CN106984324B - 可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法 - Google Patents
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- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 title claims abstract description 25
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- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
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- 229910001981 cobalt nitrate Inorganic materials 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 6
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- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法,称取NH4VO3固体,溶解于去离子水中,获得NH4VO3水溶液;称取Cu(NO3)2·3H2O固体,溶解于上述NH4VO3水溶液中;将溶液转移到高压反应釜中,再将反应釜置于高温干燥箱中;反应结束后冷至室温,用循环水式多用真空泵过滤样品,用去离子水充分洗涤过滤,干燥过夜;将充分干燥后的样品研磨,得到水热法制备的可见光响应型笼型结构钒酸铜水合物光催化剂。本发明制备的光催化剂可作为产氧剂用于可见光下分解水产氧,其产氧量远远高于目前所熟知的其他产氧剂。本发明制备方法简单,成本低,光催化性能优异,可应用于能源转换及环境治理等领域。
Description
技术领域
本发明化工领域,涉及一种光催化剂,具体来说是一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法。
背景技术
随着环境污染和能源危机日益加剧,环境治理和可再生能源利用受到广泛关注。其中光催化技术具有操作简单、绿色无污染、可直接转化利用太阳能等优点,成为当代化学与材料研究领域热点之一。而传统光催化材料TiO2,由于其能带隙过大(3.2eV左右)导致其只在紫外光激发下才具有光催化活性,紫外光部分能量仅占太阳能总能量约4%,而未利用的可见光能量占43%左右,因此开发出高效稳定的可见光响应光催化剂成为了光催化领域的研究热点。
过渡金属钒酸盐材料,包括BiVO4、Cu3V2O8、InVO4、Ag3VO4和Ag2V4O11等,一直以来在电催化和锂电池等领域都有着极为广泛的应用。其中,Cu3V2O7(OH)2·2H2O水钒铜矿作为一种天然矿产,自从被人类发现以来,大多数研究均基于其结构和磁性的性质研究,以及钠离子电池和超级电容器领域的应用研究。迄今为止,有关Cu3V2O7(OH)2·2H2O光催化性能的研究未见报道,尤其是光解水产氧方面。基于其笼型晶格结构特性,Cu3V2O7(OH)2·2H2O极可能是一种极具潜力的光催化材料,因此探究Cu3V2O7(OH)2·2H2O可见光催化性能具有一定的研究价值,此外,明晰Cu3V2O7(OH)2·2H2O的光催化活性与其特殊晶体结构之间的构-效关系有助于解释材料光催化机制。
发明内容
针对现有技术中的上述技术问题,本发明提供了一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法,所述的这种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法要解决现有技术中的光催化剂可见光光催化效果不佳的技术问题。
本发明提供了一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法,包括如下步骤:
1)称取NH4VO3固体,溶解于70~90℃去离子水中,搅拌至NH4VO3溶解完全,获得浓度为0.04~0.08mol/L的NH4VO3水溶液;
2)称取Cu(NO3)2·3H2O固体,溶解于上述NH4VO3水溶液中,所述的NH4VO3与Cu(NO3)2·3H2O的摩尔之比为2:3,搅拌至Cu(NO3)2·3H2O溶解完全;
3)将溶液转移到高压反应釜中,再将反应釜置于高温干燥箱中,反应温度为180℃,反应时间为8h,反应时间从升温到180℃开始计时;
4)反应结束后取出反应釜,空气中冷至室温,用循环水式多用真空泵过滤样品,用去离子水充分洗涤过滤,放入80℃真空干燥箱中过夜干燥;
5)将充分干燥后的样品研磨,得到水热法制备的可见光响应型笼型结构钒酸铜水合物光催化剂。
进一步的,步骤1)中离子水的温度为80℃。
本发明还提供了上述制备的光催化剂用于可见光催化降解有机染料亚甲基蓝中。
本发明还提供了上述制备的光催化剂用于催化分解水产氧剂中。
本发明以NH4VO3和Cu(NO3)2·3H2O为原料,在高温干燥箱中反应温度为180℃的条件下,水热8h制备出笼型结构钒酸铜水合物光催化剂,再以亚甲基蓝为目标有机污染物,通过测试黑暗条件下亚甲基蓝被光催化剂吸附后其吸光度随时间变化情况表征光催化材料的亚甲基蓝吸附性能;再在可见光照射下(λ>420nm),通过计算亚甲基蓝降解速率表征其可见光光催化活性。本发明采用简单水热处理制备Cu3V2O7(OH)2·2H2O光催化剂具有极强的亚甲基蓝吸附性能及优异可见光亚甲基蓝降解和分解水产氧活性。
本发明制备的V基光催化剂HT在可见光下具有高光催化活性,可见光(>420nm)下催化80min时,HT对亚甲基蓝(50ppm)的降解率已经达到90%,其光催化降解有机污染物亚甲基蓝活性远高于其他焙烧或共沉淀制备的V基样品。本发明制备的V基光催化剂HT还可作为产氧剂用于可见光下分解水产氧,其产氧量远远高于目前所熟知的其他产氧剂。综合来看,该样品制备方法简单,成本低,光催化性能优异,可应用于能源转换及环境治理等领域。
本发明和已有技术相比,其技术进步是显著的。以亚甲基蓝为目标污染物,在可见光激发下(λ>420nm),使用水热法制备的HT可见光催化剂具有优于CP、CC-200、CC-250、CC-300、CP-2000、P25等样品的强物理吸附性能和可见光催化降解活性;在可见光激发下,所制备的HT光催化剂产氧效果要优于BiVO4、WO3、g-C3N4等目前常见产氧光催化剂;而且Cu3V2O7(OH)2·2H2O是一种天然矿产,在自然界中储量丰富,其实验室制备工艺简单,反应条件温和,合成成本低,有利于实现规模化生产,具有巨大的经济价值和社会价值。
附图说明
图1为采用本发明方法制备的笼型结构钒酸铜水合物光催化剂X射线衍射图。
图2为采用本发明方法制备的笼型结构钒酸铜水合物光催化剂扫描电镜图。
图3a为采用本发明方法制备的笼型结构钒酸铜水合物光催化剂黑暗条件下对亚甲基蓝(50ppm)的吸附-时间曲线。
图3b为采用本发明方法制备的笼型结构钒酸铜水合物光催化剂可见光照射下(λ>420nm)对亚甲基蓝(50ppm)的光催化降解-时间曲线。
图4为采用本发明方法制备的笼型结构钒酸铜水合物光催化剂可见光照射下(λ>420nm)在不同硝酸钴负载量时光催化分解水产氧速率。
具体实施方式
以下用实例对本发明作进一步说明,但不限于此。
实施例1:
笼型结构钒酸铜水合物光催化剂制备具体步骤:
(1)称取0.2808g(0.0024mol)NH4VO3固体,溶解于40ml 80℃去离子水中,搅拌至NH4VO3溶解完全,获得浓度为0.06mol/L的NH4VO3水溶液;
(2)称取0.8698g(0.0036mol)Cu(NO3)2·3H2O固体,溶解于上述NH4VO3水溶液中,搅拌至Cu(NO3)2·3H2O溶解完全;
(3)将溶液用循环水式多用真空泵过滤,用去离子水充分洗涤过滤固体,放入80℃真空干燥箱中过夜干燥,将充分干燥后的样品研磨,获得共沉淀法制备的Cu3V2O7(OH)2·2H2O样品(简称CP);
(4)将溶液转移到高压反应釜中,再将反应釜置于高温干燥箱中,反应温度为180℃,反应时间为8h(从升温到180℃开始计时);
(5)反应结束后立马取出反应釜,空气中冷至室温。用循环水式多用真空泵过滤样品,用去离子水充分洗涤过滤,放入80℃真空干燥箱中过夜干燥;
(6)将充分干燥后的样品研磨,得到水热法制备的Cu3V2O7(OH)2·2H2O样品(简称HT);
(7)将水热法制备的纯相Cu3V2O7(OH)2·2H2O样品,在持续通入氩气的管式炉中分别焙烧200℃、250℃、300℃,获得样品分别标记为CC-200、CC-250、CC-300。
(8)将共沉淀法制备的纯相Cu3V2O7(OH)2·2H2O样品,在持续通入氩气的管式炉中焙烧200℃,获得样品标记为CP-200。
图1为笼型结构钒酸铜水合物光催化剂X射线衍射图,由图1可知,按照上述步骤,可以制备出纯相高结晶度的笼型结构钒酸铜水合物。图2为笼型结构钒酸铜水合物光催化剂扫描电镜图,由图2可知,按照上述步骤制备出的可见光响应型笼型结构钒酸铜水合物光催化剂有着不同的微观形貌。
实施例2:高效V基可见光催化剂性能分析
分别取10mg HT、CP、CC-200、CC-250、CC-300、CP-2000、P25样品粉末,加入到50ml50ppm的亚甲基蓝溶液中,在黑暗条件下搅拌溶液直至催化剂吸附-脱附平衡,并在吸附0min、10min、30min、60min、90min、150min时,在以上6种溶液中分别取3ml,除去光催化剂后测试亚甲基蓝溶液的吸光度;
吸附-脱附平衡后,打开已装有滤光片(λ>420nm)的光催化反应仪汞灯(500W),在可见光条件下照射溶液直至亚甲基蓝降解完全,同时在0min、1min、3min、5min、10min、20min、50min、80min、140min时,在以上6种溶液中分别取X ml,除去光催化剂后测试亚甲基蓝溶液的吸光度,对比6种样品的可见光催化降解性能。
图3(a)为黑暗条件下笼型结构钒酸铜水合物光催化剂对亚甲基蓝(50ppm)的吸附-时间曲线;图3(b)可见光照射下(λ>420nm)笼型结构钒酸铜水合物光催化剂对亚甲基蓝(50ppm)的光催化降解-时间曲线。由图3可知,以亚甲基蓝为目标污染物,在可见光激发下(λ>420nm),使用水热法制备的HT可见光催化剂具有优于CP、CC-200、CC-250、CC-300、CP-2000、P25等样品的强物理吸附性能和可见光催化降解活性,同时HT黑暗条件下吸附脱附污染物的活性也为最佳。
实施例3
取50mg HT、BiVO4、WO3、g-C3N4样品,分别分散于50ml去离子水中,在获得的4种溶液中继续加入20mg NaIO3作为牺牲剂。在容器中充分搅拌溶液,并使用高纯氮气赶走溶液和容器中的空气。在保证良好气密性的容器中,在可见光条件下照射溶液(λ>420nm);
可见光照射1h后,测量不同溶液单位小时产氧量,并分别在光催化剂上负载0wt%硝酸钴,于2h后测量不同溶液单位小时产氧量。继续负载0.4wt%硝酸钴,于3h后测量不同溶液单位小时产氧量。继续负载1.2wt%硝酸钴,于4h后测量不同溶液单位小时产氧量。继续负载2.0wt%硝酸钴,于5h后测量不同溶液单位小时产氧量。最后负载3.0wt%硝酸钴,于6h后测量不同溶液单位小时负氧量。对比4种样品的可见光催化产氧性能,确定V基可见光催化剂上硝酸钴的最优负载比例。
硝酸钴在HT光催化剂上的负载比例为2.0wt%时,HT样品的可见光催化产氧效果最好。
图4为可见光照射下(λ>420nm)笼型结构钒酸铜水合物光催化剂在不同硝酸钴负载量时光催化分解水产氧速率,由图4可知,在可见光激发下,所制备的HT光催化剂产氧效果要优于BiVO4、WO3、g-C3N4等目前常见产氧光催化剂。
上述内容仅为本发明构思下的基本说明,而依据本发明的技术方案所做的任何等效变换,均应属本发明的保护范围。
Claims (4)
1.一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法,其特征在于包括如下步骤:
1)称取NH4VO3固体,溶解于70~90℃去离子水中,搅拌至NH4VO3溶解完全,获得浓度为0.04~0.08 mol/L的NH4VO3水溶液;
2)称取Cu(NO3)2·3H2O固体,溶解于上述NH4VO3水溶液中,所述的NH4VO3与Cu(NO3)2·3H2O的摩尔之比为2:3,搅拌至Cu(NO3)2·3H2O溶解完全;
3)将溶液转移到高压反应釜中,再将反应釜置于高温干燥箱中,反应温度为180℃,反应时间为8 h,反应时间从升温到180℃开始计时;
4)反应结束后取出反应釜,空气中冷至室温,用循环水式多用真空泵过滤样品,用去离子水充分洗涤过滤,放入80℃真空干燥箱中过夜干燥;将充分干燥后的样品研磨,将充分干燥后的样品研磨,得到水热法制备的可见光响应型笼型结构钒酸铜水合物光催化剂。
2.根据权利要求 1 所述一种可见光响应型笼型结构钒酸铜水合物光催化剂的制备方法,其特征在于:步骤1)中去离子水的温度为80℃。
3.权利要求1制备的光催化剂用于可见光催化降解有机染料亚甲基蓝中。
4.权利要求1制备的光催化剂用于催化分解水产氧。
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