CN108772090A - The g-C of iron-based quantum dot modification3N4It can be seen that optical drive class fenton catalyst - Google Patents
The g-C of iron-based quantum dot modification3N4It can be seen that optical drive class fenton catalyst Download PDFInfo
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- CN108772090A CN108772090A CN201810542162.6A CN201810542162A CN108772090A CN 108772090 A CN108772090 A CN 108772090A CN 201810542162 A CN201810542162 A CN 201810542162A CN 108772090 A CN108772090 A CN 108772090A
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- iron
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- optical drive
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000003054 catalyst Substances 0.000 title claims abstract description 76
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 61
- 239000002096 quantum dot Substances 0.000 title claims abstract description 49
- 230000003287 optical effect Effects 0.000 title claims abstract description 31
- 238000012986 modification Methods 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000003344 environmental pollutant Substances 0.000 claims description 4
- 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 4
- 231100000719 pollutant Toxicity 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 239000000975 dye Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 16
- 229940012189 methyl orange Drugs 0.000 abstract description 16
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 9
- -1 Iron ion Chemical class 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000010802 sludge Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 231100000614 poison Toxicity 0.000 abstract description 2
- 230000007096 poisonous effect Effects 0.000 abstract description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 21
- 238000013019 agitation Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- RRMAPYQIZUZWHY-UHFFFAOYSA-K C(C)O.O.O.O.O.O.O.[Fe](Cl)(Cl)Cl Chemical compound C(C)O.O.O.O.O.O.O.[Fe](Cl)(Cl)Cl RRMAPYQIZUZWHY-UHFFFAOYSA-K 0.000 description 2
- 239000012028 Fenton's reagent Substances 0.000 description 2
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/345—Phenols
-
- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
-
- 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
Abstract
The present invention provides a kind of g-C of iron-based quantum dot modification3N4It can be seen that optical drive class fenton catalyst；With g-C3N4For carrier, visible optical drive class fenton catalyst material is prepared in area load iron-based quantum dot.This kind of visible optical drive class fenton catalyst preparation method is simple, and pilot process does not generate poisonous and harmful substances.Catalyst prepared by the present invention under the irradiation of hydrogen peroxide and visible light can the persistent organic pollutants such as fast degradation methyl orange, phenol and the catalyst there is good catalytic activity and stability.Iron ion number of dropouts is small (when pH is 5, number of dropouts is that 0.005ppm is far below standard limited value) after catalyst reaction, and therefore, which can solve iron containing sludge caused by the heterogeneous fenton catalyst of tradition is lost in due to iron ion and improve pure g-C3N4The problem of class fenton catalyst catalytic efficiency.
Description
Technical field
The present invention relates to catalyst fields, and in particular to a kind of g-C of iron-based quantum dot modification3N4It can be seen that optical drive class is fragrant
Pause catalyst and its preparation method and application.
Background technology
In recent years, with the high speed development of the industrial trades such as textile printing and dyeing, petrochemical industry, dyeing waste water, phenol wastewater
Water environment pollution problem is more serious caused by discharge.Phenols, the light of dye molecule, thermally and chemically property is stable and antimicrobial
Invasion, conventional biological treatment are difficult to eliminate.High-level oxidation technology (AOPs) can utilize the physics such as light, sound, electricity, magnetic and
Chemical process generates high activity intermediate hydroxyl free radical (OH), quick mineralising persistent organic pollutants, Fenton
(Fenton) oxidizing process and photocatalytic oxidation are two kinds of common high-level oxidation technologies.Conventional homogeneous Fenton reagent utilizes Fe2+
Activate H2O2Generating OH being capable of efficiently and rapidly degradation of contaminant, but Fe2+It can be quickly turned to Fe3+, in partial neutral and alkaline item
Part further aspect easily precipitates, and leads to the problem of the secondary pollution of molysite sludge, another aspect Fe3+H can be catalyzed2O2Generate O2It is (secondary
Reaction).Heterogeneous class Fenton's reaction is by iron-bearing mineral, and oxide and hydrate etc. are directly or by its nanomaterial loadings
Class Fenton oxidation is carried out on a support material handles pollutant.Heterogeneous class fenton catalyst is convenient at the end of reaction to catalysis
Agent is recycled to be detached with reaction system, to reduce because molysite generates a large amount of sludge.But general heterogeneous Fenton is urged
Agent efficiency under close neutral and alkaline condition is relatively low, and Fe under acid condition2+It is dissolved in water by reduction process, from
And the problem for bringing homogeneous Fenton reagent same.
Carbonitride (the g-C of graphite-phase3N4) be made of C widely distributed on the earth, N element, photocatalysis cheap and easy to get
Semi-conducting material.g-C3N4Energy band band gap (about 2.7eV) compares TiO2It is narrow, can electrons and holes be generated by excited by visible light.And g-
C3N4Stable in physicochemical property can be used as the electron donor in Fenton's reaction.g-C3N4It prepares reference literature and prepares Angewandte
Chemie-international Edition,2012,51(1)68-69。
Invention content
It is an object of the invention to solve, the oxidative degradation organic matter efficiency of heterogeneous fenton catalyst is low and iron ion
It is lost in and causes secondary pollution and the high defect of cost recovery, a kind of g-C of iron-based quantum dot modification is provided3N4It can be seen that optical drive class
Fenton catalyst and its preparation method and application；The Fe clusters loaded have the characteristics that unbodied, and particle size is small, required negative
Carrying capacity is few, realizes and the sunlight of cleanliness without any pollution is made full use of to promote Fenton high-level oxidation technology processing Recalcitrant chemicals, be
Advanced oxidation field provides a kind of new fenton catalyst.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention relates to a kind of g-C of iron-based quantum dot modification3N4It can be seen that optical drive class fenton catalyst, the catalyst
Including g-C3N4The iron-based quantum dot of carrier and modification in the carrier surface；The iron-based quantum dot object is mutually amorphous iron
Oxygen compound.
Preferably, the load capacity of the iron-based quantum dot in the catalyst is 0.1wt%~10wt%.
Preferably, the iron-based quantum dot is uniformly distributed in carrier surface in unformed quantum dots.
Preferably, the iron-based quantum dot particles size is less than 10nm..
The invention further relates to a kind of g-C of the iron-based quantum dot of present invention modification3N4It can be seen that optical drive class fenton catalyst
Preparation method, the preparation method comprises the following steps：
S1, soluble ferric iron salt is added in ethanol solution, stirring is allowed to be completely dissolved；
S2, graphite phase carbon nitride (g-C is added in through step S1 treated solution3N4), ultrasonic disperse；
S3, weak base reagent is added, stirring centrifuges, obtains the catalyst after washing drying, also referred to as load-type iron-based
Quantum dot modifies graphite phase carbon nitride (FeOOH/g-C3N4) catalyst.
Preferably, the soluble ferric iron salt is one or both of ferric nitrate, Iron(III) chloride hexahydrate.
Preferably, the weak base reagent is one or more of sodium bicarbonate, ammonium hydrogen carbonate, sodium carbonate.
Preferably, the soluble ferric iron salt and the molal weight of weak base ratio are 1:5~1:1, the iron oxide amount of generation
Son point is in graphite phase carbon nitride (g-C3N4) on mass fraction ranging from 0.1%-10%.
It is furthermore preferred that the support type FeOOH/g-C3N4The mass fraction of FeOOH is 0.1%~10% in catalyst.
Preferably, in step S1, the soluble ferric iron salt is 1mmol with ethanol solution proportioning：75~100ml；The second
Alcoholic solution it is a concentration of：99.7wt%.
Preferably, in step S2, the ultrasonic disperse time is 10~20min.
Preferably, in step S3, the time of the stirring is 8~12h.
The invention further relates to the g-C of the iron-based quantum dot of present invention modification3N4It can be seen that optical drive class fenton catalyst is organic
Application in wastewater treatment.
Preferably, it can be used for the dyestuff in degrading waste water and phenolic comp ' ds pollution.
The g-C of the iron-based quantum dot modification of the present invention3N4It can be seen that can to effectively improve unit dense for optical drive class fenton catalyst
The Fenton catalytic activity of iron species is spent, and plays g-C3N4Electronics is provided for Fenton's reaction promote Fe under excited by visible light3+/Fe2+
Cycle reduces iron species and is lost in and improves heterogeneous Fenton catalytic activity.Compared with prior art, the present invention has with following
Beneficial effect：
1) catalyst carrier material of the present invention is made of the C that is widely present in the earth, N element, cheap and easy to get, is adopted
With thermal polymerization, building-up process is simple, stable in physicochemical property, large specific surface area.
2) catalyst of the present invention, iron-based quantum dot are uniformly distributed in carrier surface in unformed quantum dots, tool
There is particle size small, pollutant is effectively contacted with catalyst activity component during intensified response；Required iron-based quantum dot load
Amount is few, and load capacity is adjustable (0.1%wt~10%wt).
3) catalyst of the present invention, utilizes g-C3N4With iron-based quantum dot can effectively it is compound, be conducive to charge transfer from
And improve catalyst reaction activity.
4) iron-based quantum dot is supported on g-C by the present invention3N4Carrier surface, catalyst stability is high, and can repeatedly recycle makes
With.
5) catalyst of the present invention is less than spectrophotometry lower limit with flowing molten iron vector after pollutant reaction
(0.03mg/L) is less than the standards for drinking water quality regulation (0.3mg/L) in China, contains caused by solving iron ion loss
Iron sludge problem.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the g-C of the iron-based quantum dot modification prepared3N4It can be seen that the XRD diagram of optical drive class fenton catalyst；
Fig. 2 is the g-C of the iron-based quantum dot modification prepared3N4It can be seen that the scanning electron microscope (SEM) photograph of optical drive class fenton catalyst；
Fig. 3 is the g-C of iron-based quantum dot modification prepared by embodiment 13N4It can be seen that optical drive class fenton catalyst is in visible light
Irradiation declines solution methyl orange reactivity curve graph；
The g-C of iron-based quantum dot modification prepared by Fig. 4 embodiments 13N4It can be seen that optical drive class fenton catalyst is shone in visible light
Penetrate lower mineralising phenol reactant activity curve figure；
Fig. 5 is the g-C of iron-based quantum dot modification prepared by embodiment 13N4The methyl it can be seen that optical drive class fenton catalyst is degraded
Five cycle activity figures of orange；
Fig. 6 is the g-C of iron-based quantum dot modification prepared by embodiment 13N4It can be seen that optical drive class fenton catalyst is in dark item
Part declines solution methyl orange reactivity curve graph；
Fig. 7 is the g-C of iron-based quantum dot modification prepared by embodiment 13N4Thus it is clear that optical drive class fenton catalyst TEM figure and
SAED schemes；Wherein, A schemes for TEM；B schemes for TEM；C schemes for SAED.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
Iron(III) chloride hexahydrate-ethanol solution of 5g/L is configured, 9.16ml solution is drawn in volumetric flask, it is molten that ethyl alcohol is added
Liquid is settled to 50ml, and magnetic agitation is allowed to be completely dissolved；The g-C prepared is added3N4Carbon is added in solid 3g, ultrasonic disperse 10min
Sour hydrogen ammonium powder 0.02mg, draught cupboard magnetic agitation 8h.Solid sample is separated and collected, vacuum is dry at 40 DEG C after washing filtering three times
Dry obtained support type 0.4%FeOOH/g-C3N4Catalyst (Fig. 2), by the scanning element electron microscope of Fig. 2 it is found that g-C3N4In stratiform
It stacks, there is larger surface area, occur the iron-based quantum dot disperseed on layered vector.
The usage amount of Iron(III) chloride hexahydrate-ethanol solution and ammonium hydrogen carbonate powder is become into 18.42ml, 0.02mg and
46.75ml, 0.20mg can obtain 0.9%FeOOH/g-C respectively3N4Catalyst and 2.3%FeOOH/g-C3N4Catalyst.
Fig. 1 is the 0.9%FeOOH/g-C of the iron-based quantum dot modification prepared3N4It can be seen that optical drive class fenton catalyst
XRD diagram, as shown in Figure 1, the catalyst and g-C of preparation3N4Characteristic peak it is consistent, have g-C3N4Identical crystal structure, and
There is no iron-based quantum dot characteristic diffraction peak, there is invisible nature property.
Fig. 7 is the 0.9%FeOOH/g-C of iron-based quantum dot manufactured in the present embodiment modification3N4It can be seen that optical drive class Fenton is urged
Agent TEM figures and SAED figures；As shown in Figure 7, catalyst surface iron-based quantum dot is evenly distributed in catalyst surface；SAED figures are in
Reveal extensively and the haloing of diffusion, it was demonstrated that synthesized iron-based quantum dot is impalpable structure.
Embodiment 2
In 50ml methyl orange solutions (25mg/L), it is separately added into the 0.4%FeOOH/g-C of 50mg3N4, 0.9%FeOOH/
g-C3N4, 2.3%FeOOH/g-C3N4Catalyst sample, magnetic agitation 30min make the H that 30 μ L are added after system adsorption equilibrium2O2
Solution (30wt%) is irradiated with xenon source and starts to react, and keeps temperature in about 30 DEG C in reaction process, methyl orange drops completely
It is respectively 90min, 60min, 90min (Fig. 3) to solve the time.
Embodiment 3
It is separately added into 0.4%FeOOH/g-C in 20ml phenol solutions (50mg/L)3N4, 0.9%FeOOH/g-C3N4、
2.3%FeOOH/g-C3N4After catalyst 80mg, magnetic agitation 30min, the H of 30 μ L is added2O2(30wt%), uses xenon source
It irradiates and starts to react, for reaction temperature between 30~33 DEG C, gas phase sample introduction needle collects 500 μ L gas every time in holding experimentation
Body sample injects gas chromatograph (GC-7900) and detects gas concentration lwevel.In 120min, the mineralization rate of phenol is respectively
61%, 74%, 24% (Fig. 4).
Embodiment 4
By 0.9%FeOOH/g-C obtained in embodiment 13N4Catalyst sample is placed in a concentration of 25mg/L of 50ml methyl oranges
Solution in, in holding system catalyst concn be 2g/L, be added 50 μ L hydrogen peroxide, temperature be 30~33 DEG C, use xenon
Lamp source irradiates and starts to react, and recycles five degradation methyl oranges.In five circulation experiments, catalyst imitates the degradation of methyl orange
Fruit, which is maintained in 90min, makes methyl orange decolourize completely, (Fig. 5) with good stability.
Embodiment 5
At the end of each methyl orange degradation experiment, draws reaction solution after 5ml filters machine filter and be added in 50ml volumetric flasks
10% hydroxylamine hydrochloride solution of the fresh configurations of 1ml, 5ml sodium acetate solutions adjust pH, and 2ml Phen solution is added
(0.15wt%), stands 10min, fully develops the color, and measures Fe concentration of element with Uv-vis, and Fe ions are not detected.Show to synthesize
Catalyst effectively limit the leaching problem of iron ion.
Comparative example 1
In 50ml methyl orange solutions (25mg/L), the g-C of 50mg is added3N4Catalyst sample, magnetic agitation 30min make
The H of 30 μ L is added after system adsorption equilibrium2O2Solution (30wt%) is put into light reaction equipment and starts to react.It is kept in reaction process
Temperature is irradiated with xenon source in about 30 DEG C and starts to react, the degradable methyl oranges of about 120min (Fig. 3).
Comparative example 2
In 50ml methyl orange solutions (25mg/L), the 0.5mg (0.9%FeOOH/g- with 50mg in embodiment 2 are added
C3N4Middle FeOOH's is identical in quality) FeOOH catalyst samples, 30 μ L are added after making system adsorption equilibrium in magnetic agitation 30min
H2O2Solution (30wt%) is put into light reaction equipment and starts to react.It keeps temperature in about 30 DEG C in reaction process, uses xenon lamp
Source is irradiated and starts to react, and methyl orange only degrades 3% after 120min.(Fig. 3).
Comparative example 3
It is separately added into g-C in 20ml phenol solutions (50mg/L)3N4After catalyst 80mg, magnetic agitation 30min, it is added
The H of 30 μ L2O2(30wt%) is irradiated with xenon source and starts to react, keep experimentation in reaction temperature 30~33 DEG C it
Between, gas phase sample introduction needle collects 500 μ L gaseous samples and injects gas chromatograph (GC-7900) detection gas concentration lwevel every time.?
In 120min, the mineralization rate of phenol is only 11% (Fig. 4).
Comparative example 4
In 50ml methyl orange solutions (25mg/L), the 0.9%FeOOH/g-C of 50mg is added3N4, 2.3%FeOOH/g-
C3N4Catalyst sample, magnetic agitation 30min make the H that 30 μ L are added after system adsorption equilibrium2O2Solution (30wt%), reacted
Heating water bath keeps temperature in 30 DEG C in journey, and methyl orange degradation rate is 5% (Fig. 6) after 150min.
Comparative example 5
In 50ml methyl orange solutions (25mg/L), the FeOOH catalyst samples of 0.5mg are added, magnetic agitation 30min makes
The H of 30 μ L is added after system adsorption equilibrium2O2Solution (30wt%), heating water bath keeps temperature in 30 DEG C in reaction process,
Methyl orange degradation rate is 23% (Fig. 6) after 150min.
In conclusion the g-C of the iron-based quantum dot modification of the present invention3N4It can be seen that optical drive class fenton catalyst preparation method
Simply, pilot process does not generate poisonous and harmful substances.Catalyst obtained can fast prompt drop under the irradiation of hydrogen peroxide and visible light
It solves the persistent organic pollutants such as methyl orange, phenol and the catalyst has good catalytic activity and stability.Catalyst is anti-
Iron ion number of dropouts is small (when pH is 5, number of dropouts is that 0.005ppm is far below standard limited value) after answering, and therefore, which can solve
Iron containing sludge caused by certainly traditional heterogeneous fenton catalyst is lost in due to iron ion and the pure g-C of raising3N4Class fenton catalyst
The problem of catalytic efficiency.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (10)
1. a kind of g-C of iron-based quantum dot modification3N4It can be seen that optical drive class fenton catalyst, which is characterized in that the catalyst packet
Include g-C3N4The iron-based quantum dot of carrier and modification in the carrier surface；The iron-based quantum dot object is mutually that amorphous iron aoxidizes
Close object.
2. a kind of g-C of iron-based quantum dot modification as described in claim 13N4It can be seen that the preparation of optical drive class fenton catalyst
Method, which is characterized in that the preparation method comprises the following steps：
S1, soluble ferric iron salt is added in ethanol solution, stirring is allowed to be completely dissolved；
S2, graphite phase carbon nitride, ultrasonic disperse is added in through step S1 treated solution；
S3, weak base reagent is added, stirring centrifuges, obtains the catalyst after washing drying.
3. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, the soluble ferric iron salt is one or both of ferric nitrate, Iron(III) chloride hexahydrate.
4. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, the weak base reagent is one or more of sodium bicarbonate, ammonium hydrogen carbonate, sodium carbonate.
5. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, the soluble ferric iron salt and the molal weight of weak base ratio are 1:5~1:1, the iron oxide quantum dot of generation
Mass fraction ranging from 0.1%-10% in graphite phase carbon nitride.
6. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, in step S1, the soluble ferric iron salt is 1mmol with ethanol solution proportioning：75~100ml；The ethyl alcohol is molten
A concentration of 99wt%~100wt% of liquid.
7. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, in step S2, the ultrasonic disperse time is 10~20min.
8. the g-C of iron-based quantum dot modification as claimed in claim 23N4It can be seen that the preparation method of optical drive class fenton catalyst,
It is characterized in that, in step S3, the time of the stirring is 8~12h.
9. a kind of g-C of iron-based quantum dot modification as described in claim 13N4It can be seen that optical drive class fenton catalyst or such as power
The g-C that the iron-based quantum dot that profit requires the method described in 2 to be prepared is modified3N4It can be seen that optical drive class fenton catalyst is organic
Purposes in wastewater treatment.
10. purposes as claimed in claim 9, which is characterized in that the catalyst is used for dyestuff and phenols in degrading waste water
Pollutant.
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| CN110743591A (en) * | 2019-10-21 | 2020-02-04 | 武汉理工大学 | Preparation method and application of doped composite catalyst |
| CN111375370A (en) * | 2020-01-19 | 2020-07-07 | 北京工业大学 | Fe-g-C3N4Preparation method of multifunctional nano composite material |
| CN111514917A (en) * | 2020-05-15 | 2020-08-11 | 扬州大学 | Na and Fe co-doped carbon nitride Fenton reaction catalyst and preparation method thereof |
| CN114471655A (en) * | 2022-01-14 | 2022-05-13 | 山西省生态环境保护服务中心(山西省环境规划院) | Preparation method of composite photocatalyst for efficiently generating hydrogen peroxide under visible light without adding sacrificial agent |
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| CN116651474A (en) * | 2023-06-16 | 2023-08-29 | 西北师范大学 | Preparation method of ferric hydroxide quantum dot modified BiOX photocatalytic material |
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| CN110743591A (en) * | 2019-10-21 | 2020-02-04 | 武汉理工大学 | Preparation method and application of doped composite catalyst |
| CN111375370A (en) * | 2020-01-19 | 2020-07-07 | 北京工业大学 | Fe-g-C3N4Preparation method of multifunctional nano composite material |
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| CN111514917B (en) * | 2020-05-15 | 2023-06-02 | 扬州大学 | Na and Fe co-doped carbon nitride Fenton reaction catalyst and preparation method thereof |
| CN114471655A (en) * | 2022-01-14 | 2022-05-13 | 山西省生态环境保护服务中心(山西省环境规划院) | Preparation method of composite photocatalyst for efficiently generating hydrogen peroxide under visible light without adding sacrificial agent |
| CN115318319A (en) * | 2022-07-18 | 2022-11-11 | 西安交通大学 | MoS 2 Preparation method of base heterojunction composite catalyst |
| CN115318319B (en) * | 2022-07-18 | 2023-08-22 | 西安交通大学 | MoS (MoS) 2 Preparation method of base heterojunction composite catalyst |
| CN116651474A (en) * | 2023-06-16 | 2023-08-29 | 西北师范大学 | Preparation method of ferric hydroxide quantum dot modified BiOX photocatalytic material |
| CN116651474B (en) * | 2023-06-16 | 2023-11-10 | 西北师范大学 | Preparation method of ferric hydroxide quantum dot modified BiOX photocatalytic material |
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