CN114950463B - 一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 - Google Patents
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 Download PDFInfo
- Publication number
- CN114950463B CN114950463B CN202210769256.3A CN202210769256A CN114950463B CN 114950463 B CN114950463 B CN 114950463B CN 202210769256 A CN202210769256 A CN 202210769256A CN 114950463 B CN114950463 B CN 114950463B
- Authority
- CN
- China
- Prior art keywords
- moo
- srfe
- solution
- prepared
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000003197 catalytic effect Effects 0.000 claims abstract description 6
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000002349 favourable effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 230000015556 catabolic process Effects 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 15
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000004098 Tetracycline Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000013264 metal-organic assembly Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 229960002180 tetracycline Drugs 0.000 description 2
- 229930101283 tetracycline Natural products 0.000 description 2
- 235000019364 tetracycline Nutrition 0.000 description 2
- 150000003522 tetracyclines Chemical class 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011206 ternary composite Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8872—Alkali or alkaline earth metals
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/612—Surface area less than 10 m2/g
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,其属于无机催化材料领域。本发明先制备了SrFe12O19和MoO3,再通过简单的水热法得到了MoO3/SrFe12O19复合光催化剂。本发明方法制备工艺简单,使用设备本少且生产成本低。制备的MoO3/SrFe12O19光催化活性高,在模拟太阳光照射下,制备的0.03g复合光催化材料降解100mL浓度为10mg/L的罗丹明B溶液,70min降解率达到96.6%。四次回收重复使用后,复合磁性光催化剂在相同降解条件下对罗丹明B溶液的降解率仍达89%,本发明制备出的产品可广泛用于光催化降解有机污染物的领域中。
Description
技术领域
本发明涉及一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,属于无机催化材料技术领域。
背景技术
与传统废水处理技术相比,以太阳光为驱动的半导体光催化技术由于反应条件温和、降解速率高和产物相对无毒害等特点,受到学者广泛关注。研究发现,ZnO、SnO2、WO3、CuO和MoO3等金属氧化物具有优异的光学性质和结构特性,被广泛应用于光催化降解废水、CO2还原和水裂解制H2等领域。其中,三氧化钼(MoO3)具有活性高、化学稳定性好和成本低等优点,具备作为光催化剂的潜质。三氧化钼有四种晶型,包括:正交相α-MoO3、单斜相β-MoO3、六方相h-MoO3和高压单斜相MoO3-Ⅱ。α-MoO3具有各向异性的层状结构,这使得其具有较高的化学稳定性,是三氧化钼的热力学稳定相。其禁带宽度区间为2.9~3.5eV,主要制备方法有水热法、溶胶-凝胶法、焙烧法和共沉淀法等。然而,现阶段制备的MoO3多为粉末状,反应后悬浮于体系中,难以回收,这制约了MoO3的产业化发展。将光催化剂与磁性材料结合构筑磁性光催化剂,能为半导体光催化材料的循环回收和重复使用提供参考。硬磁性半导体材料锶铁氧体(SrFe12O19)具有饱和磁化强度高、磁导率高、稳定性好和损耗低等优点;与软磁性材料Fe3O4、Fe2O3等相比,SrFe12O19的磁稳定性好、饱和磁化强度高且抗退磁能力更强;此外,作为n型半导体,SrFe12O19带隙宽度较小(2.0eV),响应可见光范围广,且我国锶储量丰富,能被广泛利用。
目前,研究者结合金属氧化物、铋系化合物、非金属半导体材料和金属有机框架等不同改性材料,制备得到了降解性能较好的MoO3基光催化剂,以改善宽禁带MoO3吸收光范围有限和光生电子-空穴对复合等缺陷。如“Journal of Energy Chemistry”,第29卷第65-71页“Construction of a few-layer g-C3N4/α-MoO3nanoneedles all-solid-state Z-scheme photocatalytic system for photocatalytic degradation”一文,分别采用水热法和焙烧法制备出MoO3和g-C3N4,再将两者进行水热复合制备出g-C3N4/α-MoO3光催化剂。该方法的不足之处是:(1)复合光催化剂的活性较低,在模拟太阳光照射下10wt%g-C3N4/α-MoO3光催化剂在120min对罗丹明B的降解率仅为71.86%;(2)复合催化剂存在回收困难问题,容易引发二次污染。又如,中国发明专利公开了“一种纳米带状MOA复合光催化剂制备方法”,在微波水热法制备的MoO3表面沉积AgBr得到异质结构MOA(MoO3/AgBr)。该方法存在的问题是:(1)制备复合物过程涉及到表面活性剂聚乙烯吡咯烷酮(PVP)和硝酸银,致使成本高,不适合推广;(2)MoO3光催化剂的制备条件严苛,需要严格控制pH和温度,对于大规模的工业化应用并不适合;(3)复合催化剂存在回收困难问题,容易引发二次污染。再如,“PLOSONE”2020年8月15卷第8期“Novel magnetic Fe3O4/g-C3N4/MoO3 nanocomposites withhighly enhanced photocatalytic activities:Visible-light-driven degradation oftetracycline from aqueous environment”一文,先以高温煅烧法分别制备出MoO3和g-C3N4,然后在80℃搅拌下制得Fe3O4/g-C3N4,再用高温煅烧法合成三元复合光催化剂Fe3O4/g-C3N4/MoO3。该方法的不足之处是:(1)制备过程采用高温煅烧法,制备工艺繁琐,能耗大;MoO3前驱体制备处于酸性条件,且焙烧均需在氮气保护下进行;(2)复合光催化剂活性有限,在1000W Xe灯模拟太阳光下Fe3O4/g-C3N4/MoO3在120min对50mL四环素废水的降解率仅为94%;(3)未开展磁回收再利用活性测试,无法判断材料的重复使用性和稳定性。
发明内容
本发明针对MoO3的催化活性不佳和粉末催化剂难以回收等问题,制备了一种新型磁性复合光催化剂MoO3/SrFe12O19,旨在提高复合光催化剂活性的同时,为材料的循环回收和重复利用提供参考。该制备工艺方法简单,复合光催化剂的催化活性高且成本低,对拓展MoO3基光催化剂的研究及光催化技术处理染料废水提供了技术支撑。本发明MoO3/SrFe12O19复合光催化材料的制备方法如下:
(1)SrFe12O19的制备
分别称取0.5332g的SrCl2·6H2O和2.1624g的FeCl3·6H2O试剂,用20mL去离子水超声溶解10min得到混合液A;称取3.3598g的NaOH试剂,用15mL去离子水超声溶解得到溶液B;30min连续磁力搅拌下,将B液缓慢滴加到A液中,得到棕褐色前驱体溶液C;将C液移入50mL高压反应釜,在200℃下反应24h,自然冷却至室温,用去离子水和稀盐酸交替洗至中性后,置于80℃烘箱下烘干12h,取出研磨,得到深棕色粉末状的SrFe12O19。
(2)MoO3的制备
称取1.5g的(NH4)6Mo7O24·4H2O试剂,用39mL去离子水超声溶解形成均一透明溶液A;将配置好的21mL浓度为3mol/L的稀硝酸溶液缓慢加入A液中,继续机械搅拌10min,得到均一透明的浅黄色前驱体溶液B;将B液置于100mL高压反应釜密闭中,在180℃反应20h,自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到白色粉末状的MoO3。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为3wt%~20wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19。
本发明采用上述技术方案,主要有以下效果:
(1)本发明方法制备的MoO3/SrFe12O19复合光催化材料具有较高的光催化活性,在模拟太阳光的氙灯照射下(340~800nm),将0.03g制备的最优复合磁性光催化材料分散于100mL浓度为10mg/L罗丹明B溶液中,光照70min,降解率达到了96.6%。
(2)本发明采用水热制备,复合光催化材料比表面积达10.0m2/g,制备方法简单,所需设备少,成本低。
(3)本发明方法制备的MoO3/SrFe12O19复合光催化材料可在外加磁场下进行回收,四次重复使用后对罗丹明B溶液的降解率达89%。
附图说明
图1为SrFe12O19、MoO3和MoO3/SrFe12O19的X射线衍射图。
图2为MoO3、MoO3/SrFe12O19和SrFe12O19的FT-IR图。
图3为SrFe12O19、MoO3和MoO3/SrFe12O19的SEM图。
图4为MoO3、SrFe12O19和不同质量比MoO3/SrFe12O19的降解率对比图。
具体实施方式
下面结合具体实施方式,进一步说明本发明。
实施例1
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,具体步骤如下:
(1)SrFe12O19的制备
分别称取0.5332g的SrCl2·6H2O和2.1624g的FeCl3·6H2O试剂,用20mL去离子水超声溶解10min得到混合液A;称取3.3598g的NaOH试剂,用15mL去离子水超声溶解得到溶液B;30min连续磁力搅拌下,将B液缓慢滴加到A液中,得到棕褐色前驱体溶液C;将C液移入50mL高压反应釜,在200℃下反应24h,自然冷却至室温,用去离子水和稀盐酸交替洗至中性后,置于80℃烘箱下烘干12h,取出研磨,得到深棕色粉末状的SrFe12O19。
(2)MoO3的制备
称取1.5g的(NH4)6Mo7O24·4H2O试剂,用39mL去离子水超声溶解形成均一透明溶液A;将配置好的21mL浓度为3mol/L的稀硝酸溶液缓慢加入A液中,继续机械搅拌10min,得到均一透明的浅黄色前驱体溶液B;将B液置于100mL高压反应釜密闭中,在180℃反应20h,自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到白色粉末状的MoO3。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为3wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19(MS-3)。
实施例2
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,具体步骤如下:
(1)同实施例1中(1)。
(2)同实施例1中(2)。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为5wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19(MS-5)。
实施例3
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,具体步骤如下:
(1)同实施例1中(1)。
(2)同实施例1中(2)。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为10wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19(MS-10)。
实施例4
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,具体步骤如下:
(1)同实施例1中(1)。
(2)同实施例1中(2)。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为15wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19(MS-15)。
实施例5
一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,具体步骤如下:
(1)同实施例1中(1)。
(2)同实施例1中(2)。
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为20wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19(MS-20)。
实验结果
实施例2制备的磁性复合光催化剂MoO3/SrFe12O19催化降解活性最佳。
SrFe12O19的XRD如图1(a)所示,在衍射角2θ=15.38°、23.15°、30.14°、31.04°、32.35°、34.24°、35.79°、37.18°、40.46°、42.59°、55.25°、56.85°、63.21°、67.67°和76.7°处可以观察到SrFe12O19特征衍射峰,分别对应于标准卡片(JCPDS No.33-1340)的(004)、(006)、(110)、(008)、(107)、(114)、(108)、(203)、(205)、(206)、(217)、(2011)、(220)、(2014)和(1018)晶面,证实了M型SrFe12O19的成功制备。SrFe12O19的红外吸收光谱如图2(c)所示,在435.26cm-1、550.65cm-1和587.21cm-1处的峰是SrFe12O19的特征吸收峰。
MoO3的XRD图如图1(a),在12.76°、23.33°、25.7°、27.33°、38.98°、45.74°、46.28°和67.53°处的衍射峰均对应纯MoO3特征峰(JCPDS No.05-0508),分别归属于(020)、(110)、(040)、(021)、(060)、(200)、(210)和(0100)晶面,证明了样品为正交结构的α-MoO3。且(0k0)晶面(k=2、4和6)为样品的择优晶面,说明制备的MoO3具有各向异性的层状晶体结构。MoO3的红外吸收光谱如图2(a),996.97cm-1、876.95cm-1和552.77cm-1处的峰值分别归属于Mo=O双键拉伸振动、Mo-O-Mo单键的拉伸振动和三配位氧(O-3Mo)的拉伸模式,证实了样品中存在MoO3的完整晶型。
复合光催化材料的XRD衍射如图1(c)所示,MoO3/SrFe12O19样品的衍射峰不仅出现了SrFe12O19的(008)、(107)、(114)和(205)特征衍射峰,而且MoO3的(020)、(110)、(040)、(021)、(060)、(200)、(210)和(0100)特征衍射峰同时存在,衍射峰尖锐且没有杂峰的出现,表明复合样品中两相能很好结合并稳定共存,MoO3/SrFe12O19制备成功。MoO3/SrFe12O19的红外吸收光谱如图2(b),其在435.3cm-1附近的微弱拉伸振动对应纯相SrFe12O19的特征吸收,表明制备的复合光催化剂中存在SrFe12O19;996.97cm-1、876.95cm-1和552.77cm-1处的吸收峰归属于MoO3,再次说明MoO3/SrFe12O19复合磁性光催化剂的成功合成。
SrFe12O19、MoO3和MoO3/SrFe12O19的SEM如图3所示。从图3(a)可以看出,SrFe12O19为六边形片状,图3(b)MoO3则为条带状,图3(c)为MoO3/SrFe12O19的形貌图,可见条带状MoO3周围负载有六边形片状SrFe12O19,复合样品形貌特征明显,证明MoO3/SrFe12O19制备成功。
光催化实验结果如图4所示,在300W Xe灯模拟太阳光照射下,制备的0.03g复合光催化材料MS-5降解100mL浓度为10mg/L的罗丹明B溶液时活性最好,70min对罗丹明B的降解率达到96.6%。反应结束后回收再利用,第四次使用回收的MS-5对罗丹明B的降解率仍能达到89%。
磁性能参数测试表明,MoO3/SrFe12O19的饱和磁化强度(Ms)为2.8emu/g,矫顽力(Hci)为1037.1Oe,说明以本方法制备的磁性复合光催化剂具有良好的磁性能优势,有利于光催化剂的磁回收利用。
Claims (2)
1.一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,包括以下步骤:
(1)SrFe12O19的制备
分别称取0.5332g的SrCl2·6H2O和2.1624g的FeCl3·6H2O试剂,用20mL去离子水超声溶解10min得到混合液A;称取3.3598g的NaOH试剂,用15mL去离子水超声溶解得到溶液B;30min连续磁力搅拌下,将B液缓慢滴加到A液中,得到棕褐色前驱体溶液C;将C液移入50mL高压反应釜,在200℃下反应24h,自然冷却至室温,用去离子水和稀盐酸交替洗至中性后,置于80℃烘箱下烘干12h,取出研磨,得到深棕色粉末状的SrFe12O19;
(2)MoO3的制备
称取1.5g的(NH4)6Mo7O24·4H2O试剂,用39mL去离子水超声溶解形成均一透明溶液A;将配置好的21mL浓度为3mol/L的稀硝酸溶液缓慢加入A液中,继续机械搅拌10min,得到均一透明的浅黄色前驱体溶液B;将B液置于100mL高压反应釜密闭中,在180℃反应20h,自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到白色粉末状的MoO3;
(3)MoO3/SrFe12O19的制备
称取0.1425g的已制备好的MoO3粉末,用15mL去离子水超声溶解3min得到混合溶液A;按照理论生成SrFe12O19在复合物中的质量百分数为3wt%~20wt%,称取SrFe12O19粉末加入A液中,超声为30min,得到灰褐色的前驱体溶液B;将B液转移到50mL高压反应釜中,在150℃反应4h自然冷却至室温,用去离子水和无水乙醇反复抽滤润洗得到滤饼,置于80℃烘箱中干燥12h,取出研磨,得到浅灰色粉末状的MoO3/SrFe12O19。
2.根据权利要求1所述的一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法,其特征在于提高MoO3催化活性的同时,使其利于通过外加磁场进行回收再利用。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210769256.3A CN114950463B (zh) | 2022-07-01 | 2022-07-01 | 一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210769256.3A CN114950463B (zh) | 2022-07-01 | 2022-07-01 | 一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN114950463A CN114950463A (zh) | 2022-08-30 |
CN114950463B true CN114950463B (zh) | 2023-09-08 |
Family
ID=82968225
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210769256.3A Active CN114950463B (zh) | 2022-07-01 | 2022-07-01 | 一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114950463B (zh) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105645470A (zh) * | 2014-09-09 | 2016-06-08 | 天津工业大学 | 一种三氧化钼纳米薄片的制备方法 |
CN108452813A (zh) * | 2018-03-23 | 2018-08-28 | 重庆大学 | 一种MoS2/SrFe12O19复合磁性光催化剂的制备方法 |
CN108911731A (zh) * | 2018-08-30 | 2018-11-30 | 安徽工业大学 | 一种六角晶系m型锶铁氧体粉末的制备方法 |
CN111974407A (zh) * | 2020-07-13 | 2020-11-24 | 重庆大学 | 一种制备磁性三氧化钨复合光催化剂的方法 |
-
2022
- 2022-07-01 CN CN202210769256.3A patent/CN114950463B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105645470A (zh) * | 2014-09-09 | 2016-06-08 | 天津工业大学 | 一种三氧化钼纳米薄片的制备方法 |
CN108452813A (zh) * | 2018-03-23 | 2018-08-28 | 重庆大学 | 一种MoS2/SrFe12O19复合磁性光催化剂的制备方法 |
CN108911731A (zh) * | 2018-08-30 | 2018-11-30 | 安徽工业大学 | 一种六角晶系m型锶铁氧体粉末的制备方法 |
CN111974407A (zh) * | 2020-07-13 | 2020-11-24 | 重庆大学 | 一种制备磁性三氧化钨复合光催化剂的方法 |
Non-Patent Citations (1)
Title |
---|
"MoO3/Fe2O3微纳米材料的制备及其光催化性能";韩雪;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》(第01期);全文 * |
Also Published As
Publication number | Publication date |
---|---|
CN114950463A (zh) | 2022-08-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Ye et al. | Hydrolytic synthesis of flowerlike BiOCl and its photocatalytic performance under visible light | |
CN113663693B (zh) | 一种硫化铟锌-二氧化钛复合材料的制备方法及其在生产双氧水用于废水治理中的应用 | |
CN102010004A (zh) | 一种制备二硫化钒纳米粉体的方法 | |
CN111036243B (zh) | 含氧空缺的过渡金属掺杂的BiOBr纳米片光催化剂及其制备方法和应用 | |
WO2017219382A1 (zh) | 一种双层ZnO空心球光催化材料及其制备方法 | |
CN110280281B (zh) | 铁酸锌/黑磷微球复合物的制备方法及其在光催化领域中的应用 | |
CN106994349A (zh) | 一种分级结构的层状钙钛矿光催化剂钛酸铁铋的制备方法及用途 | |
CN102408132B (zh) | 一种微波法制备铁酸镧纳米粉体的方法 | |
Qu et al. | A new visible-light-induced Z-scheme photocatalytic system: Er3+: Y3Al5O12/(MoS2/NiGa2O4)-(BiVO4/PdS) for refractory pollutant degradation with simultaneous hydrogen evolution | |
Ji et al. | One-step synthesis of porous BiOCl microflowers with oxygen vacancies for photoreduction of CO2 under visible light irradiation | |
CN110339843B (zh) | 一种磁性氧化铋/钒酸铋复合光催化剂的制备方法 | |
CN115301225A (zh) | 一种中空微球结构的铋/二氧化钛光催化降解材料的制备方法及其应用 | |
CN114950463B (zh) | 一种新型磁性复合光催化剂MoO3/SrFe12O19的制备方法 | |
CN116351438B (zh) | 一种二氧化铈硫化铟光催化材料及其制备方法与应用 | |
CN108793267B (zh) | 一种MCo2O4纳米线的制备方法 | |
CN108686672B (zh) | 一种MnO2/Bi2O3/MnxZn1-xFe2O4复合磁性光催化剂的制备方法 | |
CN108404948B (zh) | 一种(BiO)2CO3-BiO2-x复合光催化剂及其制备方法和应用 | |
CN110586057A (zh) | 杂化改性TiO2复合光催化剂、其制备及用途 | |
Xue et al. | Construction of Cu 2+-doped CeO 2 nanocrystals hierarchical hollow structure and its enhanced photocatalytic performance | |
CN116618035A (zh) | 一种具有高光催化活性的中空不规则金红石TiO2微米球的制备方法 | |
CN104624180A (zh) | 具有可见光响应的钛基底上低维钛酸铋体系纳米材料的制备方法 | |
CN115041182B (zh) | 一种磁性三元复合光催化剂In-MoO3/SrFe12O19的制备方法 | |
CN108993554B (zh) | 三维片状纳米线的制备方法及其产品和应用 | |
CN108067277A (zh) | 高掺氮量单晶TiO2介孔材料的制备方法 | |
CN111744467A (zh) | 一种CaTiO3/CaO/TiO2复合材料的制备方法及其应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |