CN109364976A - A kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, preparation method and antibiotic biodegrading process - Google Patents
A kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, preparation method and antibiotic biodegrading process Download PDFInfo
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- CN109364976A CN109364976A CN201811405748.4A CN201811405748A CN109364976A CN 109364976 A CN109364976 A CN 109364976A CN 201811405748 A CN201811405748 A CN 201811405748A CN 109364976 A CN109364976 A CN 109364976A
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- carbon nitride
- phase carbon
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- bismuth titanates
- graphite phase
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 91
- 239000002131 composite material Substances 0.000 title claims abstract description 84
- RDQSSKKUSGYZQB-UHFFFAOYSA-N bismuthanylidyneiron Chemical compound [Fe].[Bi] RDQSSKKUSGYZQB-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 68
- 239000010439 graphite Substances 0.000 title claims abstract description 68
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 230000003115 biocidal effect Effects 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910002115 bismuth titanate Inorganic materials 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000002525 ultrasonication Methods 0.000 claims abstract description 11
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 239000013049 sediment Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910001200 Ferrotitanium Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 150000002823 nitrates Chemical class 0.000 claims description 4
- 150000004677 hydrates Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
- 229910052757 nitrogen Inorganic materials 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000004098 Tetracycline Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 229960002180 tetracycline Drugs 0.000 description 4
- 229930101283 tetracycline Natural products 0.000 description 4
- 235000019364 tetracycline Nutrition 0.000 description 4
- 150000003522 tetracyclines Chemical class 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
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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
- 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
- B01J37/343—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 ultrasonic wave energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The present invention relates to a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, preparation method and antibiotic biodegrading process, and preparation method includes the following steps: step 1: preparing iron bismuth titanates nanometer sheet；Step 2: the iron bismuth titanates nanometer sheet being put into dehydrated alcohol and is uniformly mixed, graphite phase carbon nitride is added later and carries out ultrasonication, to obtain product；Step 3: by product washing, it is dry after to get arriving iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst.The present invention prepares iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst by hydro-thermal-ULTRASONIC COMPLEX method, and preparation process is simple；Stratiform ferroelectric material iron bismuth titanates is modified with graphite phase carbon nitride to prepare heterojunction photocatalyst simultaneously, using the interface charge separation effect of heterojunction photocatalyst, so that iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of preparation has excellent photocatalytic degradation antibiotic activity under visible light.
Description
Technical field
The present invention relates to photocatalyst technology field, in particular to a kind of iron bismuth titanates-graphite phase carbon nitride complex light is urged
The biodegrading process of agent, preparation method and antibiotic.
Background technique
Photocatalysis technology presents unique potential using value in Environment control problem and in terms of solving energy crisis, special
It is not the very advantageous in terms of antibiotic in efficient degradation water body.Stratiform ferroelectric material, because its is low in cost, has redox
The features such as ability and higher photochemical stability, becomes one of the photocatalyst material being currently concerned；Wherein the most often
The stratiform ferroelectric material seen has iron bismuth titanates, because of the diversity of crystal structure and electronic structure, suitable band structure and height
Photo-generated carrier mobility, by as potential high efficiency photocatalysis agent material.But iron bismuth titanates holds because of photo-generate electron-hole
It is easily compound, cause the utilization rate to solar energy low, photocatalysis efficiency is low；In addition, the quantum efficiency of iron bismuth titanates also seriously limits
Its further application in terms of photocatalytic degradation.
People also start to find energetically and other kinds of partly lead while research is to Photocatalysts such as iron bismuth titanates
Body catalyst especially has visible light-responded catalyst.In recent years, graphite phase carbon nitride photochemical catalyst is good because having
Thermal stability, chemical stability and cheap preparation approach, and have been favored by people.But common graphite phase carbon nitride
For photochemical catalyst because the photo-generate electron-hole of graphite phase carbon nitride is easy compound, photocatalysis efficiency is also very low.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst,
The biodegrading process of preparation method and antibiotic, to overcome the deficiencies in the prior art described above.
The technical scheme to solve the above technical problems is that a kind of iron bismuth titanates-graphite phase carbon nitride complex light
The preparation method of catalyst, comprising the following steps:
Step 1: preparing iron bismuth titanates nanometer sheet；
Step 2: the iron bismuth titanates nanometer sheet being put into dehydrated alcohol and is uniformly mixed, graphite-phase nitrogen is added later
Change carbon and carry out ultrasonication, to obtain product；
Step 3: by product washing, it is dry after to get arriving iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst.
Further, the step 1 specifically:
Step 11: five nitric hydrate bismuths, nine water ferric nitrates and butyl titanate being dissolved in nitric acid solution, stirred evenly
After obtain mixture I；
Step 12: sodium hydroxide solution is added dropwise into the mixture I, obtains mixture II after mixing evenly；
Step 13: the mixture II being subjected to hydro-thermal reaction, isolates sediment after cooling；
Step 14: will obtain ferrotitanium acid bismuth nanometer sheet after sediment washing, drying.
Further, the mass ratio of the five nitric hydrates bismuth, the nine water ferric nitrate and the butyl titanate is 6:1:
2.53。
Further, the concentration of the nitric acid solution is 4mol/L, the concentration of the sodium hydroxide solution is 4mol/L；It is described
Nitric acid solution and the volume ratio of the sodium hydroxide solution are 1:1.
Further, the temperature of the hydro-thermal reaction is 180 DEG C, time 72h.
Further, the time of ultrasonication described in the step 2 is for 24 hours.
Further, the temperature when ultrasonication is 25 DEG C.
Further, iron bismuth titanates nanometer sheet described in the step 2 and the quality of the graphite phase carbon nitride are than range
5:1-20:1。
A kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, using a kind of any of the above-described iron bismuth titanates-graphite-phase
The preparation method of nitridation carbon composite photocatalyst is prepared.
Above-mentioned iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst is used for antibiosis by a kind of biodegrading process of antibiotic
The photocatalytic degradation of element.
The beneficial effects of the present invention are: the present invention prepares iron bismuth titanates-graphite-phase nitrogen by hydro-thermal-ULTRASONIC COMPLEX method
Change carbon composite photocatalyst, preparation process is simple, and raw material sources are easy to get extensively；Stratiform is modified with graphite phase carbon nitride simultaneously
Ferroelectric material iron bismuth titanates prepares heterojunction photocatalyst, using the interface charge separation effect of heterojunction photocatalyst, makes
Iron bismuth titanates-graphite phase carbon nitride the composite photo-catalyst that must be prepared has excellent photocatalytic degradation antibiotic under visible light
Activity.
Detailed description of the invention
Fig. 1 is a kind of preparation flow of the preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the present invention
Figure；
Fig. 2 is graphite phase carbon nitride, iron bismuth titanates, composite photo-catalyst -1, composite photo-catalyst -2, composite photocatalyst
The XRD spectra of agent -3 and composite photo-catalyst -4；
Fig. 3 is the SEM scanning electron microscope (SEM) photograph of composite photo-catalyst -3；
Fig. 4 is not urge using photochemical catalyst, using graphite phase carbon nitride, iron bismuth titanates, composite photo-catalyst -1, complex light
Agent -2, composite photo-catalyst -3 and composite photo-catalyst -4 are used as photochemical catalyst Degradation of Antibiotics effect picture.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
A kind of preparation method of the iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 1, including it is following
Step:
Step 1: preparing iron bismuth titanates nanometer sheet；
Step 2: the iron bismuth titanates nanometer sheet being put into dehydrated alcohol and is uniformly mixed, graphite-phase nitrogen is added later
Change carbon and carry out ultrasonication, to obtain product；
Step 3: by product washing, it is dry after to get arriving iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 2, in embodiment
On the basis of 1, the step 1 specifically:
Step 11: five nitric hydrate bismuths, nine water ferric nitrates and butyl titanate being dissolved in nitric acid solution, stirred evenly
After obtain mixture I；
Step 12: sodium hydroxide solution is added dropwise into the mixture I, obtains mixture II after mixing evenly；
Step 13: the mixture II being subjected to hydro-thermal reaction, isolates sediment after cooling；
Step 14: will obtain ferrotitanium acid bismuth nanometer sheet after sediment washing, drying.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 3, in embodiment
On the basis of 2, the mass ratio of the five nitric hydrates bismuth, the nine water ferric nitrate and the butyl titanate is 6:1:2.53.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 4, in embodiment
On the basis of 2 or 3, the concentration of the nitric acid solution is 4mol/L, and the concentration of the sodium hydroxide solution is 4mol/L；The nitre
The volume ratio of acid solution and the sodium hydroxide solution is 1:1.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 5, in embodiment
In 2 to 4 on the basis of any embodiment, the temperature of the hydro-thermal reaction is 180 DEG C, time 72h.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 6, in embodiment
In 1 to 5 on the basis of any embodiment, the time of ultrasonication described in the step 2 is for 24 hours.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 7, in embodiment
In 1 to 6 on the basis of any embodiment, the temperature when ultrasonication is 25 DEG C.
The preparation method of a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 8, in embodiment
In 1 to 7 on the basis of any embodiment, the matter of iron bismuth titanates nanometer sheet and the graphite phase carbon nitride described in the step 2
Amount is 5:1-20:1 than range.
A kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of the embodiment of the present invention 9, using a kind of any of the above-described iron
Bismuth titanates-graphite phase carbon nitride composite photo-catalyst preparation method is prepared.
The biodegrading process of a kind of antibiotic of the embodiment of the present invention 10, by above-mentioned iron bismuth titanates-graphite phase carbon nitride complex light
Catalyst is used for the photocatalytic degradation of antibiotic.
Specific embodiment 1, a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst preparation method, including it is following
Step:
Step 1: by the five nitric hydrate bismuths of 2.425g, the nine water ferric nitrates of 0.404g and the butyl titanate of 1.021g are molten
Solution obtains mixture I in 5ml, the nitric acid solution that concentration is 4mol/L after mixing evenly；Add dropwise into the mixture I
Enter 40ml, the sodium hydroxide solution that concentration is 4mol/L, obtains mixture II after mixing evenly；By the mixture II in 180
Hydro-thermal reaction 72h at a temperature of DEG C, isolates sediment after cooling；Ferrotitanium will be obtained after sediment washing, drying
Sour bismuth nanometer sheet；
Step 2: taking the iron bismuth titanates nanometer sheet of 1g to be scattered in 100ml dehydrated alcohol, 0.05g graphite-phase nitrogen is added later
Change carbon and carry out ultrasonication for 24 hours at a temperature of 25 DEG C, to obtain product；
Step 3: by product washing, it is dry after to get arriving iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst,
It is denoted as composite photo-catalyst -1.
As shown in Figure 2, the XRD base peak (JCPDS of the XRD diffraction maximum position of composite photo-catalyst -1 and iron bismuth titanates
82-0063) position is identical, shows that iron bismuth titanates object does not change mutually in composite photo-catalyst obtained；But graphite-phase is carbonized
The XRD diffraction maximum of nitrogen does not detect that the content for being primarily due to sample surfaces graphite-phase nitrogen carbide is few, the low reason of crystallinity.
Specific embodiment 2, a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst preparation method, using with tool
The identical method of body embodiment 1, is only changed to 0.10g for the dosage of wherein graphite phase carbon nitride, and iron bismuth titanates-graphite-phase nitrogen is made
Change carbon composite photocatalyst, is denoted as composite photo-catalyst -2.
As shown in Figure 2, the XRD base peak (JCPDS of the XRD diffraction maximum position of composite photo-catalyst -2 and iron bismuth titanates
82-0063) position is identical, shows that iron bismuth titanates object does not change mutually in composite photo-catalyst obtained；But graphite-phase is carbonized
The XRD diffraction maximum of nitrogen does not detect that the content for being primarily due to sample surfaces graphite-phase nitrogen carbide is few, the low reason of crystallinity.
Specific embodiment 3, a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst preparation method, using with tool
The identical method of body embodiment 1, is only changed to 0.15g for the dosage of wherein graphite phase carbon nitride, and iron bismuth titanates-graphite-phase nitrogen is made
Change carbon composite photocatalyst, is denoted as composite photo-catalyst -3.
As shown in Figure 2, the XRD base peak (JCPDS of the XRD diffraction maximum position of composite photo-catalyst -3 and iron bismuth titanates
82-0063) position is identical, shows that iron bismuth titanates object does not change mutually in composite photo-catalyst obtained；Simultaneously with graphite
Mutually be carbonized the increase of nitrogen consumption, occurs the XRD base peak with graphite phase carbon nitride in the XRD diffraction maximum of composite photo-catalyst -3
(JCPDS 87-1526) identical diffraction maximum, illustrates composite photo-catalyst -3 compared with composite photo-catalyst -1 and composite photo-catalyst -
Graphite-phase carbonization nitrogen content increases in 2.
From the figure 3, it may be seen that the bismuth titanates of iron made from embodiment 3-graphite phase carbon nitride composite photo-catalyst surface is uniform.
Specific embodiment 4, a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst preparation method, using with tool
The identical method of body embodiment 1, is only changed to 0.20g for the dosage of wherein graphite phase carbon nitride, and iron bismuth titanates-graphite-phase nitrogen is made
Change carbon composite photocatalyst, is denoted as composite photo-catalyst -4.
As shown in Figure 2, the XRD base peak (JCPDS of the XRD diffraction maximum position of composite photo-catalyst -4 and iron bismuth titanates
82-0063) position is identical, shows that iron bismuth titanates object does not change mutually in composite photo-catalyst obtained；Simultaneously with graphite
Mutually be carbonized the increase of nitrogen consumption, occurs the XRD base peak with graphite phase carbon nitride in the XRD diffraction maximum of composite photo-catalyst -4
(JCPDS 87-1526) identical diffraction maximum, illustrates composite photo-catalyst -4 compared with composite photo-catalyst -1 and composite photo-catalyst -
Graphite-phase carbonization nitrogen content increases in 2.
Iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst prepared by preparation method of the present invention is urged as light
Agent is in visible light photocatalytic degradation activity experiment:
Preparing six parts of concentration is the tetracycline of 20mg/L as the antibiotic waste water simulated, and a copy of it is as control
Group does not add any photochemical catalyst, and the iron bismuth titanates of 0.05g, graphite phase carbon nitride, complex light are separately added into other five parts
Catalyst -1, composite photo-catalyst -2, composite photo-catalyst -3 and composite photo-catalyst -4, are then stirred under the conditions of being protected from light
30min is with the photochemical catalyst in fully dispersed solution；The Single wavelength LED light visible light source for opening 420nm later, at interval of
15min draws the solution after a small amount of reaction, using the extinction for the reaction solution that ultraviolet-visible spectrophotometer measurement is drawn
Degree, and according to the concentration of tetracycline in the concentration of tetracycline-absorbance standard curve measurement solution, and then calculate tetracycline
Degradation rate；Specific experiment result is as shown in Figure 4.
As shown in Figure 4, it is urged using composite photo-catalyst -1, composite photo-catalyst -2, composite photo-catalyst -3 and complex light
Agent -4 is used as photochemical catalyst, and the degradation rate of tetracycline is respectively 61%, 63%, 88% and 70% after 60min；Compared to not adding
Add photochemical catalyst, only with iron bismuth titanates or only with graphite phase carbon nitride as photochemical catalyst for, system of the present invention
Iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst of Preparation Method preparation has excellent photocatalytic degradation antibiotic activity.
Meanwhile the mass ratio of iron bismuth titanates nanometer sheet and graphite phase carbon nitride composite photo-catalyst obtained when being 20:3
The photocatalytic degradation antibiotic activity of (i.e. composite photo-catalyst -3) is best.
The foregoing is merely a prefered embodiment of the invention, is not intended to limit the invention, all in the spirit and principles in the present invention
Within, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, it is characterised in that: including following step
It is rapid:
Step 1: preparing iron bismuth titanates nanometer sheet；
Step 2: the iron bismuth titanates nanometer sheet being put into dehydrated alcohol and is uniformly mixed, graphite phase carbon nitride is added later
And ultrasonication is carried out, to obtain product；
Step 3: by product washing, it is dry after to get arriving iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst.
2. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 1, feature
It is: the step 1 specifically:
Step 11: five nitric hydrate bismuths, nine water ferric nitrates and butyl titanate are dissolved in nitric acid solution, after mixing evenly
To mixture I；
Step 12: sodium hydroxide solution is added dropwise into the mixture I, obtains mixture II after mixing evenly；
Step 13: the mixture II being subjected to hydro-thermal reaction, isolates sediment after cooling；
Step 14: will obtain ferrotitanium acid bismuth nanometer sheet after sediment washing, drying.
3. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 2, feature
Be: the mass ratio of the five nitric hydrates bismuth, the nine water ferric nitrate and the butyl titanate is 6:1:2.53.
4. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 3, feature
Be: the concentration of the nitric acid solution is 4mol/L, and the concentration of the sodium hydroxide solution is 4mol/L；The nitric acid solution with
The volume ratio of the sodium hydroxide solution is 1:1.
5. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 4, feature
Be: the temperature of the hydro-thermal reaction is 180 DEG C, time 72h.
6. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 1, feature
Be: the time of ultrasonication described in the step 2 is for 24 hours.
7. a kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst according to claim 6, feature
Be: the temperature when ultrasonication is 25 DEG C.
8. according to claim 1 to any a kind of preparation side of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst in 7
Method, it is characterised in that: the quality of iron bismuth titanates nanometer sheet described in the step 2 and the graphite phase carbon nitride is 5 than range:
1-20:1。
9. a kind of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst, it is characterised in that: using any in claim 1 to 8
A kind of preparation method of iron bismuth titanates-graphite phase carbon nitride composite photo-catalyst is prepared.
10. a kind of biodegrading process of antibiotic, it is characterised in that: by iron bismuth titanates-graphite phase carbon nitride as claimed in claim 9
Composite photo-catalyst is used for the photocatalytic degradation of antibiotic.
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| CN110871101A (en) * | 2019-12-12 | 2020-03-10 | 肇庆学院 | Preparation and application of mesoporous carbon-bismuth titanate composite photocatalytic material |
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