AU2021101107A4 - A LOW-DIMENSIONAL MxOy/Bi2WO6 HETEROSTRUCTURED NANO-MATERIAL PHOTOCATALYST, A PREPARATION METHOD AND AN APPLICATION THEREOF - Google Patents
A LOW-DIMENSIONAL MxOy/Bi2WO6 HETEROSTRUCTURED NANO-MATERIAL PHOTOCATALYST, A PREPARATION METHOD AND AN APPLICATION THEREOF Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910016287 MxOy Inorganic materials 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000975 dye Substances 0.000 claims abstract description 12
- 238000001523 electrospinning Methods 0.000 claims abstract description 12
- 239000004065 semiconductor Substances 0.000 claims abstract description 10
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- 238000012546 transfer Methods 0.000 claims abstract description 5
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- 238000004043 dyeing Methods 0.000 claims abstract description 3
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- 239000002243 precursor Substances 0.000 claims description 34
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
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- 229910021641 deionized water Inorganic materials 0.000 claims description 12
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 7
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- -1 Fe2 03 Chemical compound 0.000 claims 1
- 238000001782 photodegradation Methods 0.000 abstract description 8
- 230000000593 degrading effect Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
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- 238000002474 experimental method Methods 0.000 description 13
- 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 11
- 229960000907 methylthioninium chloride Drugs 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
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- 239000000706 filtrate Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N trimethylxanthine Natural products CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 241001198704 Aurivillius Species 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004577 artificial photosynthesis Methods 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
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- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 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 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 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
- B01J23/16—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
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- B01J35/58—
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to the field of water pollution control technical, in particular to a
low-dimensional M,y/Bi2WO 6 heterostructured nano-material photocatalyst, a preparation method
and an application thereof. Disclosed in the present invention is low-dimensional heterostructured
nano-material photocatalyst, which the general formula is MOY/Bi2WO6 , and M,O is In203 , CeO 2 ,
ZnO, Fe203, CuO, W03, MoO 3 , CoO4 TiO 2 , NiO or Bi 20 3 . The low-dimensional heterostructured
nano-material photocatalyst was synthesized by combining an electrospinning technique with a
sintering process in the present invention. Low dimensional nano-material has the advantages of
large specific surface area and favorable charge transfer. Bi2WO 6 is a visible light responsive
semiconductor, which can effectively compensate for the defects of the large band gap and low
sunlight utilization rate of commercial TiO 2 . The heterojunctions effectively can promote the
separation and inhibit the recombination of photogenerated electron-hole. The photodegradation ratio
of photocatalyst in the present invention reached above 80% for degrading the organic dyes with
certain concentration under ultraviolet-visible light. The photocatalyst is specifically applicable for
controlling sewage discharge from some factories, such as chemical indicators, printing and dyeing
textiles, biological dyes, colored glass, pharmaceuticals and the like.
Description
Specification
A low-dimensional MO/Bi 2 WO 6 heterostructured nano-material photocatalyst,
a preparation method and an application thereof
Field of the invention
The present invention belongs to the field of water pollution control technical, in particular to a low-dimensional MxOy/Bi 2WO 6 heterostructured nano-material photocatalyst, a preparation method and an application thereof.
Description of related art
Chang in the rate of a chemical reaction or its initiation under the action of ultraviolet, visible, or infrared radiation in the presence of a substance-the photocatalysy-that absorbs light and is involved in the chemical transformation of the reaction partners. Photocatalytic technology convert the inexhaustible solar energy into chemical energy or electrical energy, and has great application potential in the fields of degradation of organic pollutants, reduction of heavy metal ions, photolysis of water to produce hydrogen and oxygen, artificial photosynthesis, and catalysis of organic synthesis reactions. Photocatalyst is the key to this technology. However, the photocatalysts still have some defects in terms of solar light absorption, photocatalytic efficiency, physical and chemical stability, and preparation cost. The solar photocatalytic oxidation technology with semiconductor photocatalytic materials has drawn more and more attention to scientific researchers. The purpose is to develop the photocatalyst with high solar energy utilization and catalytic activity, good stability and recyclability. The primary property related to the photocatalytic activity of a semiconductor material is the energy band structure, thereby, implementing energy band engineering is the basis for the design and construction of efficient semiconductor photocatalytic materials. The photocatalytic performance of the classic TiO 2-based semiconductor photocatalyst has been improved after structural design, but still difficult to efficiently use sunlight. In recent years, researchers have spended a large effort to find some high-performance visible-near infrared photocatalysts and expected to realize the high-efficiency conversion of solar photocatalysis by extending the light absorption range of the photocatalyst. Bi 2 WO 6 has Aurivillius layered structure with the band gap of 2.75 eV. While single Bi 2 WO 6 material has low quantum efficiency and a few active sites, and can only utilize the visible light below 450 nm, which restricts the practical application of Bi2 WO material. Constructing heterojunction interface and taking advantage of the synergistic coupling between semiconductors in energy band structure engineering can promote the separation of photogenerated carriers, cause the two-photon process and improve the photocatalytic activity significantly. Liu Hong et al. assembled Bi2 WO nanosheets with visible-near-infrared photocatalytic activity onto TiO2 nanobelts, achieved the catalysis in the range of UV-Vis-NIR broad spectrum, which provides important design ideas and material foundations for realizing solar-driven photocatalytic degradation. The nano-particle photocatalyst has the characteristics of easy agglomeration, poor dispersibility, low utilization rate, difficult recovery, and poor repeatability. While the fiber materials prepared by electrospinning are uniform dispersion, and using the polymer as template make them have good flexibility and easy operation. The materials synthesized by electrospinning generally have large specific surface area, porosity and heterojunction interface. Large specific surface area is in favor of increasing the contact area between the catalyst and the reactants, increasing the reactive sites, and pores facilitate gas transport and diffusion, all which are the key factors to improve the catalytic efficiency in the field of catalysis. Electrospinning, a simple and low-cost technology, has been developed as a universal method for preparing nano- or micro-fibers with a specified one-dimensional structure, and applied in many research fields, such as photocatalysis, lithium ion batteries, sodium ion batteries, etc. This technology, simple in process, high in yield, can continuously produce ultra-long fibers with controllable one-dimensional morphology, and is easy to form a microporous structure during the firing process, and therefore has attracted the attention of many researchers. Chinese invention patents with publication numbers CN108607498A and CN109894123A disclosed a preparation method and application of Bi 2 WO6 with enhanced adsorption performance and Preparation method and application of supported Bi2 WO 6 photocatalyst, respectively. In both of them, Bi2 WO 6 with strong adsorption were prepared by hydrothermal method and using Bi(N ) 3 3 and Na2 WO 6 as raw materials. However, the catalyst needs to have a degree of adsorption capacity to adsorb the reactants on the surface, and then charges transfer occurs on the interface during the catalytic reaction process. Too strong adsorption is not good for the catalytic reaction, because too strong adsorption is not conducive to the desorption of the products. The Bi2 WO material prepared by hydrothermal method limits its application in the field of photocatalysis. So, there is broad application prospects to develop a low-dimensional MOy/Bi 2WO6 heterostructured nano-material photocatalyst.
Summary of the invention
The technical problem to be solved by the present invention: Commercial TiO 2 has large band gap and low sunlight utilization rate. Single oxide semiconductor has high recombination rate of photogenerated electron-hole. To solve the existing technology defects, this invention provides a low-dimensional MxOy/Bi 2WO 6 heterostructured nano-material photocatalyst, a preparation method and an application thereof. The nano-material photocatalyst in the present invention is a low-dimensional heterostructured nano-material photocatalyst, and the general formula is MOy/Bi 2WO6
. M,y in the present invention is a metal oxide semiconductor, chosen from In 2 0 3 , CeO 2 , ZnO, Fe 203, CuO, W03, MoO3, Co 3 O 4 TiO2, NiO or Bi 2 0 3
. The method for preparing the low-dimensional M,y/Bi2 WO heterostructured nano-material photocatalyst mentioned above, and the specific steps are as follows: (1) Dissolve the acid and bismuth precursor in deionized water under magnetic stirring, then add HNO3 into the solution and keep on stirring. (2) Dissolve the metatungstate in deionized water. (3) Add the solution obtained in step (2) to the solution obtained in step (1) dropwise, and keep on stirring. (4) Disperse M precursor in the solution obtained in step (3), and keep on stirring. (5) Dissolve the organic Templates into absolute ethanol. (6) Transfer the solution obtained in step (4) to the solution obtained in step (5), and keep the mixed solution further stirring to form a homogeneous and transparent precursor sols. (7) Place the precursor sols in a syringe fitted with a stainless steel needle. Fix the syringe on a syringe pump and clam an electrode of a high voltage power supply to the stainless steel needle tip. (8) Set the parameters well for the electrospinning machine, and collect the gel fibers with stainless steel mesh or aluminum foil. (9) Dry the gel fibers collected in step (8). (10) Put the dried gel fiber into a muffle furnace for calcining, and get the low-dimensional M2O/Bi 2 WO 6heterostructured nano-material photocatalyst. Preferably, the acid described in step (1) is one or more of nitric acid, sulfuric acid, hydrochloric acid, acetic acid, citric acid and oxalic acid, and the Bi precursor is one or more of nitrate, sulfate, chloride, oxalate and acetate of Bi. Preferably, the M precursor described in step (4) is one or more of nitrate, sulfate, chloride, oxalate and acetate of M, and the molar ratio of M and Bi described in step (4) is 1:1. Preferably, the template described in step (5) is one or more of polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), and polyacrylonitrile (PAN). Preferably, the electrospinning parameters described in step (8) are the feed rate of the solution is 0.001 ~ 0.005 mm/s, the applied voltage is 10 ~ 30 k, and the tipto-collector distance is 10 ~ 40 cm. Preferably, the drying temperature described in step (9) is 60 ~ 100 °C, and the drying time is 8 ~ 16 h. Preferably, the calcination temperature described in step (10) is 400 ~ 700 °C, the heating rate is 1
~ 5 °C/min, and the calcination time is 1 ~ 4 h.
Benefits of the invention:
In the present invention, an electrospinning technique combined with a sintering process is used to synthesis the low-dimensional heterostructured nano-material photocatalyst. Low dimensional nano-material has the advantages of large specific surface area and favorable charge transfer. Bi 2 WO 6 is a visible light responsive semiconductor, which can effectively compensate for the defects of the large band gap and low sunlight utilization rate of commercial TiO 2. The heterojunctions effectively promote the separation and inhibit the recombination of photogenerated electron-hole. The photodegradation ratio of photocatalyst in the present invention reached above 80% for degrading the organic dyes with certain concentration under ultraviolet-visible light. The photocatalyst is specifically applicable for controlling sewage discharge from some factories, such as chemical indicators, printing and dyeing textiles, biological dyes, colored glass, pharmaceuticals and the like.
Specific implementation modalities
The present invention will be further elaborated below in conjunction with specific embodiments. It should be understood that these embodiments are merely as illustrative of the inventions and not in limitation thereof. The experimental methods without indicated specific conditions in the following embodiments usually follow the conventional conditions or the conditions suggested by the manufacturer.
Embodiment 1:
1. The preparation of photocatalyst: In a typical experiment, 2.52 g citric acid and 0.971 g Bi(N0 3)3 -5H2 0 were dissolved in 7 mL of deionized water under magnetic stirring for 15 min at room temperature, then 5 mL HNO3 was put into the solution and kept on stirring. This mixture was marked as solution 1. Meanwhile, 0.2552 g (NH4 )10 H 2 (W 2 0 7) 6 was dissolved in 15 mL deionized water, and added dropwise to the solution 1. After addition, the mixture was kept under the vigorous magnetic stirring for an additional 30 min to ensure that the reaction was complete which was marked as solution 2. Subsequently, 0.7645 g In(N0 3)3 -4.5H2 0 (1:1 in molar ratio with Bi(N0 3)3 -5H2 0) was dispersed in the solution 2. Then the clarified mixed precursor solution was obtained (labeled as precursor a). 1.0 g PVP-K90 was dissolved in 10 mL absolute ethanol (denoted as precursor b). Finally, 3.5 mL precursor a was transferred to the precursor b with a pipette and the mixed solution was further stirred for 2 h to form a homogeneous and transparent precursor sols. The precursor sols were placed in a 20 mL syringe fitted with a stainless steel needle of 0.8 mm inner diameter. The syringe was fixed horizontally on a syringe pump and an electrode of a high voltage power supply was clamped to the stainless steel needle tip. The feed rate of the solution was 0.002 mm/s, and the applied voltage was 20 k. The tipto-collector distance was set to 30 cm, and the aluminium foil was used for collecting the electrospun microbelts. The as-collected fibers were dried at 80 C for 12 h. The fibers were calcined from room temperature to 600 C at a rate of1I C/min and kept for 1 h of the soaking time, and then naturally cooled to room temperature in the furnace. The photocatalyst In 2 0 3 /Bi2 WO 6heterostructured microbelts were obtained finally. 2. The performance test of photocatalyst: MO was used as model chemicals to evaluate the activity and properties of the photocatalysts. Experiments on the photocatalytic activities were performed under the simulated sunlight source by using a 500 W Xe lamp at room temperature. In a typical experiment, 40 mL aqueous suspensions of MO and 60 mg In 2 0 3 /Bi 2 WO6 photocatalysts were put into a 50 mL beaker. Prior to irradiation, the suspensions were magnetically stirred in the dark for 30 min to establish adsorption/desorption equilibrium between the dye and the surface of the In 2 0 3 /Bi 2 WO 6photocatalysts under the room conditions. At given irradiation time intervals, the 4 mL mixed solution was sampled and centrifuged to remove the catalyst particulates for analysis. The concentration of the MO filtrates was detected with a UV-vis spectrophotometer (UV-2550). Meanwhile, the photocatalytic activity of Bi2 WO 6 microbelts synthesized via electrospnning method was tested. The final photodegradation efficiency of theIn 2 0 3/Bi 2 WO6 heterostructured microbelts reaches 82%, whereas that of pure Bi 2 WO 6 only reached 54.1 %, proving that theIn 2 0 3/Bi 2 WO6 heterostructured microbelts exhibit the enhanced photocatalytic activity.
Embodiment 2:
1. The preparation of photocatalyst: In a typical experiment, 2.52 g citric acid and 0.971 g Bi(NO3) 3 -5H2 0 were dissolved in 7 mL deionized water with magnetic stirring for 15 min at room temperature. Then 5 mL HNO 3 was added into the aforementioned solution and kept stirring for 30 min. This mixture was marked as solution 1. Meanwhile, 0.2552 g (NH14 )0 H2 (W 2O 7 )6 was dissolved in 15 mL deionized water, and then added dropwise to the solution 1. The resultant solution marked as solution 2 was kept under vigorous stirring for 30 min to ensure a thorough reaction. Subsequently, 0.869 g Ce(NO3 ) 3 (1:1 in molar ratio with Bi 3 ) was dissolved in the solution 2. As a result, the yellow transparent precursor solution was obtained. The precursor solution (3.0 mL) was transferred to the mixture obtained by dissolving 1.0 g PVP-K90 in 10 mL absolute ethanol, and the mixed solution was further stirred for 12 h to form a homogeneous and transparent precursor sols. The precursor sols were subsequently placed in a 20 mL syringe attached to a stainless steel needle with an inner diameter of 0.6 mm, and then ejected from the needle with a voltage of 20 k. The tip-to-collector distance was set to 20 cm, and aluminium foil was used to collect the electrospun fibers. The flow rate of the precursor sols was 0.002 mm/s and the humidity level was maintained around 30% RH. The as-collected nanofibers were dried at 80 C for 12 h. the electrospun nanofibers were put into an air-atmosphere programmable tube furnace for heating from room temperature to 600 C at a rate of 1 C/min and kept for a soaking time of 1 h, and then naturally cooled to room temperature in the furnace. The photocatalyst CeO 2/Bi 2 WO6 heterostructured nanofibers were obtained finally. 2. The performance test of photocatalyst: Experiments on the photocatalytic activity were performed under a simulated solar light source by using a 350W Xe lamp equipped with cutoff filters at room temperature. RhB was used as a model substance to evaluate the activity and property of the CeO2 /Bi 2 WO 6photocatalyst. The experiments were carried out in a sealed block box, and the Xe lamp was placed in a Pyrex photocatalytic reactor with a circulating water system to cool the RhB solution and prevent thermal catalytic effects. An aqueous solution of RhB (40 mL, 10 mg/L) and 60 mg of photocatalyst were put into a 50 mL beaker. Prior to irradiation, the suspensions were magnetically stirred in the dark for 30 min to establish adsorption/desorption equilibrium between the dye and the surface of the CeO 2 /Bi 2 WO6 photocatalyst under the room conditions. At given irradiation time intervals, 4 mL aliquots were taken out and centrifuged to remove the catalyst particulates for subsequent analysis. Meanwhile, the photocatalytic activity with regard to RhB and MB degradation mediated by Bi2 WO 6 and CeO 2 nanofibers synthesized via the electrospinning method was tested. The photodegradation ratio of degrading RhB reached 82.96% after irradiation for 4.5 h in the presence of the Ce 2/Bi 2 WO6 heterostructured nanofibers, whereas that of pure CeO 2 and Bi2 WO 6 nanofibers only reached 48.15% and 67.83% under the same conditions. The photodegradation ratio of degrading MB reached 83% after irradiation for 70 min in the presence of the CeO 2 /Bi 2 WO 6 heterostructured nanofibers, whereas that of pure CeO 2 and Bi2 WO6 nanofibers only reached 39.63% and 54.69% under the same conditions. Based on the above results, CeO 2 /Bi 2 WO 6heterostructured nanofibers show the superior photocatalytic activity.
Embodiment 3:
1. The preparation of photocatalyst: In a typical experiment, 2.52 g citric acid and 0.971 g Bi(NO3) 3 -5H2 0 were dissolved in 7 mL deionized water with the magnetic stirring for 15 min at room temperature, then 5 mL HNO 3 was added into the aforementioned solution and kept stirring for min. This mixture was marked as solution 1. Meanwhile, 0.2552 g (NH4)H2 (W O 2 7 )6 was
dissolved in 15 mL deionized water, and then was added dropwise to the solution 1. The resultant solution marked as solution 2 was kept under the vigorous stirring for 30 min to ensure the thorough reaction. Subsequently, 0.439 g Zn(CH3 COO) 2 (1:1 in molar ratio with Bi3 ) was dissolved in the solution 2. As a result, the transparent precursor solution was obtained. 3.0 mL precursor solution was transferred to the mixture obtained by dissolving 1.0 g PVP-K90 in 10 mL absolute ethanol and the mixed solution was further stirred for 12 h to form a homogeneous and transparent precursor sols. The precursor sols were subsequently placed in a 20 mL syringe attached to a stainless steel needle with the inner diameter of 0.8 mm, and then ejected from needle with a voltage of 20 k. The tip-tocollector distance was set to 25 cm, and the aluminum foil was used to collect the electrospun fibers. The flow rate of the precursor sols was 0.002 mm/s and the humidity level ismaintained around 30% RH. The as-collected nanofibers were dried at 80 C for 12 h. The electrospun nanofibers were put into an airatmosphere programmable tube furnace for heat treatment from room temperature to 500 C at a rate of 1 C/min and kept soaking time for 1 h, and then naturally cooled to room temperature in the furnace. The photocatalyst ZnO/Bi2 WO heterostructured submicrobelts were obtained finally. 2. The performance test of photocatalyst: Experiments on the photocatalytic activity were performed under the simulated solar light source by using a 350 W Xe lamp at room temperature. Different organic dyes aqueous solutions (Rhodamine B (RhB, 10 mg/L) and Methylene Blue (MB, mg/L)) were used as model substances to evaluate the activity and property of the ZnO/Bi2 WO photocatalyst. The experiments were carried out in a sealed block box and the Xe lampwas placed in a quartzose cold hydrazine with a circulating water system to cool down the dye solution and prevent the thermal catalytic effects. 40 ml aqueous solution of dye and 60 mg samples were put into a 50 ml beaker. Prior to irradiation, the suspensions were magnetically stirred in the dark for 0.5 h to establish the adsorption/desorption equilibrium between the dye and the surface of the ZnO/Bi 2 WO photocatalyst under the room conditions. At given irradiation time intervals, 4 mL mixed solution was sampled and centrifuged to remove the photocatalysts for analysis. Meanwhile, the photocatalytic activity of RhB and MB respectively mediated by ZnO and Bi 2 WO nanofibers synthesized via the electrospinning method were tested. The photodegradation ratio of degrading RhB reached 90.4% after irradiation for 2.5 h in the presence of the ZnO/Bi 2 WO heterostructured submicrobelts, whereas that of pure ZnO and Bi 2 WO6 nanofibers only reached 29.2% and 67.8% under the same conditions. The photodegradation ratio of degrading MB reached 91.6% after irradiation for 70 min in the presence of the ZnO/Bi2 WO heterostructured submicrobelts, whereas that of pure ZnO and Bi2 WO nanofibers only reached 50.03% and 54.69% under the same conditions. From the above results, ZnO/Bi 2 WO6 heterostructured submicrobelts possess the excellent photocatalytic activity.
Embodiment 4:
1. The preparation of photocatalyst: In a typical experiment, 2.52 g citric acid and 0.971 g Bi(N0 3)3 -5H2 0 were dissolved in 7mL deionized water with the magnetic stirring for 15 min at room temperature, then 5 mL HNO 3 was added into the aforementioned solution and kept stirring for min. This mixture was marked as solution 1. Meanwhile, 0.2552 g (NH4)H2 (W 20 7 )6 was dissolved in 15 mL deionized water, and then was added dropwise to the solution 1. The resultant solution marked as solution 2 was kept under the vigorous stirring for 30 min to ensure the thorough reaction. Subsequently, 0.8087 g Fe(N 3 )3 (1:1 in molar ratio with Bi3 ) was dissolved in the solution 2. As a result, the yellow transparent precursor solution was obtained. 3.0 mL precursor solution was transferred to the mixture obtained by dissolving 1.0 g PVP-K90 in 10 mL absolute ethanol and the mixed solution was further stirred for 2 h to form a homogeneous and transparent precursor sols. The precursor sols were subsequently placed in a 20 mL syringe attached to a stainless steel needle with the inner diameter of 0.6 mm, and then ejected from needle with a voltage of 20 k. The tip-to-collector distance was set to 20 cm, and the aluminium foil was used to collect the electrospun fibers. The flow rate of the precursor sols was 0.002 mm/s and the humidity level is maintained around 30% RH. The as-collected nanofibers were dried at 80 C for 12 h. the dried nanofibers were put into an airatmosphere programmable tube furnace for heat treatment and calcined from room temperature to 500 Cat a rate of 1 C/min and kept soaking time for 1 h, and then naturally cooled to room temperature in the furnace. The photocatalyst a-Fe 2 0 3 /Bi2 WO6 heterostructured nanofibers were obtained finally. 2. The performance test of photocatalyst: Experiments on the photocatalytic activities were performed under the simulated solar light source by using a 500 W Xe lamp equipped with cutoff filters at room temperature and the wavelength range of the visible light is 400-760 nm. Methylene blue (MB) was used as a model chemical to evaluate the activity and properties of the a-Fe 2 0 3 /Bi 2 WO6 photocatalyst. The experiments were carried out in a sealed block box and the Xe lamp was placed in a quartzose cold hydrazine with a circulating water system to cool down the MB solution and prevent thermal catalytic effects. 40 mL aqueous suspension of MB (20 mg/L) and 60 mg samples calcined at 500 C for 1 h were put into a 50 mL beaker. Prior to irradiation, the suspensions were magnetically stirred in the dark for 30 min to establish the adsorption-desorption equilibrium between the dye and the surface of the a-Fe 2 0 3/Bi 2 WO 6 photocatalyst under the room conditions. At given irradiation time intervals, 4 mL mixed solution was sampled and centrifuged to remove the catalyst particulates for analysis. The concentration of MB filtrates was detected with a UV-vis spectrophotometer (UV-2550). Meanwhile, the photocatalytic activity of Bi2 WO nanofibers synthesized via the electrospinning method was tested. The photodegradation ratio reached 82.04% after irradiation for 70 min in the presence of the a-Fe 2 03/Bi 2 WO6 heterostructured nanofibers, whereas that of pure Bi2 WO6 nanofibers only reached 54.69% under the same conditions. Therefore, a-Fe 2 0 3 /Bi 2 WO 6heterostructured nanofibers exhibit the enhanced photocatalytic activity.
Claims (1)
1. A low-dimensional M,y/Bi 2WO 6 heterostructured nano-material photocatalyst, the characteristics of which lie in that the general formula is MOy/Bi 2WO6 , and M20 is a metal oxide semiconductor, chosen from In 203, CeO2, ZnO, Fe2 03, CuO, WO 3 , MoO 3 , Co 3 O 4 TiO2, NiO or Bi2 0 3
. 2. The method for preparing a low-dimensional M,y/Bi 2WO heterostructured nano-material photocatalyst described according to claim 1, the characteristics of which lie in that the specific steps are as follows: (1) Dissolve the acid and bismuth precursor in deionized water under magnetic stirring, then add HN03 into the solution and keep on stirring. (2) Dissolve the metatungstate in deionized water. (3) Add the solution obtained in step (2) to the solution obtained in step (1) dropwise, and keep on stirring. (4) Disperse M precursor in the solution obtained in step (3), and keep on stirring. (5) Dissolve the organic Templates into absolute ethanol. (6) Transfer the solution obtained in step (4) to the solution obtained in step (5), and keep the mixed solution further stirring to form a homogeneous and transparent precursor sols. (7) Place the precursor sols in a syringe fitted with a stainless steel needle. Fix the syringe on a syringe pump and clam an electrode of a high voltage power supply to the stainless steel needle tip. (8) Set the parameters well for the electrospinning machine, and collect the gel fibers with stainless steel mesh or aluminum foil. (9) Dry the gel fibers collected in step (8). (10) Put the dried gel fiber into a muffle furnace for calcining, and get the low-dimensional M,y/Bi 2WO 6heterostructured nano-material photocatalyst. 3. The preparation method defined according to claim 2, the characteristics of which lie in that the acid described in step (1) is one or more of nitric acid, sulfuric acid, hydrochloric acid, acetic acid, citric acid and oxalic acid, and the Bi precursor is one or more of nitrate, sulfate, chloride, oxalate and acetate of Bi. 4. The preparation method defined according to claim 2, the characteristics of which lie in that the M precursor described in step (4) is one or more of nitrate, sulfate, chloride, oxalate and acetate of M, and the molar ratio of M and Bi described in step (4) is 1:1. 5. The preparation method defined according to claim 2, the characteristics of which lie in that the template described in step (5) is one or more of polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), and polyacrylonitrile (PAN). 6. The preparation method defined according to claim 2, the characteristics of which lie in that the electrospinning parameters described in step (8) are the feed rate of the solution is 0.001 ~ 0.005 mm/s, the applied voltage is 10 ~ 30 k, and the tipto-collector distance is 10 ~ 40 cm. 7. The preparation method defined according to claim 2, the characteristics of which lie in that the drying temperature described in step (9) is 60 ~ 100 °C, and the drying time is 8 ~ 16 h. 8. The preparation method defined according to claim 2, the characteristics of which lie in that the calcination temperature described in step (10) is 400 ~ 700 °C, the heating rate is 1 ~ 5 °C/min, and the calcination time is 1 ~ 4 h. 9.The application of a low-dimensional MxOy/Bi 2WO 6 heterostructured nano-material photocatalyst described according to claim 1, the characteristics of which lie in that the photocatalyst above can be applicable for controlling sewage discharge from some factories, such as chemical indicators, printing and dyeing textiles, biological dyes, colored glass, pharmaceuticals.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115228481A (en) * | 2022-07-15 | 2022-10-25 | 西北大学 | Z-shaped heterojunction SnFe 2 O 4 /Bi 2 WO 6 Composite photocatalyst, preparation method and application |
| CN115501869A (en) * | 2022-09-30 | 2022-12-23 | 齐鲁工业大学 | Heterojunction type photocatalyst and preparation method thereof |
| CN116120094A (en) * | 2023-01-03 | 2023-05-16 | 武汉理工大学 | Anti-pollution flashover ceramic insulator and preparation method thereof |
| CN116120094B (en) * | 2023-01-03 | 2024-05-03 | 武汉理工大学 | Anti-pollution flashover ceramic insulator and preparation method thereof |
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2021
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115228481A (en) * | 2022-07-15 | 2022-10-25 | 西北大学 | Z-shaped heterojunction SnFe 2 O 4 /Bi 2 WO 6 Composite photocatalyst, preparation method and application |
| CN115228481B (en) * | 2022-07-15 | 2024-04-05 | 浙江聚泰新能源材料有限公司 | Z-type heterojunction SnFe 2 O 4 /Bi 2 WO 6 Composite photocatalyst, preparation method and application |
| CN115501869A (en) * | 2022-09-30 | 2022-12-23 | 齐鲁工业大学 | Heterojunction type photocatalyst and preparation method thereof |
| CN115501869B (en) * | 2022-09-30 | 2023-10-20 | 齐鲁工业大学 | Heterojunction type photocatalyst and preparation method thereof |
| CN116120094A (en) * | 2023-01-03 | 2023-05-16 | 武汉理工大学 | Anti-pollution flashover ceramic insulator and preparation method thereof |
| CN116120094B (en) * | 2023-01-03 | 2024-05-03 | 武汉理工大学 | Anti-pollution flashover ceramic insulator and preparation method thereof |
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