CN105618090A - 一种高效异质结紫外光催化剂及其制备方法和应用 - Google Patents
一种高效异质结紫外光催化剂及其制备方法和应用 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 38
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 27
- 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 claims abstract description 12
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
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- 238000001035 drying Methods 0.000 claims abstract description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J35/39—
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
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Abstract
本发明公开了一种高效异质结紫外光催化剂及其制备方法,所述的催化剂是由SrTiO3和BiPO4形成的异质结催化剂,其制备方法如下:将SrTiO3置于Bi(NO3)3·5H2O和Na3PO4溶液中,HNO3调节溶液pH,超声搅拌后置于水热釜内加热,产物经洗涤干燥即可得到。本发明简单易行,制备过程简单,成本低,可在紫外光的照射下高效降解亚甲基蓝(MB)溶液(降解率达97.94%),对难生物降解的栲胶、松香和糠醛生产等林产化工废水及其它工业废水有良好的应用前景。
Description
技术领域
本发明涉及到光催化材料及废水处理领域,特别是难生物降解的栲胶、松香和糠醛生产等林产化工废水及其它工业废水,具体涉及到SrTiO3/BiPO4光催化剂及其制备方法。
背景技术
当今社会,林产化工、纺织印染、制浆造纸和农药化工等行业排放的有机化工废水由于其具有颜色深、毒性大和难降解等特点,日益引起了全世界各国的高度重视。而且这些工业废水成分复杂,含有多种有机染料和芳香族化合物,使得这类废水很难降解和处理。科学家们也探索了一些处理化工废水的方法,如活性炭吸附技术、高级氧化技术、氧化絮凝技术、生化处理技术合光催化技术等等。半导体光催化技术由于在环境修复、抗菌自洁和有机废水处理中的潜在应用而备受关注。
长期以来,人们通常采用TiO2作为光催化剂,但是由于其具有较窄的吸收带和光生电子和空穴的负荷率较高和分离困难等问题,因此开发新型高效的光催化剂是现代科学研究的热点。磷酸铋(BiPO4)由于其自身独特的物理和化学特性,展现出了非常优越的光催化性能,而且磷酸根(PO4 3-)具有结构稳定、电子传输效率高、电子-空穴复合几率地和抗光腐蚀等特点,使得BiPO4的催化性能更好。Pan等人发现光催化降解有机染料时,BiPO4的催化活性是TiO2(P25,Degussa)的两倍(Environ.Sci.Technol.,2010,44,5570-5574.)。中国发明专利(CN103934010A)报道柏树叶状、正方体状、松针状和百合花状的BiPO4光催化剂的制备方法,其对于对罗丹明B(RhB)降解具有高的催化活性。然而BiPO4本身存在吸附性能差、带隙宽和受形貌影响等缺陷,因此对BiPO4及其复合结构进行调控以提高BiPO4的光催化性能成为近年来的研究热点。此外,钛酸锶(SrTiO3)具有好的热稳定性、催化活性位点多和抗腐蚀性能好等特性,也引起来科学界的广泛研究。中国发明专利(CN104437575A)报道了氟、氮共掺杂磷酸铋-氧化镍复合光催化剂的制备方法,其在紫外光照射50min后,对甲基橙的降解效率高于90%。但文献调研发现,钛酸锶/磷酸铋异质结光催化剂及其制备方法未见报道。
发明内容
发明目的:本发明的目的是为了解决紫外光下催化剂光催化效率低、稳定性差、光腐蚀性能差及光范围窄等问题,提供了一种高效异质结紫外光催化剂及其制备方法和应用。
技术方案:为实现上述技术目的,本发明提出一种高效异质结紫外光催化剂,所述的光催化剂是由SrTiO3和BiPO4组合形成的异质结催化剂,其中SrTiO3与BiPO4质量比1∶200~1∶5。
本发明进一步提出了上述高效紫外SrTiO3/BiPO4光催化剂的制备方法,包括如下步骤:
(1)制备SrTiO3粉末;
(2)制备SrTiO3/BiPO4光催化剂:将SrTiO3、铋酸盐和含磷钠盐置于蒸馏水中,超声搅拌均匀,加入硝酸调节溶液pH,然后将反应体系装于水热釜中反应,冷却后用离子水和乙醇洗涤,真空干燥,即可SrTiO3/BiPO4光催化剂。
具体地,步骤(1)中,采用共沉淀法制备SrTiO3粉末,将TiCl4的盐酸溶液和Sr(OH)2·8H2O的水溶液混合均匀,然后加入NaOH溶液,转移到水热釜中反应,干燥后即得SrTiO3粉末;
步骤(2)中,铋酸盐和磷酸盐的摩尔比为3∶1~1∶3,反应体系在水热釜中的反应条件为160~220℃下反应16~72h。
优选地,步骤(2)中,所述的铋酸盐为硝酸铋、硫酸铋、氯化铋或醋酸铋中的任意一种;所述的含磷钠盐为磷酸钠、磷酸氢二钠或磷酸二氢钠中的任意一种或两种。
步骤(2)中,使用硝酸调节溶液pH至1~4。
本发明进一步提出了上述高效紫外SrTiO3/BiPO4光催化剂在降解染料中的应用。
具体地,所述的染料为亚甲基蓝、甲基橙和罗丹明B等染料。
更进一步地,本发明提出了所述的高效紫外SrTiO3/BiPO4光催化剂在处理有机废水中的应用。
其中,所述有机废水为有机染料废水或工业有机废水。
有益效果:本发明与现有技术相比,具有以下优点:
(1)本发明方法的原料低廉、反应条件温和、工业步骤简单、环保经济,在工业废水处理领域具有潜在的价值;
(2)本发明所制备的新型的光催化剂的光催化性能高、结构稳定、使用寿命长,可有效替代贵金属催化剂;
(3)本发明制备的SrTiO3/BiPO4光催化剂属于异质结范畴,能加速光生电子和空穴快速分离,抑制和光生空穴的结合,加快对有机染料废水的降解。
具体实施方式
本发明提供了一种高效异质结紫外SrTiO3/BiPO4光催化剂,通过如下方法制备得到:
(1)制备SrTiO3粉末:利用现有技术制备SrTiO3粉末,如参照文献(Langmuir,2011,27,2946-2952.)
(2)制备SrTiO3/BiPO4光催化剂:将SrTiO3、铋酸盐和含磷钠盐按照不同的比例置于蒸馏水中,超声搅拌均匀,加入硝酸调节溶液pH,然后将反应体系装于水热釜中反应,冷却后用离子水和乙醇洗涤,真空干燥,即可SrTiO3/BiPO4光催化剂。
下面通过实施例对本发明技术方案作进一步详细说明。
实施例1
将1.1mLTiCl4稀释在2.3mL的2mol/L的盐酸溶液中,然后将2.6659gSr(OH)2·8H2O在超声波下溶于40mL去离子水中,将这两种溶液混合均匀。在上述溶液中加入13mL的6mol/L的NaOH溶液,转移到水热釜中,180℃保持48h。洗涤干燥即可得到1.73g的SrTiO3粉末。将0.0091gSrTiO3、3mmolBi(NO3)3·6H2O和3mmolNa3PO4·12H2O加入到40ml的蒸馏水中,磁力搅拌形成均匀的溶液。在磁力搅拌下,加入硝酸调节pH为1。上述溶液室温搅拌30min后,放到反应釜中180℃反应48h,冷却后用离子水和乙醇洗涤多次,真空干燥,即可得到1wt%-SrTiO3/BiPO4光催化剂(1%表示SrTiO3占整个催化剂的百分比含量)。将0.2g的BiPO4和SrTiO3/BiPO4催化剂分别加入到250mL的30mg/L的亚甲基蓝溶液中,100w的Hg灯照射,3h后亚甲基蓝的降解率分别为80.78%和92.21%。
实施例2:
SrTiO3粉末的制备方法同实施例1。将0.0270gSrTiO3、3mmolBiCl3和5mmolNa2HPO4·12H2O加入到40ml的蒸馏水中,磁力搅拌形成均匀的溶液。在磁力搅拌下,加入硝酸调节pH为2。上述溶液室温搅拌30min后,放到反应釜中160℃反应54h,冷却后用离子水和乙醇洗涤多次,真空干燥,即可得到2wt%-SrTiO3/BiPO4光催化剂。将0.2g的SrTiO3/BiPO4催化剂加入到250mL的30mg/L的亚甲基蓝溶液中,100w的Hg灯照射,3h后亚甲基蓝的降解率为94.84%。
实施例3:
SrTiO3粉末的制备方法同实施例1。将0.04570gSrTiO3、3mmolBi(Ac)3和6mmolNaH2PO4·12H2O加入到40ml的蒸馏水中,磁力搅拌形成均匀的溶液。在磁力搅拌下,加入硝酸调节pH为3。上述溶液室温搅拌30min后,放到反应釜中200℃反应24h,冷却后用离子水和乙醇洗涤多次,真空干燥,即可得到5wt%-SrTiO3/BiPO4光催化剂。将0.2g的SrTiO3/BiPO4催化剂加入到250mL的30mg/L的亚甲基蓝溶液中,100w的Hg灯照射,3h后亚甲基蓝的降解率为97.94%。
实施例4
将1.1mLTiCl4稀释在2.3mL的2mol/L的盐酸溶液中,然后将2.6659gSr(OH)2·8H2O在超声波下溶于40mL去离子水中,将这两种溶液混合均匀。在上述溶液中加入13mL的6mol/L的NaOH溶液,转移到水热釜中,180℃保持48h。洗涤干燥即可得到SrTiO3粉末。将0.0730gSrTiO3、3mmolBi2(SO4)3和3mmolNa3PO4·12H2O加入到40ml的蒸馏水中,磁力搅拌形成均匀的溶液。在磁力搅拌下,加入硝酸调节pH为1。上述溶液室温搅拌30min后,放到反应釜中200℃反应48h,冷却后用离子水和乙醇洗涤多次,真空干燥,即可8wt%-SrTiO3/BiPO4光催化剂。将0.2g的SrTiO3/BiPO4催化剂加入到250mL的COD为300mg/L的松香废水中,100w的Hg灯照射,3h后COD的去除率为61.32%。
实施例5:
将1.1mLTiCl4稀释在2.3mL的2mol/L的盐酸溶液中,然后将2.6659gSr(OH)2·8H2O在超声波下溶于40mL去离子水中,将这两种溶液混合均匀。在上述溶液中加入13mL的6mol/L的NaOH溶液,转移到水热釜中,180℃保持48h。洗涤干燥即可得到SrTiO3粉末。将0.0091gSrTiO3、3mmolBi(NO3)3·6H2O和1mmolNa2HPO4·12H2O加入到40ml的蒸馏水中,磁力搅拌形成均匀的溶液。在磁力搅拌下,加入硝酸调节pH为2。上述溶液室温搅拌30min后,放到反应釜中180℃反应24h,冷却后用离子水和乙醇洗涤多次,真空干燥,即可得到10wt%-SrTiO3/BiPO4光催化剂。将0.2g的SrTiO3/BiPO4催化剂加入到250mL的COD为300mg/L的烤胶废水中,100w的Hg灯照射,3h后COD的去除率为64.26%。
从上述实施例中可以看出,该异质结光催化剂中SrTiO3的含量影响亚甲基蓝的降解效果,在紫外光照射下,亚甲蓝的基本可以完全降解。同时,对于本发明的异质结光催化剂对其他染料,如甲基橙和罗丹明B的降解效果同时做了研究,得到了类似的结果。本发明制备的SrTiO3/BiPO4光催化剂属于异质结范畴,能加速光生电子和空穴快速分离,抑制和光生空穴的结合,加快对有机染料废水的降解。
Claims (10)
1.一种高效异质结紫外光催化剂,其特征在于,所述的光催化剂是由SrTiO3和BiPO4组合形成的异质结催化剂,其中SrTiO3与BiPO4质量比1∶200~1∶5。
2.权利要求1所述的高效异质结紫外光催化剂的制备方法,其特征在于,包括如下步骤:
(1)制备SrTiO3粉末;
(2)制备SrTiO3/BiPO4光催化剂:将SrTiO3、铋酸盐和含磷钠盐置于蒸馏水中,超声搅拌均匀,加入硝酸调节溶液pH,然后将反应体系装于水热釜中反应,冷却后用离子水和乙醇洗涤,真空干燥,即可得到SrTiO3/BiPO4光催化剂。
3.根据权利要求2所述的制备方法,其特征在于,步骤(1)中,采用共沉淀法制备SrTiO3粉末,将TiCl4的盐酸溶液和Sr(OH)2·8H2O的水溶液混合均匀,然后加入NaOH溶液,转移到水热釜中反应,干燥后即得SrTiO3粉末。
4.根据权利要求2所述的制备方法,其特征在于,步骤(2)中,铋酸盐和磷酸盐的摩尔比为3∶1~1∶3,反应体系在水热釜中的反应条件为160~220℃下反应16~72h。
5.根据权利要求2所述的制备方法,其特征在于,步骤(2)中,所述的铋酸盐为硝酸铋、硫酸铋、氯化铋或醋酸铋中的任意一种;所述的含磷钠盐为磷酸钠、磷酸氢二钠或磷酸二氢钠中的任意一种或两种。
6.根据权利要求2所述的制备方法,其特征在于,步骤(2)中,使用硝酸调节溶液pH至1~4。
7.权利要求1所述的高效异质结紫外光催化剂在降解染料中的应用。
8.根据权利要求7所述的应用,其特征在于,所述的染料为亚甲基蓝、甲基橙和罗丹明B中的任意一种或几种的混合物。
9.权利要求1所述的高效异质结紫外光催化剂在降解有机染料废水或工业有机废水中的应用。
10.根据权利要求9所述的应用,其特征在于,将高效异质结紫外光催化剂加入到待处理的有机染料废水或工业有机废水中,紫外照射2~5h,其中,催化剂的添加量为每g染料添加2~10mg催化剂。
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