CN105903486A - Z-type photocatalyst and preparation method thereof - Google Patents
Z-type photocatalyst and preparation method thereof Download PDFInfo
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- CN105903486A CN105903486A CN201610316341.9A CN201610316341A CN105903486A CN 105903486 A CN105903486 A CN 105903486A CN 201610316341 A CN201610316341 A CN 201610316341A CN 105903486 A CN105903486 A CN 105903486A
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- titanium
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 66
- 239000003054 catalyst Substances 0.000 claims description 40
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 229910052742 iron Inorganic materials 0.000 claims description 21
- 239000004408 titanium dioxide Substances 0.000 claims description 19
- -1 iron ion Chemical class 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 230000001476 alcoholic effect Effects 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 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
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910001447 ferric ion Inorganic materials 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000004887 air purification Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 11
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 10
- 230000004044 response Effects 0.000 description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004435 EPR spectroscopy Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/39—
Abstract
The invention relates to the technical field of photocatalysis, in particular to a preparation method of a photocatalyst. The preparation method comprises the following steps of mixing a titanium precursor, alcohol solvent, acid, ferric ion, and g-carbon nitride into a mixture in proportion, wherein the mass ratio of g-carbon nitride and titanium precursor is 1:(100-1000); the volume ratio of titanium precursor, alcohol solvent and acid is (5-20):(100-200):(0.3-70); the molar ratio of ferric ion and titanium precursor is (0.1-5):100; putting the mixture into a high-pressure kettle, reacting for 2-4h at the temperature of 160-240 DEG C, cooling to room temperature, and obtaining alcohol dispersing liquid of the photocatalyst; centrifuging and separating the alcohol dispersing liquid, washing, and drying, so as to obtain the photocatalyst. The prepared g-C3N4/Fe-TiP2 photocatalyst has the advantages that the good organic pollutant degrading function is realized under irradiate of visible light, and the application prospect is broad in the fields of water treatment, air purification, sterilization and disinfection.
Description
Technical field
The present invention relates to nano-photocatalyst material technical field, particularly relate to the Fe2O3 doping that g-carbonitride is compound
Titanium dioxide (g-C3N4/Fe-TiO2) and preparation method thereof.
Background technology
It is found that titanium dioxide (TiO from Fujishima and Honda in 19722) electrode glazing decomposition water
Since phenomenon (Nature, 1972,238 (5358): 37-39), Photocatalitic Technique of Semiconductor has stepped into one completely newly
Stage.In numerous photochemical catalysts, TiO2Because it is stable, nontoxic, non-secondary pollution, fast light burn into
The advantages such as photocatalytic activity is high and preparation cost is cheap, and become the photochemical catalyst being most widely used, at ring
Border improvement, DSSC, water photodissociation hydrogen manufacturing and CO2The fields such as reduction play to closing weight
The effect wanted.
TiO2Main shortcoming energy gap (anatase and brockite 3.2eV, rutile 3.0eV) mistake
It is wide so that it is be less than the ultraviolet light (only accounting for 4～5% in sunshine composition) of 385nm only with wave-length coverage,
Thus limit TiO2Large-scale application.By with other semiconductors coupling, nonmetal doping, mistake
Cross metal ion mixing, ion co-doped, and the means such as noble metal surface deposition all can effectively extend TiO2
Spectral response range is to visible region.But, traditional TiO2Base visible light catalyst, such as N doping TiO2,
The quantum efficiency still suffering from photo-generate electron-hole recombination rate height and cause is low, reducing power is low and photohole
The problems such as mobility is low.
g-C3N4It is also called graphite phase carbon nitride, there is good photocatalysis performance, it is desirable to find one
Plant and meet the advantage that material combines both.
Summary of the invention
For overcoming the deficiencies in the prior art, the present invention provides the iron that a kind of visible-light response type g-carbonitride is compound
Titania-doped (g-C3N4/Fe-TiO2) preparation method of Z-type photochemical catalyst, comprise the steps:
Titanium precursors, alcoholic solvent, acid and iron ion and g-carbonitride are mixed to form mixture in proportion；Institute
The mass ratio stating g-carbonitride and described titanium precursors is 1:100～1000；Described titanium precursors, alcoholic solvent,
The volume ratio of acid is 5～20:100～200:0.3～70；Described iron ion and described titanium precursors mol ratio are 0.
1～5:100；The concentration of described acid is 1～6mol/L.
Described mixture is inserted 160～240 DEG C of reactions 4～24h in autoclave, obtains after being cooled to room temperature
The alcohol dispersion liquid of the Fe2O3 doping titanium dioxide Z-type photochemical catalyst that g-carbonitride is compound；
The alcohol dispersion liquid of the Fe2O3 doping titanium dioxide Z-type photochemical catalyst that g-carbonitride described in centrifugation is compound,
The Fe2O3 doping titanium dioxide Z-type photochemical catalyst that described g-carbonitride is compound is obtained after washing and drying.
Wherein, the mol ratio of described iron ion and described titanium precursors is 0.2～2:100.
Wherein, during Iron source chooses ferric nitrate, iron chloride, ferric sulfate at least one.
Wherein, described titanium precursors selected from titanium tetrachloride, butyl titanate, tetraisopropyl titanate at least one.
Wherein, described alcoholic solvent selected from ethanol, normal propyl alcohol, isopropanol any one.
Wherein, described acid selected from hydrochloric acid, acetic acid, nitric acid, sulfuric acid at least one, described aqueous acid is dense
Degree is 1～6mol/L.
The present invention also provides for this Z-type photochemical catalyst, and described Z-type photochemical catalyst includes the two of iron ion doping
Titanium oxide and the g-carbonitride compound with the titanium dioxide of doping.
Wherein, described iron ion is 0.1～5:100 with the mol ratio of described titanium dioxide.
Wherein, described iron ion and described g-carbonitride mole-mass ratio is 0.0045～0.09mol:
2～10g.
Beneficial effect:
(1) present invention prepares the Fe2O3 doping titanium dioxide that visible-light response type g-carbonitride is compound
(g-C3N4/Fe-TiO2) Z-type photochemical catalyst, with TiO2Comparing, this photochemical catalyst shows higher visible
Photocatalytic activity, shows the Strong oxdiative reproducibility of this photochemical catalyst and high quantum efficiency；
(2) in the photochemical catalyst of the present invention, iron is mixed with TiO2In lattice, restrained effectively photoproduction
Hole and electronics compound, enhances the photocatalysis efficiency of photochemical catalyst；
(3) compared with traditional semiconductors coupling, a kind of non-metal semiconductive g-C that the present invention selects3N4
Material, overcomes the heavy metal pollution caused by traditional metal semiconductor, and this technique is simple simultaneously, saves
Raw material and equipment
(4) g-C that the present invention is prepared by one step hydro thermal method3N4/Fe-TiO2Z-type photochemical catalyst, gives
While TiO 2 visible light catalysis activity, also make prepared g-C3N4/Fe-TiO2Z-type photochemical catalyst exists
Good degradable organic pollutant effect under radiation of visible light, at water process, air cleaning and sterilizing etc.
Field all has broad application prospects.
Accompanying drawing explanation
Fig. 1 is the XRD of the embodiment of the present invention 1 photochemical catalyst；
Fig. 2 is the infrared spectrum of the embodiment of the present invention 1 photochemical catalyst；
Fig. 3 is electron spin resonance (ESR) figure of the embodiment of the present invention 1 photochemical catalyst；
Fig. 4 is the photocatalytic degradation benzene that control experiment 1 of the present invention, control experiment 2 and embodiment 1 obtain respectively
The efficiency comparison figure of phenol.
Fig. 5 is the transmission electron microscope picture of the embodiment of the present invention 1.
Fig. 6 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1.
Detailed description of the invention
Below, the embodiment of the present invention will be described in detail.
The present invention provides the Fe2O3 doping titanium dioxide that a kind of visible-light response type g-carbonitride is compound
(g-C3N4/Fe-TiO2) preparation method of Z-type photochemical catalyst, comprise the steps:
Step one: titanium precursors, alcoholic solvent, acid and iron ion are mixed to form mixed with g-carbonitride in proportion
Compound；Described titanium precursors, alcoholic solvent, the volume ratio of acid are 5～20:100～200:0.3～70；Described iron
Ion is 0.1～5:100 with the mol ratio of described titanium precursors.Wherein, before described g-carbonitride and described titanium
The mass ratio driving body is 1:100～1000.
Described titanium precursors can be selected from titanium tetrachloride, butyl titanate, tetraisopropyl titanate at least one；
Described alcoholic solvent selected from ethanol, normal propyl alcohol, isopropanol any one；Described acid selected from hydrochloric acid, acetic acid, nitric acid,
Sulfuric acid at least one, the concentration of described acid is 1～6mol/L.
Wherein, during Iron source chooses ferric nitrate, iron chloride, ferric sulfate at least one.Ensure iron ion
With the mol ratio of titanium precursors in the range of 0.1～5:100, preferably 0.2～2:100.
Step 2: be transferred in autoclave by described mixture, reacts 4～24h at a temperature of 160～240 DEG C.
Question response naturally cools to room temperature after terminating, it is thus achieved that the Fe2O3 doping titanium dioxide Z-type light that g-carbonitride is combined is urged
The alcohol dispersion liquid of agent.
Step 3: the alcohol of the Fe2O3 doping titanium dioxide Z-type photochemical catalyst that g-carbonitride described in centrifugation is compound
Dispersion liquid, successively uses ethanol to wash 1 time and deionized water is washed 2 times, be dried the most in an oven,
Obtain the Fe2O3 doping titanium dioxide Z-type photochemical catalyst that described g-carbonitride is compound.
Below for control experiment 1, control experiment 2, embodiment 1, embodiment 2, embodiment 3, embodiment 4
With response parameter and the properties of product analysis of embodiment 5, wherein embodiment 2 to 5 products obtained therefrom performance and reality
Execute example 1 similar.
Table 1 control experiment 1, control experiment 2 and the response parameter of embodiment 1～5
It is below product physical and chemical performance parameter and the analysis thereof of embodiment 1 acquisition:
As it is shown in figure 1, XRD spectrum understands the TiO of only Anatase in sample2Exist, 2 θ are 25.3 °,
37.8 °, 48.0 °, the peak at 54.0 ° and 62.4 ° correspond to respectively anatase (101), (004), (200),
(204) and (211) crystal face, the TiO using hydro-thermal method to prepare is described2Nano particle be photocatalysis performance relatively
Strong anatase.
Shown in Fig. 2, g-C3N4Compound Fe-TiO2Nano particle is at 1100-1650cm-1Wavelength band
Interior (1246,1321,1404,1456,1561 and 1629cm-1) there is multiple peak (Fig. 2) at place, corresponding
For C N and the characteristic peak of C=N heterocyclic compound stretching vibration；810cm-1The spy that absworption peak is triazine at place
Levy peak；3000-3300cm-1Peak in wave band is the stretching vibration characteristic peak of-NH；At 500-700cm-1Ripple
Being Ti O and Ti O Ti stretching vibration characteristic peak in segment limit, this shows in composite containing g-C3N4
And TiO2。
As it is shown on figure 3, the product of embodiment 1 occurs in that signal peak at g=1.99, at this, signal peak is three
Valency iron replaces the titanic in titanium dioxide octahedron, illustrates successfully to be doped into by hydro-thermal method ferric ion
In the lattice of titanium dioxide.
Illustrate to be prepared for Z-type g-C by simple hydro-thermal method in conjunction with above 3 width datagrams3N4/TiO2Compound
Photochemical catalyst.
Hereinafter the light degradation property test for using control experiment 1, control experiment 2 and embodiment 1 Pyrogentisinic Acid is real
Test.
Initial phenol concentration is 10mg/L, and liquor capacity is 50ml.
The product taking control experiment 1, control experiment 2 and embodiment 1 respectively as photochemical catalyst, concentration is
1g/L, the light source (wavelength is more than 420nm) with xenon lamp as light-catalyzed reaction.
First in the dark adsorb 1h before experiment, start illumination after reaching adsorption equilibrium, sample once every 10min,
Detecting phenol concentration with high performance liquid chromatograph (HPLC), result is as indicated at 4.
Shown in Figure 4, the photochemical catalyst that embodiment 1 is obtained after illumination 80min, the degraded of phenol
Rate is 100%, and its activity is better than the titania nanoparticles that do not mixes and the compound titanium dioxide of g-carbonitride
Titanium particle.
According to transmissioning electric mirror test result (Fig. 5), it is known that prepared titania nanoparticles a size of 5～10
Nm, thus there is high specific surface area, there is greater catalytic efficiency.Fig. 6 is the scanning electricity of described catalyst
Mirror figure, it is seen that granular Fe2O3 doping titanium dioxide has been compound on stratiform g-carbonitride.
The above is only the detailed description of the invention of the application, it is noted that common for the art
Technical staff, on the premise of without departing from the application principle, it is also possible to make some improvements and modifications, these
Improvements and modifications also should be regarded as the protection domain of the application.
Claims (9)
1. the preparation method of a Z-type photochemical catalyst, it is characterised in that comprise the steps:
Titanium precursors, alcoholic solvent, acid and iron ion and g-carbonitride are mixed to form mixture in proportion；Institute
The mass ratio stating g-carbonitride and described titanium precursors is 1:100～1000；Described titanium precursors, alcoholic solvent,
The volume ratio of acid is 5～20:100～200:0.3～70；Described iron ion with the mol ratio of described titanium precursors is
0.1～5:100；
Described mixture is inserted 160～240 DEG C of reactions 4～24h in autoclave, after being cooled to room temperature, obtains light
The alcohol dispersion liquid of catalyst；
The alcohol dispersion liquid of photochemical catalyst described in centrifugation, obtains described photochemical catalyst after washing and drying.
The preparation method of Z-type photochemical catalyst the most according to claim 1, it is characterised in that described iron
The mol ratio of ion and described titanium precursors is 0.2～2:100.
The preparation method of Z-type photochemical catalyst the most according to claim 1, it is characterised in that described iron
Ion source chooses at least one in ferric nitrate, iron chloride, ferric sulfate.
The preparation method of Z-type photochemical catalyst the most according to claim 1, it is characterised in that described titanium
Presoma selected from titanium tetrachloride, butyl titanate, tetraisopropyl titanate at least one.
The preparation method of Z-type photochemical catalyst the most according to claim 1, it is characterised in that described alcohol
Solvent selected from ethanol, normal propyl alcohol, isopropanol any one.
The preparation method of Z-type photochemical catalyst the most according to claim 1, it is characterised in that described acid
Selected from hydrochloric acid, acetic acid, nitric acid, sulfuric acid at least one, the concentration of described acid is 1～6mol/L.
7. a Z-type photochemical catalyst, it is characterised in that described Z-type photochemical catalyst includes iron ion doping
Titanium dioxide and the g-carbonitride compound with the titanium dioxide of doping.
Z-type photochemical catalyst the most according to claim 7, it is characterised in that described iron ion is with described
The mol ratio of titanium dioxide is 0.1～5:100.
Z-type photochemical catalyst the most according to claim 7, it is characterised in that described iron ion is with described
G-carbonitride mole-mass ratio is 0.0045～0.09mol:2～10g.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622310A (en) * | 2016-12-08 | 2017-05-10 | 济宁学院 | Preparation method of silver phosphate-titanium dioxide composite photocatalyst |
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| CN106622310A (en) * | 2016-12-08 | 2017-05-10 | 济宁学院 | Preparation method of silver phosphate-titanium dioxide composite photocatalyst |
| CN107149938A (en) * | 2017-04-21 | 2017-09-12 | 华中科技大学 | One kind is based on g nitrogen carbides and Ag3PO4Composite photo-catalyst preparation method and products thereof |
| CN107376968A (en) * | 2017-06-30 | 2017-11-24 | 湖南大学 | Tungstic acid/double Z shaped photochemical catalyst of carbonitride/bismuth oxide and its preparation method and application |
| CN107376968B (en) * | 2017-06-30 | 2019-08-16 | 湖南大学 | Tungstic acid/double Z shaped photochemical catalyst of carbonitride/bismuth oxide and its preparation method and application |
| WO2019021189A1 (en) * | 2017-07-27 | 2019-01-31 | Sabic Global Technologies B.V. | Methods of producing a nanocomposite heterojunction photocatalyst |
| CN107952464A (en) * | 2017-12-13 | 2018-04-24 | 大连理工大学 | A kind of novel photocatalysis material and double photochemical catalyst electrode automatic bias pollution control systems |
| CN107952464B (en) * | 2017-12-13 | 2020-09-11 | 大连理工大学 | Novel photocatalytic material and double-photocatalytic-electrode self-bias pollution control system |
| CN108355692A (en) * | 2018-01-22 | 2018-08-03 | 华中科技大学 | Graphite phase carbon nitride/titanic oxide nano compound material of carbon auto-dope and preparation method thereof, application |
| CN108855189A (en) * | 2018-07-05 | 2018-11-23 | 盐城工学院 | A kind of Z-type Ag6Si2O7/g-C3N4Complex light photochemical catalyst and preparation method thereof |
| CN111545185A (en) * | 2020-05-09 | 2020-08-18 | 深圳市尤佳环境科技有限公司 | Preparation method and application of photocatalyst based on ionic liquid |
| CN111545185B (en) * | 2020-05-09 | 2023-04-28 | 深圳市尤佳环境科技有限公司 | Preparation method and application of photocatalyst based on ionic liquid |
| CN115430451A (en) * | 2022-08-29 | 2022-12-06 | 湖南大学 | Iron-titanium co-doped porous graphite phase carbon nitride photo-Fenton catalyst and preparation method and application thereof |
| CN115430451B (en) * | 2022-08-29 | 2023-10-31 | 湖南大学 | Iron-titanium co-doped porous graphite phase carbon nitride photo-Fenton catalyst and preparation method and application thereof |
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