CN107335461A - A kind of high exposure (001) crystal face TiO2/g‑C3N4The preparation method of composite photo-catalyst - Google Patents
A kind of high exposure (001) crystal face TiO2/g‑C3N4The preparation method of composite photo-catalyst Download PDFInfo
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- CN107335461A CN107335461A CN201710620148.9A CN201710620148A CN107335461A CN 107335461 A CN107335461 A CN 107335461A CN 201710620148 A CN201710620148 A CN 201710620148A CN 107335461 A CN107335461 A CN 107335461A
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 239000013078 crystal Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 9
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 6
- 239000011737 fluorine Substances 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 26
- 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 claims description 25
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 229910004039 HBF4 Inorganic materials 0.000 claims description 3
- 229910011006 Ti(SO4)2 Inorganic materials 0.000 claims description 3
- 229910010298 TiOSO4 Inorganic materials 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- KADRTWZQWGIUGO-UHFFFAOYSA-L oxotitanium(2+);sulfate Chemical compound [Ti+2]=O.[O-]S([O-])(=O)=O KADRTWZQWGIUGO-UHFFFAOYSA-L 0.000 claims description 3
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000001338 self-assembly Methods 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
- 230000000593 degrading effect Effects 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000009878 intermolecular interaction Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- -1 after centrifugation Substances 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000002943 spectrophotometric absorbance Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of high exposure (001) crystal face TiO2/g‑C3N4The preparation method of composite photo-catalyst, comprises the following steps：(1) by water miscible titanium source, Fluorine source, the organic compound rich in N according to mol ratio 1:(0.3~30):(0.1~10) aqueous solution is made into after mixing, and is transferred in hydrothermal reaction kettle, reacts and composite is made；(2) by above-mentioned composite after filter washing, calcined in Muffle furnace and high exposure (001) crystal face TiO is made2/g‑C3N4Composite photo-catalyst.The present invention uses hydro-thermal reaction self assembly, and a step prepares high exposure (001) crystal face TiO2/g‑C3N4Composite photo-catalyst, its preparation technology is simple, and production cost is greatly reduced, obtained TiO2/g‑C3N4Photocatalysis composite interface is more uniform；TiO2/g‑C3N4The pure g C of speed ratio of composite photo-catalyst degradable organic pollutant under visible light3N4Nearly an order of magnitude is improved, shows stronger photocatalysis performance and lower photogenerated charge combined efficiency.
Description
Technical field
The invention belongs to photocatalysis technology field, is related to a kind of high exposure (001) crystal face TiO2/g-C3N4Composite photocatalyst
The preparation method of agent.
Background technology
In numerous semiconductor light-catalyst materials, TiO2Band gap width is 3.2eV, and its chemical property is stable, nontoxic,
And the characteristic with strong absorption organic molecule and low photogenerated charge combined efficiency, it is a kind of preferable photocatalyst material.
g-C3N4As the two-dimensional material of a species graphene-structured, there is visible light absorbing, chemical stability is good, nontoxic, source is wide
The features such as general and preparation technology is simple.At present, narrow gap semiconductor and TiO2The compound of photochemical catalyst is to improve TiO2Material is can
The effective means of Jian Guang areas response, TiO2/g-C3N4Study hotspot of the composite as semiconductor light-catalyst, has taken into account g-
C3N4Visible light optical performance and TiO2The characteristic of relatively low photogenerated charge combined efficiency.
2016 Nano Energy (volume 19,446-454) report and utilize TiO2Nanotube is template, and melamine is
Synthesize g-C3N4Nitrogen source, TiO is prepared using vapour deposition process2/g-C3N4Compound, the compound features go out preferable light and urged
Change the performance of water decomposition；2016 Appl.Catal.B-Environ. (volume 187,47-58) report based on porous TiO2For mould
Plate, by melamine and porous TiO2After mixing, TiO is prepared for2/g-C3N4Compound, the compound can degrade Luo Dan well
Bright B.But above-mentioned TiO2/g-C3N4The preparation method of composite photo-catalyst is the method for fractional steps, and preparation technology is complicated, composite photocatalyst
TiO in agent2And g-C3N4Combination it is not close, and it is higher to equipment requirement, adds the cost of production.
The content of the invention
It is an object of the invention to provide a kind of high exposure (001) crystal face TiO2/g-C3N4The preparation side of composite photo-catalyst
Method, to solve, existing preparation technology is complicated, composite material interface is uneven and the technical problems such as production cost is higher.
This high exposure (001) crystal face TiO provided by the invention2/g-C3N4The preparation method of composite photo-catalyst, including
Following steps：
(1) by water miscible titanium source, Fluorine source, the organic compound rich in N according to mol ratio 1:(0.3~30):(0.1~
10) aqueous solution is made into after mixing, and is transferred in hydrothermal reaction kettle, reacts and composite is made；
(2) by above-mentioned composite after filter washing, calcined in Muffle furnace and high exposure (001) crystal face TiO is made2/
g-C3N4Composite photo-catalyst.
Water-soluble titanium salt is TiCl in the step (1)4、TiOSO4、Ti(SO4)2、TiBr4In one or more.
Fluorine source is NH in the step (1)4F、HF、C6H15N·3HF、HBF4In one or more.
The organic compound rich in N is melamine, dicyandiamide, urea, one kind in thiocarbamide or one in the step (1)
More than kind.
The aqueous solution is transferred in hydrothermal reaction kettle in the step (1), and 4~24h is heated at a temperature of 100~200 DEG C.
Preferably, the aqueous solution is transferred in hydrothermal reaction kettle in the step (1), and 6 are heated at a temperature of 150~200 DEG C
~12h.
Composite in the step (2) after filter washing, in Muffle furnace at 450 DEG C~650 DEG C calcining 1~
5h, heating rate are 10 DEG C/min.
Preferably, the composite in the step (2) after filter washing, in Muffle furnace at 500 DEG C~600 DEG C
Calcine 2~4h.
The present invention principle be：TiO is prepared by the self assembling process in hydro-thermal reaction2/g-C3N4Composite photo-catalyst.
Self assembly refers to that basic structural unit passes through intermolecular interaction, such as the effect of hydrogen bond, hydrophobic-hydrophobic, electrostatic interaction, π-π
Accumulation etc. combines a kind of technology for spontaneously forming ordered structure, due to being non-covalent bond connection, so each component is one in entirety
Determine to remain some intrinsic physics and chemical property in degree, while again because being shown influencing each other or disturbing to each other
Some overall performances.
The present invention has following advantageous effects compared with prior art：
1) present invention uses hydro-thermal reaction self assembly, and a step prepares high exposure (001) crystal face TiO2/g-C3N4Complex light
Catalyst, its preparation technology is simple, and production cost is greatly reduced, obtained TiO2/g-C3N4Photocatalysis composite interface is more
Add uniformly；
2)TiO2/g-C3N4The pure g-C of speed ratio of composite photo-catalyst degradable organic pollutant under visible light3N4Improve
Nearly an order of magnitude, show stronger photocatalysis performance and lower photogenerated charge combined efficiency.
Brief description of the drawings
Fig. 1 is high exposure (001) crystal face TiO2/g-C3N4The preparation flow figure of composite photo-catalyst.
Fig. 2 is ESEM (SEM) figure of the composite photo-catalyst of embodiment 1.
Fig. 3 is X-ray diffraction (XRD) figure of the composite photo-catalyst of embodiment 1.
Fig. 4 is the concentration-time profile of photocatalyst for degrading rhodamine B.
Embodiment
Clear, complete description will be carried out to the technical scheme in the embodiment of the present invention below, it is clear that described implementation
Example is only the part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
All other embodiment that technical staff is obtained on the premise of creative work is not made, belong to what the present invention protected
Scope.
High exposure (001) crystal face TiO in the present invention2/g-C3N4The preparation method of composite photo-catalyst, comprises the following steps：
(1) by water miscible titanium source, Fluorine source, the organic compound rich in N according to mol ratio 1:(0.3~30):(0.1~
10) aqueous solution is made into after mixing, and is transferred in hydrothermal reaction kettle, reacts and composite is made；
(2) by above-mentioned composite after filter washing, calcined in Muffle furnace and high exposure (001) crystal face TiO is made2/
g-C3N4Composite photo-catalyst.
By obtained TiO2/g-C3N4The application of composite photo-catalyst rhodamine B degradation under visible light, is concretely comprised the following steps：
20mg catalyst accurately is weighed, is added to 50mL, the 10mg/L rhdamine B aqueous solution；Before illumination, stirred under dark room conditions
60min, make to reach adsorption-desorption balance between rhodamine B and catalyst；Turn on light illumination, take out about 3 at regular intervals~
4mL solution, after centrifugation, supernatant liquor is taken, with the absorbance at ultraviolet-uisible spectrophotometer measure 553nm, calculate reaction one
The concentration of rhodamine B after fixing time.
It is the section Example of inventor in test below：
Embodiment 1
According to the flow chart shown in Fig. 1, by Ti (SO4)2, HF, melamine is according to mol ratio 1:10:It is made into after 10 mixing
The aqueous solution, and be transferred in hydrothermal reaction kettle, composite, filtration washing, in Muffle furnace is made after 12h is heated at 180 DEG C
In calcine 2h at 500 DEG C.Now, the organic compound rich in N passes through intermolecular interaction (hydrogen bond, electrostatic etc. with anion
Effect) the orderly macromolecular structure of generation.Meanwhile the stronger amino of electronegativity is inhaled by electrostatic interaction in macromolecular structure
Attached Ti4+To its surface.TiO is obtained after hydro-thermal process2-g-C3N4Presoma, then by high-temperature calcination, obtain high exposure
(001) crystal face TiO2/g-C3N4Composite photo-catalyst product.
Morphology characterization is carried out to product of the present invention using SEM, as shown in Fig. 2 TiO in catalyst2Particle and g-C3N4Lamella
It is tightly combined.Material phase analysis is carried out to product using XRD, as shown in figure 3, catalyst is by anatase TiO2And g-C3N4Composition.
By taking rhodamine B degradation as an example, 20mg catalyst is added to 50mL, in the 10mg/L rhdamine B aqueous solution.Illumination
Before, stir 60min under dark room conditions so that reach adsorption-desorption balance between rhodamine B and catalyst.Using λ>400nm
Xenon light shining, take out about 3~4mL solution at regular intervals, after centrifugation, take supernatant liquor.With UV, visible light spectrophotometric
Absorbance at meter measure 553nm, the concentration of rhodamine B after reaction certain time is calculated, as a result as shown in figure 4, after reaction 4h
Rhodamine B concentration is only 1.5% before degrading.
Comparative example 1
5g melamines are placed in the crucible with lid, and 500 DEG C are heated to 10 DEG C/min speed in Muffle furnace,
2h is incubated, room temperature is down to, obtains the g-C of yellow3N4Cake mass.
The evaluation method of catalyst photocatalytic activity determines the speed of its photocatalytic degradation rhodamine B, tied with embodiment 1
Fruit is as shown in figure 4, it is only 67.1% before degrading to react rhodamine B concentration after 4h.
Comparative example 2
Ti(SO4)2, HF is according to mol ratio 1:The aqueous solution is made into after 10 mixing, and is transferred in hydrothermal reaction kettle, at 180 DEG C
The TiO of high exposure crystal face is made after lower heating 12h2。
The evaluation method of catalyst photocatalytic activity determines the speed of its photocatalytic degradation rhodamine B, tied with embodiment 1
Fruit is as shown in figure 4, rhodamine B concentration is only for 86.6% before degrading after reaction 4h.
Comparative example 3
By existing block g-C3N4With the TiO of high exposure crystal face2It is 4 according to mass ratio:1 ground and mixed is uniform, is mixed
The block g-C of conjunction3N4With TiO2。
The evaluation method of catalyst photocatalytic activity determines the speed of its photocatalytic degradation rhodamine B, tied with embodiment 1
Fruit is as shown in figure 4, it is only 66.6% before degrading to react rhodamine B concentration after 4h.
The TiO that Fig. 4 is embodiment 1 and comparative example 1-3 is obtained2/g-C3N4RATES's figure of photocatalytic degradation rhodamine B,
As can be seen from Fig., rhodamine B concentration is 67.1% before degraded after the light-catalyzed reaction 4h of comparative example 1；The photocatalysis of comparative example 2 is anti-
Rhodamine B concentration is 86.6% before degraded after answering 4h；Before rhodamine B concentration is degraded after the light-catalyzed reaction 4h of comparative example 3
66.6%；Rhodamine B concentration is only 1.5% before degrading after the light-catalyzed reaction 4h of embodiment 1.Compared with comparative example 1-3, pass through
TiO synthesized by method provided by the invention2/g-C3N4The speed of rhodamine B degradation is obviously improved, and illustrates to close by the present invention
Into TiO2/g-C3N4Composite photo-catalyst has more excellent photocatalysis performance.
Inventor has also done following examples, as a result also illustrates TiO provided by the invention2/g-C3N4Composite photo-catalyst drops
The speed for solving rhodamine B is very fast：
Embodiment 2
By TiCl4、NH4F, urea is according to mol ratio 1:0.3:The aqueous solution is made into after 1 mixing, and is transferred to hydrothermal reaction kettle
In, composite is made after 10h is heated at 150 DEG C, filtration washing, 3h is calcined at 550 DEG C in Muffle furnace, complex light is made
Catalyst.The evaluation method of catalyst photocatalytic activity is with embodiment 1, and rhodamine B concentration is only before degrading after reacting 4h
18.5%, compared with comparative example 1-3, TiO provided by the invention2/g-C3N4The speed of rhodamine B degradation is obviously improved.
Embodiment 3
By TiOSO4、HBF4, thiocarbamide is according to mol ratio 1:30:The aqueous solution is made into after 10 mixing, and is transferred to hydrothermal reaction kettle
In, composite is made after 6h is heated at 200 DEG C, filtration washing, 2h is calcined at 600 DEG C in Muffle furnace, complex light is made
Catalyst.The evaluation method of catalyst photocatalytic activity is with embodiment 1, and rhodamine B concentration is only before degrading after reacting 4h
20.5%, compared with comparative example 1-3, TiO provided by the invention2/g-C3N4The speed of rhodamine B degradation is obviously improved.
Claims (10)
- A kind of 1. high exposure (001) crystal face TiO2/g-C3N4The preparation method of composite photo-catalyst, comprises the following steps：(1) by water miscible titanium source, Fluorine source, the organic compound rich in N according to mol ratio 1:(0.3~30):(0.1~10) mix The aqueous solution is made into after conjunction, and is transferred in hydrothermal reaction kettle, reacts and composite is made；(2) by above-mentioned composite after filter washing, calcined in Muffle furnace and high exposure (001) crystal face TiO is made2/g-C3N4 Composite photo-catalyst.
- A kind of 2. high exposure (001) crystal face TiO according to claim 12/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, water-soluble titanium source is TiCl in the step (1)4、TiOSO4、Ti(SO4)2、TiBr4In one kind or it is a kind of with On.
- A kind of 3. high exposure (001) crystal face TiO according to claim 12/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, Fluorine source is NH in the step (1)4F、HF、C6H15N·3HF、HBF4In one or more.
- A kind of 4. high exposure (001) crystal face TiO according to claim 12/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, the organic compound rich in N is one kind in melamine, dicyandiamide, urea, thiocarbamide in the step (1) Or more than one.
- A kind of 5. high exposure (001) crystal face TiO according to claim 12/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, hydrothermal reaction kettle heats 4~24h at 100~200 DEG C in the step (1).
- A kind of 6. high exposure (001) crystal face TiO according to claim 52/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, hydrothermal reaction kettle heats 6~12h at 150~200 DEG C in the step (1).
- A kind of 7. high exposure (001) crystal face TiO according to claim 12/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, composite calcines 1~4h, heating rate in Muffle furnace at 450 DEG C~650 DEG C in the step (2) For 10 DEG C/min.
- A kind of 8. high exposure (001) crystal face TiO according to claim 72/g-C3N4The preparation method of composite photo-catalyst, Characterized in that, composite calcines 2~4h in Muffle furnace at 500 DEG C~600 DEG C in the step (2).
- A kind of 9. height exposure (001) crystal face TiO according to claim any one of 1-82/g-C3N4Composite photo-catalyst TiO made from preparation method2/g-C3N4Composite photo-catalyst.
- A kind of 10. height exposure (001) crystal face TiO according to claim any one of 1-82/g-C3N4Composite photo-catalyst exists The application of rhodamine B degradation under visible ray.
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| CN111111727A (en) * | 2019-12-12 | 2020-05-08 | 西安建筑科技大学 | Ternary magnetic composite visible light catalytic nano material and preparation method and application thereof |
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| CN111111727A (en) * | 2019-12-12 | 2020-05-08 | 西安建筑科技大学 | Ternary magnetic composite visible light catalytic nano material and preparation method and application thereof |
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