CN106540676A - A kind of simple regulation and control prepare the method for different crystal forms bismuth titanium composite oxide photocatalyst and its application - Google Patents
A kind of simple regulation and control prepare the method for different crystal forms bismuth titanium composite oxide photocatalyst and its application Download PDFInfo
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- CN106540676A CN106540676A CN201610805368.4A CN201610805368A CN106540676A CN 106540676 A CN106540676 A CN 106540676A CN 201610805368 A CN201610805368 A CN 201610805368A CN 106540676 A CN106540676 A CN 106540676A
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- QAKMMQFWZJTWCW-UHFFFAOYSA-N bismuth titanium Chemical compound [Ti].[Bi] QAKMMQFWZJTWCW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 title claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 16
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims abstract description 15
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 13
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 7
- 238000001523 electrospinning Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000009987 spinning Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 238000007146 photocatalysis Methods 0.000 claims description 9
- 230000001699 photocatalysis Effects 0.000 claims description 9
- 238000002835 absorbance Methods 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 150000002576 ketones Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims description 2
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 abstract description 9
- 239000002121 nanofiber Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 description 9
- 239000010936 titanium Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 229910003080 TiO4 Inorganic materials 0.000 description 1
- 229910003083 TiO6 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- -1 hydrochloric acid Tetracycline Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
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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
- B01J23/18—Arsenic, antimony or bismuth
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Plasma & Fusion (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses method and its application that a kind of simple regulation and control prepare different crystal forms bismuth titanium composite oxide photocatalyst.Using preparation electrostatic spinning solution, composite nano fiber, by electrostatic spinning apparatus, prepared polyvinylpyrrolidone/bismuth chloride/tetrabutyl titanate precursor solution electrospinning is calcined at different temperatures under high-pressure electrostatic effect the bismuth titanium composite oxide for generating different crystal forms into polyvinylpyrrolidone/bismuth chloride/tetrabutyl titanate composite nano fiber, then.Prepared polyvinylpyrrolidone/bismuth chloride/tetrabutyl titanate composite nano fiber can regulate and control oxide crystal formation by controlling calcining heat, and the composite oxides for calcining gained effectively can be degraded under simulated solar irradiation quadracycline solution.
Description
Technical field
The present invention relates to a kind of preparation method of the bismuth titanium composite oxide photocatalyst of antibioticses treatment of Organic Wastewater
And its application.
Background technology
From nineteen forty-three, penicillin is applied to clinic, and antibiotic is developed rapidly.Nowadays, in actual production and life
Antibiotic agents are all used in work in a large number, result in the abuse of antibiotic, have in making subsoil water, surface water or soil
The residual of antibiotic.Although the concentration of residual is not high, the long-term existence of antibiotic may result in drug-resistant bacteria and antibiosis
The transmission and propagation of plain resistant gene, so as to have a strong impact on ecosystem.The problem of environmental pollution and toxicity of antibiotic is imitated at present
One of environmental problem that the whole world faces should be become.Quadracycline is a kind of broad ectrum antibiotic, other antibiotic of comparing, hydrochloric acid
Tetracycline energy long-term existence is in environment, and is difficult to degrade, thus is easier to residue in environment.Photocatalysis technology is in the sun
Under the driving of energy, can be both a kind of green with catalytic decomposition water generating hydrogen and oxygen again with each pollutant of catalytic degradation
Color, effective ways efficient, that the energy and problem of environmental pollution can be solved.TiO2Photocatalyst is that environment and field of energy chemistry are ground
The focus studied carefully：TiO2Efficiently, it is nontoxic, but its energy gap is big, quantum yield is low, it is difficult to effectively utilizes sunlight, so light is urged
It is novel semi-conductor photocatalyst of the exploitation with greater activity to change one of focus of investigation of materials.BiOCl is a kind of with height
Anisotropic layer structure quasiconductor is spent, is conducive to light induced electron to separate with hole, and there is wide spectrum response performance.Titanium
Sour bismuth compound is by Bi2O3And TiO2The composite oxides with various crystal phase structures being compounded to form, in their structure
In there is TiO6Octahedra or TiO4Tetrahedron, and connected BiOnIn polyhedron, the 6s tracks and the 2p of O of Bi
Orbital hybridization and constitute valence band so that the band gap of compound narrows, ABSORPTION EDGE red shift, and this kind of compound has relatively low band-gap energy
(2.6 eV-2.8 eV).So, bismuth titanium composite oxide catalysis material of the exploitation with more high catalytic activity is photocatalysis section
Learn a direction in research.
The content of the invention
It is an object of the invention to provide a kind of simple regulation and control prepare different crystal forms bismuth titanium composite oxide photocatalyst
Method and its application, the bismuth titanium composite oxide antibioticses of effectively degrading under simulated solar irradiation prepared with the method are organic
Pollutant, and only need to simply regulate and control calcining heat can just regulate and control crystal formation, search out optimal bismuth titanium composite oxide photocatalysis
Agent, operational approach are simple.
To realize that the purpose of the present invention is as follows using technical scheme：A kind of electrostatic spinning prepares bismuth titanium composite oxide light and urges
The preparation method of agent, it is characterised in that：
(1) weigh bismuth chloride to be dissolved in 20 mL DMFs and 5 mL acetic acid, add 2 g polyvinylpyrrolidines
Ketone, stirs to solution and clarifies, and Deca tetrabutyl titanate solution stirs 2 h, and the spinning presoma for forming homogeneous yellow transparent is molten
Liquid；
(2) precursor solution is pipetted in syringe, be put in electrospinning device, carry out spinning；
(3) fiber for being obtained is carried out into calcination processing, calcining heat is 300 oC-700 oC, finally it is cooled in atmosphere
Room temperature is obtained the bismuth titanium composite oxide of different crystal forms.
Described bismuth chloride is 1 with the mol ratio of tetrabutyl titanate:1.
Spinning condition is：Voltage is 23 kV, and plug-flow speed is 1 mL/h, receives distance for 15 cm, and ambient temperature is
35 oC。
Calcination process heating rate 2 oC/ min, 3 h of constant temperature.
Bismuth titanium composite oxide photocatalyst obtained by said method, answering in antibioticses treatment of Organic Wastewater
With.
The method of the bismuth titanium composite oxide photocatalyst treatment quadracycline solution obtained by said method, its step
For：Take the bismuth titanium composite oxide photocatalyst obtained by claim 1 to be placed in photo catalysis reactor, add quadracycline
Solution, first dark treatment 1h reach adsorption desorption balance；Then use xenon lamp（Simulated solar irradiation）Irradiation, is taken at set intervals
Sample, centrifugation determine supernatant absorbance, wherein the absorption maximum spike of quadracycline solution with ultraviolet spectrophotometer
A length of 364 nm, calculates degraded situation according to the absorbance of gained（η=C/C0=A/A0）.
Specifically, a kind of electrostatic spinning of the present invention prepares the preparation side of bismuth titanium composite oxide photocatalyst
Method, comprises the steps：Weigh bismuth chloride and be dissolved in 20 mL N, in N-dimethylformamide and 5 mL acetic acid；2 g are added to gather
Vinylpyrrolidone, stirs to solution clarification；Deca tetrabutyl titanate solution, stirs 2 H-shapeds into the spinning of homogeneous yellow transparent
Silk precursor solution.Precursor solution is taken in syringe, is put in electrospinning device, carry out spinning.By the fibre for being obtained
Dimension carries out calcination processing, and calcining heat is 300 oC-700 oC, room temperature is finally cooled in atmosphere, and different crystal forms are obtained
Bismuth titanium composite oxide.
In above-mentioned steps, described bismuth chloride and the mol ratio of tetrabutyl titanate are 1:1.
Described spinning condition is：Voltage is 23 kV, and plug-flow speed is 1 ml/h, receives distance for 15 cm, and temperature is
35 oC。
Described calcination process heating rate 2 oC/ min, 3 h of constant temperature.
Bismuth titanium composite oxide photocatalyst is used for the application for the treatment of of Organic Wastewater.
It is an advantage of the invention that：Oxide is prepared using electrostatic spinning technique, equipment is simple, and processing ease can be made in a large number
It is standby；It is controllable crystal formation by calcining heat, photocatalysis effect is reached most preferably.Material can be directly used under simulated solar irradiation
In the photocatalysis treatment of antibioticses waste water such as quadracycline.Synthesis technique is simple, has good in terms of organic wastewater
Application prospect.
Description of the drawings
Fig. 1 is schemed for the SEM of polyvinylpyrrolidone/bismuth chloride/tetrabutyl titanate composite nano fiber.
Fig. 2 is polyvinylpyrrolidone/bismuth chloride/tetrabutyl titanate composite nano fiber under different temperatures calcining
XRD schemes.
Fig. 3 is that, under simulated solar light irradiation, the bismuth titanium composite oxide photocatalyst of the present invention is degraded to quadracycline
Situation contrast curve.
Specific embodiment
Embodiment 1：Bismuth chloride (BiCl3) 20 mlN are dissolved in, in N-dimethylformamide and 5 ml acetic acid；Add 2 g
Polyvinylpyrrolidone (PVP), stirs to solution clarification；Deca tetrabutyl titanate (Ti (OiPr)4) solution, stir 2 H-shapeds
Into the spinning precursor solution of homogeneous yellow transparent.Precursor solution is taken in syringe, is put in electrospinning device, carried out
Spinning.The fiber for being obtained is carried out into calcination processing, calcining heat is 300 oC-700 oC, room temperature is finally cooled in atmosphere
The metatitanic acid bismuth composite oxide of different crystal forms is obtained.
Concretely comprise the following steps：
1st, 0.315 g bismuth chlorides are taken and is dissolved in 20 mlN, in N-dimethylformamide and 5 ml acetic acid, stirred to clarify.
2nd, under stirring, 2 g polyvinylpyrrolidones are added in above-mentioned solution, is stirred to clarify.
3rd, the 0.34 ml tetrabutyl titanate solution of Deca in above-mentioned solution, stirs 2 H-shapeds into the spinning of homogeneous yellow transparent
Precursor solution.
4th, by electrospinning device, it is 23 KV in voltage, plug-flow speed is 1 ml/h, receives distance for 15 cm, temperature
Spend for 35oUnder conditions of C, electrostatic spinning obtains PVP/BiCl3/Ti(OiPr)4Composite nano fiber.
5th, by PVP/BiCl3/Ti(OiPr)4Composite nano fiber is calcined in Muffle furnace, and heating rate is 2 oCUnder/min,
Respectively in temperature 300 oC-700 oC3 h of constant temperature.
Embodiment 2：
Under simulated solar light irradiation, the hydrochloric acid Fourth Ring respectively to 50 mg/L of the photocatalyst obtained by 1 preparation method of embodiment
Plain solution carries out photocatalysis treatment.
1st, weigh the photocatalyst obtained by 100 mg embodiments, 1 preparation method respectively to be placed in photo catalysis reactor.
2nd, 100 ml quadracycline solution are added（50 mg/L）.
3rd, before illumination, by mixed liquor under darkroom 1 h of lucifuge magnetic agitation, make system reach absorption/desorption equilibrium, take
Sample centrifugation.
4th, and then use simulated solar irradiation（Xenon lamp）Irradiation, as the excitation source of photocatalyst, samples simultaneously every 20 min
Centrifugation.
By the supernatant for being obtained, with ultraviolet spectrophotometer mensuration absorbance, (wherein the maximum of quadracycline solution is inhaled
Receive a length of 364 nm of spike), degraded situation contrast curve is drawn according to the absorbance of gained, as shown in Figure 3.
Claims (6)
1. a kind of electrostatic spinning prepares the preparation method of bismuth titanium composite oxide photocatalyst, it is characterised in that：Including following step
Suddenly：
(1) weigh bismuth chloride to be dissolved in 20 mL DMFs and 5 mL acetic acid, add 2 g polyvinylpyrrolidines
Ketone, stirs to solution and clarifies, and Deca tetrabutyl titanate solution stirs 2 h, and the spinning presoma for forming homogeneous yellow transparent is molten
Liquid；
(2) precursor solution is pipetted in syringe, be put in electrospinning device, carry out spinning；
(3) fiber for being obtained is carried out into calcination processing, calcining heat is 300 oC-700 oC, room is finally cooled in atmosphere
Temperature is obtained the bismuth titanium composite oxide of different crystal forms.
2. the preparation method of bismuth titanium composite oxide photocatalyst according to claim 1, it is characterised in that described chlorine
The mol ratio for changing bismuth with tetrabutyl titanate is 1:1.
3. the preparation method of bismuth titanium composite oxide photocatalyst according to claim 1, it is characterised in that spinning condition
For：Voltage is 23 kV, and plug-flow speed is 1 mL/h, and it is 15 cm to receive distance, and ambient temperature is 35oC。
4. the preparation method of bismuth titanium composite oxide photocatalyst according to claim 1, it is characterised in that calcination process
Heating rate 2 oC/ min, 3 h of constant temperature.
5. the bismuth titanium composite oxide photocatalyst obtained by claim 1-4, in antibioticses treatment of Organic Wastewater should
With.
6. the method for the bismuth titanium composite oxide photocatalyst treatment quadracycline solution obtained by claim 1-4, its step
Suddenly it is：Take the bismuth titanium composite oxide photocatalyst obtained by claim 1 to be placed in photo catalysis reactor, add hydrochloric acid Fourth Ring
Plain solution, first dark treatment 1h reach adsorption desorption balance；Then use xenon lamp（Simulated solar irradiation）Irradiation, is taken at set intervals
Sample, centrifugation determine supernatant absorbance, wherein the absorption maximum spike of quadracycline solution with ultraviolet spectrophotometer
A length of 364 nm, calculates degraded situation according to the absorbance of gained（η=C/C0=A/A0）.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106994349A (en) * | 2017-05-11 | 2017-08-01 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy |
| WO2020224429A1 (en) * | 2019-05-07 | 2020-11-12 | 清华大学 | Anisotropic layered inorganic fiber aerogel material and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106994349A (en) * | 2017-05-11 | 2017-08-01 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the laminated perovskite photochemical catalyst iron titanate bismuth of hierarchy |
| WO2020224429A1 (en) * | 2019-05-07 | 2020-11-12 | 清华大学 | Anisotropic layered inorganic fiber aerogel material and preparation method therefor |
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