大型设备,合成条件简易;(2)本发明将光催化材料用于降解亚甲基蓝模拟染料废水,表现出一定的吸附能力和光催化降解效果;(3)本发明通过调整磷酸铋与二硫化钼的比例获得最佳的吸附和光催化效果。
附图说明
图1是本发明的吸附光催化剂的XRD谱线图。
图2是本发明的吸附光催化剂的SEM照片。
图3是利用本发明的吸附光催化剂和单独磷酸铋对亚甲基蓝吸附降解情况的对比曲线图。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
实施例1
步骤1,通过水热法制备磷酸铋,将3mmol/L五水硝酸铋加入到120mL去离子水中配置五水硝酸铋水溶液,加入10.8mmol磷酸二氢钠,搅拌1h,转入到以聚四氟乙烯为内衬的高压反应釜中,160℃水热24小时,待反应釜冷却至室温后,以转速8500r/min离心将产物用去离子水和无水乙醇交替洗涤3次,120℃干燥12小时。
步骤2,通过水热法制备二硫化钼,将0.4839g钼酸铵加入到40ml去离子水中配置成钼酸铵溶液,加入0.6090g硫脲,搅拌溶解后超声处理30min,转入到50ml以聚四氟乙烯为内衬的高压反应釜中,200℃反应24小时,待反应釜冷却至室温后,以转速9500r/min离心将产物用去离子水和无水乙醇交替洗涤3次,45℃干燥12小时。
步骤3,将步骤1的磷酸铋,步骤2的二硫化钼分别称取0.5g和0.05g,并用玛瑙研钵充分研磨20分钟,然后将混合物放进马弗炉设定300℃煅烧1小时获得MoS2/MoO3/BiPO4吸附光催化剂,待产物自然冷却至室温后用玛瑙研钵再次充分研磨20分钟获得最终产品。
实施例2
步骤1,通过水热法制备磷酸铋,将3mmol/L五水硝酸铋加入到120mL去离子水中配置五水硝酸铋水溶液,加入10.8mmol磷酸二氢钠,搅拌1h,转入到以聚四氟乙烯为内衬的高压反应釜中,160℃水热24小时,待反应釜冷却至室温后,以转速8500r/min离心将产物用去离子水和无水乙醇交替洗涤3次,120℃干燥12小时。
步骤2,通过水热法制备二硫化钼,将0.4839g钼酸铵加入到40ml去离子水中配置成钼酸铵溶液,加入0.6090g硫脲,搅拌溶解后超声处理30min,转入到50ml以聚四氟乙烯为内衬的高压反应釜中,200℃反应24小时,待反应釜冷却至室温后,以转速9500r/min离心将产物用去离子水和无水乙醇交替洗涤3次,45℃干燥12小时。
步骤3,将步骤1的磷酸铋,步骤2的二硫化钼分别称取0.5g和0.1g,并用玛瑙研钵充分研磨20分钟,然后将混合物放进马弗炉设定300℃煅烧1小时获得MoS2/MoO3/BiPO4吸附光催化剂,待产物自然冷却至室温后用玛瑙研钵再次充分研磨20分钟获得最终产品。
以实施例1和2制备的MoS2/MoO3/BiPO4吸附光催化剂,依据参考文献制备的磷酸铋对亚甲基蓝吸附降解情况进行吸附光催化实验测试。
配置亚甲基蓝溶液,测定标准曲线;灯源:功率为25W,波长为254nm的紫外汞灯;称取50mg的催化剂和150mL浓度为10PPM的亚甲基蓝溶液于烧杯中,昏暗条件下超声处理20分钟,由于材料具有较好的吸附作用,进行单独的光催化实验没有重要意义,于是一个烧杯用锡纸包裹进行避光用于对照(标记为Dark),另一个烧杯在紫外灯下继续光催化实验(标记为Light)。每隔一定的时间间隔取样5ml后离心(6000rpm,4min),取上清液在654nm下测吸光度,根据标准曲线换算为浓度,用C/C0来进行评价,C和C0分别为亚甲基蓝在反应t时间和反应前的浓度。
由图3中曲线1可知,单一的磷酸铋在进行光催化降解时,未表现出明显的吸附性能,但是在30min内就能将亚甲基蓝染料废水降解75%;
由图3中曲线2、3可知,磷酸铋基催化剂在进行光催化降解时,可以发现在暗处理20min后,亚甲基蓝染料废水的吸光度就分别降低了50%和80%,说明复合材料具有一定的吸附能力,继续降解浓度继续降低;
由曲线2、4和3、5对比,在暗处理条件下亚甲基蓝溶液的浓度会降低,进一步说明材料具有吸附性质,在添加紫外灯照射后,溶液的浓度降低更多,由此说明了催化剂具有一定的光催化性能,即本发明的催化剂在吸附光催化亚甲基蓝中的应用。
根据本发明内容进行工艺参数的调整,均可实现吸附光催化剂的制备,且表现出与本发明基本一致的性能。以上对本发明做了示例性的描述,应该说明的是,在不脱离本发明的核心的情况下,任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。
Claims (10)
1.一种吸附光催化剂,其特征在于,按照下述步骤进行制备:将磷酸铋和二硫化钼进行研磨并混合均匀,置于空气氛围中自室温以每分钟5—10摄氏度的速度升温至280—300摄氏度并保温1—5小时,自然冷却至室温后研磨得到吸附光催化剂;二硫化钼和磷酸铋的质量比为(0.05—0.3):1,催化剂中存在磷酸铋、二硫化钼和MoO3混合相。
2.根据权利要求1所述的一种吸附光催化剂,其特征在于,二硫化钼和磷酸铋的质量比为(0.1—0.2):1。
3.根据权利要求1或者2所述的一种吸附光催化剂,其特征在于,将磷酸铋和二硫化钼混合均匀后,自室温以每分钟8—10摄氏度的速度升温至290—300摄氏度并保温1—2小时。
4.根据权利要求1或者2所述的一种吸附光催化剂,其特征在于,磷酸铋为磷酸铋纳米棒,通过水热法制备。
5.根据权利要求1或者2所述的一种吸附光催化剂,其特征在于,二硫化钼为二硫化钼纳米微球,通过水热法制备。
6.一种吸附光催化剂的制备方法,其特征在于,按照下述步骤进行制备:将磷酸铋和二硫化钼进行研磨并混合均匀,置于空气氛围中自室温以每分钟5—10摄氏度的速度升温至280—300摄氏度并保温1—5小时,自然冷却至室温后研磨得到吸附光催化剂;二硫化钼和磷酸铋的质量比为(0.05—0.3):1。
7.根据权利要求6所述的一种吸附光催化剂的制备方法,其特征在于,二硫化钼和磷酸铋的质量比为(0.1—0.2):1。
8.根据权利要求6或者7所述的一种吸附光催化剂的制备方法,其特征在于,将磷酸铋和二硫化钼混合均匀后,自室温以每分钟8—10摄氏度的速度升温至290—300摄氏度并保温1—2小时。
9.根据权利要求6所述的一种吸附光催化剂的制备方法,其特征在于,磷酸铋为磷酸铋纳米棒,二硫化钼为二硫化钼纳米微球,都通过水热法制备。
10.如权利要求1—5之一所述的吸附光催化剂在吸附光催化亚甲基蓝中的应用。
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