CN108607539A - 一种片状三氧化钨及其制备方法和用作光催化剂的用途 - Google Patents
一种片状三氧化钨及其制备方法和用作光催化剂的用途 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000011941 photocatalyst Substances 0.000 title abstract description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 229910020350 Na2WO4 Inorganic materials 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 14
- 229960000907 methylthioninium chloride Drugs 0.000 description 14
- 239000000243 solution Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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Abstract
本发明公开了一种片状三氧化钨及其制备方法和用作光催化剂的用途,制备方法包括如下步骤:步骤S1,取适量Na2WO4·2H2O溶于硝酸溶液中,搅拌;步骤S2,通过离心分离得淡黄色沉淀,然后用去离子水洗涤;步骤S3,步骤S2所得产物在常温下干燥过夜,即得。本发明提供了一种片状WO3·2H2O,具有优异的光催化活性,具有良好的应用前景,可用于制备光催化剂。本发明还提供了片状WO3·2H2O的制备方法,步骤简单、可控,成本低廉,可推广性强。
Description
技术领域
本发明属于化学领域,涉及一种片状WO3·2H2O及其制备方法和用作光催化剂的用途。
背景技术
进入21世纪,人类面临着能源和环境两个非常严峻的问题,特别是有毒且难降解有机污染物(如多环芳烃、多氯联苯、农药、染料等)引起的环境问题,已成为影响人类生存与健康的重大问题。利用半导体氧化物材料在太阳光照射下表面能受激活化的特性,可有效地氧化分解有机污染物。与传统的净化环境处理方法相比,半导体光催化技术拥有反应条件温和、无二次污染、操作简单和降解效果显著等优势。自光催化技术开发以来,研究和应用最多的光催化剂是TiO2。但是TiO2是紫外光响应型光催化剂,对光能的利用率十分低,因此寻找性能优异的新型光催化材料以获得具有高效光催化活性的光催化剂非常有意义。WO3有着广泛的用途,不仅用于气敏元件和电致变色的研究,也广泛用于研究光催化。我国钨的储量丰富,位居世界第一。它的禁带宽度小,约为2.5V,光吸收范围广(小于500nm的可见光),能有效利用占太阳辐射能量近一半的可见光。但其产生的光生电子空穴对很容易复合,导致电子和空穴不能及时迁移至表面参与氧化还原反应,从而光转化效率较低。
发明内容
本发明目的在于提供一种片状WO3·2H2O及其制备方法和用作光催化剂的用途。
本发明的上述目的是通过下面的技术方案得以实现的:
一种三氧化钨,为片状WO3·2H2O。
上述三氧化钨的制备方法,包括如下步骤:
步骤S1,取适量Na2WO4·2H2O溶于硝酸溶液中,搅拌;
步骤S2,通过离心分离得淡黄色沉淀,然后用去离子水洗涤;
步骤S3,步骤S2所得产物在常温下干燥过夜,即得。
优选地,硝酸溶液浓度为4.8mol/L。
优选地,取400mg的Na2WO4·2H2O溶于300mL的4.8mol/L硝酸溶液中。
优选地,步骤S1于20℃搅拌72小时。
上述三氧化钨用于制备光催化剂的用途。
有益效果:
本发明提供了一种片状WO3·2H2O,具有优异的光催化活性,具有良好的应用前景,可用于制备光催化剂。本发明还提供了片状WO3·2H2O的制备方法,步骤简单、可控,成本低廉,可推广性强。
附图说明
图1为实施例1所制备的二水合三氧化钨的扫面电子显微镜(SEM)图;由图1可见,产品呈均匀片状结构。
图2为实施例1所制备的产品的X射线衍射(XRD)图;由图2可以看出,制备出的WO3·2H2O和WO3产品分别与标准卡(JCPDS:18-1420)(JCPDS:83-0950)一致,证明制备出的样品是纯相二水合三氧化钨。
图3为测试制备的WO3·2H2O光催化剂和WO3在降解含有亚甲基蓝(MB)的染料废水溶液的活性对比图。其中C0为MB的初始浓度,C为经过可见光照射一段时间后测量的MB浓度,t为时间。由图3可以看出,WO3·2H2O降解MB的速率较WO3有比较大的提高。
具体实施方式
下面结合附图和实施例具体介绍本发明实质性内容,但并不以此限定本发明的保护范围。
实施例1:
将400mg Na2WO4·2H2O溶于300mL的4.8mol/L硝酸溶液中,室温下搅拌混合物72小时;离心分离得到淡黄色沉淀,再用去离子水洗涤数次;最后,粉末状产物在室温下干燥过夜,得到产品WO3·2H2O。再在300摄氏度低温脱水得到产品WO3。WO3·2H2O的扫面电子显微镜(SEM)图如图1所示,WO3·2H2O和WO3的X射线衍射(XRD)图如图2所示。
测试例:
将实施例1制得到的WO3·2H2O光催化剂、纯相的WO3,降解含有MB的废水溶液。
称取样品0.1g,分别加入200ml MB水溶液,其中MB浓度都10mg/L,先避光搅拌30min,使染料在催化剂表面达到吸附/脱附平衡。然后开启氙灯光源在可见光照射下进行光催化反应,每30min取上清液用分光光度计检测。根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化。当吸光物质相同、厚度相同时,可以用吸光度的变化直接表示溶液浓度的变化。因为MB在556nm处有一个特征吸收峰,所以可以利用吸光度的变化来衡量溶液中MB的浓度变化。从图上(横坐标:紫外光照射时间;纵坐标:经过紫外光照射一段时间后测量的MB浓度值与MB的初始浓度的比值。)可以看出光照150min后,WO3·2H2O光催化剂降解MB高达82.5%,与纯相的WO3相比,WO3·2H2O光催化剂对MB显示出更高的催化活性(图3)。
我们通过在层状WO3晶体内加入两个结晶水的方法进一步提高其可见光利用率,同时,降低其电子空穴的复合效率。在此,我们通过简单的沉淀法得到WO3·2H2O。在已有报道中,方岩雄等报道了一种单层水合三氧化钨纳米片及制备方法(申请公布号:CN201710702469.3)。目前,还没有关于二水合三氧化钨纳米片的制备及其性能的报道。因为我们制备WO3·2H2O的方案简单并且产品显示出较好的可见光响应性能,所以我们合成的二水合三氧化钨具有更广阔的应用前景。
上述实施例的作用在于具体介绍本发明的实质性内容,但本领域技术人员应当知道,不应将本发明的保护范围局限于该具体实施例。
Claims (6)
1.一种三氧化钨,其特征在于为片状WO3·2H2O。
2.权利要求1所述三氧化钨的制备方法,其特征在于,包括如下步骤:
步骤S1,取适量Na2WO4·2H2O溶于硝酸溶液中,搅拌;
步骤S2,通过离心分离得淡黄色沉淀,然后用去离子水洗涤;
步骤S3,步骤S2所得产物在常温下干燥过夜,即得。
3.根据权利要求2所述的制备方法,其特征在于:硝酸溶液浓度为4.8mol/L。
4.根据权利要求3所述的制备方法,其特征在于:取400mg的Na2WO4·2H2O溶于300mL的4.8mol/L硝酸溶液中。
5.根据权利要求2所述的制备方法,其特征在于:步骤S1于20℃搅拌72小时。
6.权利要求1所述三氧化钨用于制备光催化剂的用途。
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