CN108554445B - A kind of visible-light response type catalyst g-C3N4/ PDI/Fe, its preparation and application - Google Patents
A kind of visible-light response type catalyst g-C3N4/ PDI/Fe, its preparation and application Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 69
- 230000004044 response Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 98
- 238000006731 degradation reaction Methods 0.000 claims abstract description 36
- 230000015556 catabolic process Effects 0.000 claims abstract description 32
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 17
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 20
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 19
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229920000877 Melamine resin Polymers 0.000 claims description 11
- 229910017135 Fe—O Inorganic materials 0.000 claims description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid group Chemical group C(C(=O)O)(=O)O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000002957 persistent organic pollutant Substances 0.000 claims description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 5
- 239000005416 organic matter Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical group C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 claims description 3
- 238000004566 IR spectroscopy Methods 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 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
- 239000007788 liquid Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 54
- 239000000463 material Substances 0.000 abstract description 16
- 239000000356 contaminant Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 7
- 231100000719 pollutant Toxicity 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 239000011941 photocatalyst Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001447 ferric ion Inorganic materials 0.000 description 2
- 230000004941 influx Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 230000005945 translocation Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0245—Nitrogen containing compounds being derivatives of carboxylic or carbonic acids
- B01J31/0247—Imides, amides or imidates (R-C=NR(OR))
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/30—Ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- 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
- 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
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to field of photocatalytic material, more particularly, to a kind of visible-light response type catalyst g-C3N4/ PDI/Fe, its preparation and application.By using the method for compound PMDA to g-C3N4It is modified, changes its band gap width and position, to increase its response range to visible light, and by changing its valence band and conduction band positions, oxygen in water can be restored and produce hydrogen peroxide.Fe is carried on catalyst, makes full use of the hydrogen peroxide building that original position efficient selective generates in photocatalytic process from Fenton-like system, is applied to contaminant degradation.The reducing agent of iron is added in system, to improve Fenton efficiency, promotes effective degradation of pollutant.
Description
Technical field
The invention belongs to field of photocatalytic material, more particularly, to a kind of visible-light response type catalyst g-C3N4/
PDI/Fe, its preparation and application.
Background technique
β-C is theoretically proposed from the Liu and Cohen of University of California in 19893N4Since covalent crystal, be carbonized nitrification
Extensive concern of the object in photocatalysis field by scientists from all over the world.1996, Teter and Hemley passed through calculating and think C3N4It can
Can have 5 kinds of structures, i.e. α phase, β phase, cubic phase, quasi- cubic phase and class graphite-phase, wherein graphite-phase C3N4It is C under room temperature3N4
In most stable of phase.Nitrogen carbide material non-toxic at the same time, have it is visible light-responded, and prepare it is simple, cheap, without golden
Belong to, is therefore widely used in photocatalysis.
But g-C3N4(graphite-phase nitrogen carbide) has some defects in itself, leads as photo-generate electron-hole recombination rate is high
The problems such as photo-quantum efficiency of cause is low, and photohole mobility is low.In addition, g-C3N4Although having good visible light-responded property
(band gap 2.7eV), but valence band is located at+1.4V (vs. Ag/AgCl, pH=6.6), and oxidability is low, it is difficult to aoxidize water, limit
Its application.
Yasuhiro Shiraishi in 2014 etc. is by by g-C3N4With PMDA is compound obtains composite photo-catalyst g-
C3N4/ PDI, changes g-C3N4Band gap width and position assign catalyst to increase its response range to visible light
Photochemical catalytic oxidation water, and reduction oxygen in water produce the ability of hydrogen peroxide.With going deep into for research, the amount of hydrogen peroxide is produced not
It is disconnected to increase, and the research in situ for utilizing hydrogen peroxide does not have been reported that also at present.On the other hand, Fenton's reaction is a kind of critically important
Depth environmental treatment technology, hydrogen peroxide are one of the most important raw materials for constituting Fenton-like system, are generated in situ using photocatalysis
Hydrogen peroxide constructs Fenton-like system, and not only all tool has very important significance in theoretical research or practical application.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of visible-light response type catalyst g-
C3N4/ PDI/Fe, its preparation and application, its object is to by using the method for compound PMDA to g-C3N4It is modified, changes
Become its band gap width and position, to increase its response range to visible light, and by changing its valence band and conduction band positions, makes
It can restore oxygen in water and produce hydrogen peroxide.Utilize g-C3N4The hydrogen peroxide that base catalyst generates in situ, Fe is loaded to and is urged
Degradation of the building from Fenton-like system, for pollutant in agent.The reducing agent of iron is added in system, to improve Fenton efficiency,
Promote effective degradation of pollutant.
To achieve the above object, according to one aspect of the present invention, a kind of visible-light response type catalyst g- is provided
C3N4/ PDI/Fe includes Fe-O key in the catalyst molecule structure, and infrared spectroscopy is in 463cm-1Position there is Fe-O
The peak of key;It passes through first by g-C3N4With the compound rear acquisition g-C of PMDA3N4/ PDI intermediate product, then by g-C3N4/ PDI is into one
Compound ferric iron is walked, iron atom is made to replace the g-C3N4Hydrogen in/PDI intermediate product forms Fe-O key.Here PDI is equal benzene
Tetramethyl pyromellitic imide.
Preferably, the band gap width of the catalyst is 2.4eV~2.8eV, can absorbing wavelength be directly 440nm's
Visible light, and the visible light of entire visible light region can be absorbed indirectly.
Other side according to the invention provides the visible-light response type catalyst g-C3N4/ PDI/Fe's
Preparation method includes the following steps:
(1) by substance A at 400 DEG C~500 DEG C, 3~5 hours are fired under inert atmosphere conditions, obtain presoma g-
C3N4;The substance A can generate the g-C of three s-triazine structures after 400 DEG C~500 DEG C polymerizations3N4;
(2) by the resulting presoma g-C of step (1)3N4With PMDA according to mass ratio 1:(1~4) mix, 300 DEG C~
400 DEG C, 3~5 hours are fired under inert atmosphere conditions, drying obtains g-C after washing3N4/PDI;
(3) g-C for obtaining step (2)3N4/ PDI is mixed with lye, stirring, and it is at lye that solid phase is obtained after separation of solid and liquid
The g-C managed3N4/PDI;The lye be sodium hydroxide solution, potassium hydroxide solution, sodium carbonate liquor or solution of potassium carbonate, it is excellent
It is selected as sodium hydroxide solution;
(4) g-C for the base extraction for obtaining step (3)3N4/ PDI and ferric salt solution, preferably FeCl3Solution is mixed
It closes, stirring, after filtering drying, obtains the visible-light response type catalyst g-C3N4/PDI/Fe。
Preferably, step (1) substance A is melamine or urea.
Preferably, step (3) lye is sodium hydroxide solution.
Preferably, Fe element and g-C in step (4) described trivalent iron salt3N4The mass ratio of/PDI is (0.4~2): 100.
Preferably, Fe element and g-C in step (4) described trivalent iron salt3N4The mass ratio of/PDI is 0.7:100.
Preferably, step (4) mixing time is 12~50h.
Preferably, step (4) mixing time is 40h.
Other side according to the invention provides visible-light response type catalyst g-C described in one kind3N4/PDI/
The degradation of organic pollutant is realized in the application of Fe applied to building from Fenton-like system.
Preferably, by the catalyst g-C when application3N4The treated waste containing organic pollutant is added in/PDI/Fe
In, reducing agent is added, adjusts pH to 2~5.
Preferably, pH to 4 is adjusted.
Preferably, the reducing agent is oxalic acid, citric acid or nitrilotriacetic acid.
Preferably, the reducing agent is nitrilotriacetic acid.
Preferably, the treated waste containing organic matter is organic wastewater, and the catalyst is in organic wastewater
Concentration is 0.5g/L~2g/L;The mass ratio of organic matter in the catalyst and the organic wastewater is 100:1;The reduction
The concentration of agent is 0.1~0.5mM.
Preferably, concentration of the catalyst in organic wastewater is 1g/L.
Preferably, the concentration of the reducing agent is 0.4mM.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
(1) the present invention provides a kind of visible-light response type catalyst g-C3N4/ PDI/Fe, by g-C3N4Basis
Upper compound PMDA and ferric ion, obtaining one kind can make full use of the system to generate by constructing from Fenton-like system
Hydrogen peroxide realizes the visible light catalyst of organic pollutant degradation.
(2) it the present invention provides the method for easy load Fe a kind of, is handled by using NaOH solution, takes sodium ion
For the hydrogen on catalyst, then will be mixed by the modified catalyst of sodium ion and ferric salt solution, make iron ion and
Exchange and in air bonding under the action of oxygen occur for sodium ion, and ferric iron is successfully finally carried on g-C3N4On/PDI,
Compared to the cost that the mode of loading such as calcining save preparation.
(3) visible-light response type catalyst g-C of the invention3N4/ PDI/Fe is applied to building and degrades from Fenton-like system
When organic pollutant, the iron being carried on catalyst is to degradation process while generating inhibition and promoting both sides effect.One side
Face competes electronics with oxygen in water on catalyst conduction band due to ferric compound, and dissolved oxygen is caused to form super oxygen certainly
The process that hydrogen peroxide is then formed by base is hindered, and influences the effect of degradation of contaminant;On the other hand, after load iron,
Catalyst for visible light influx and translocation, and the recombination rate in light induced electron and hole reduce, promote light-catalysed efficiency with
And the generation of hydrogen peroxide, facilitation effect is generated to degradation process.
(4) most of Fenton-like system degradation of contaminant is required to additionally add hydrogen peroxide at present, and the present invention is by by Fe
It is supported on g-C3N4/ PDI is upper to realize for g-C3N4The a large amount of hydrogen peroxide generated in/PDI catalyst photocatalytic process
Make full use of, build from Fenton-like system and for degradation of contaminant;But due to g-C3N4The design feature of/PDI/Fe, makes
Obtain it has inhibition and engagement each other for the generation of hydrogen peroxide simultaneously, and catalyst prepared by the present invention is applied to degradation dirt
When contaminating object, it is used as ferric reducing agent by the way that NTA (nitrilotriacetic acid) is added, by the ferric iron loaded on catalyst in visible light
Under be reduced to ferrous iron, can eliminate ferric iron to generate hydrogen peroxide inhibition, greatly promote the generation of hydrogen peroxide, thus
Can high degree promote its degradation for pollutant;
(5) reducing agent NTA (nitrilotriacetic acid) used in degradation process has very strong Biodegradable.NTA is logical
Cross bacterial action decomposition run, final product CO2And NH3.NTA in river, 2 DEG C at a temperature of, resolution ratio after two weeks
Be 82~88%, after several weeks can complete biodegradable, use will not cause secondary pollution to environment.
Detailed description of the invention
Fig. 1 is g-C3N4, g-C3N4The g-C that/PDI and embodiment 1 are modified3N4The UV-vis abosrption spectrogram of/PDI/Fe;
Fig. 2 is g-C3N4, g-C3N4The g-C that/PDI and embodiment 1 are modified3N4The band gap diagram of/PDI/Fe;
Fig. 3 is g-C3N4The g-C that/PDI and embodiment 1 are modified3N4The photoluminescence spectra figure of/PDI/Fe;
Fig. 4 is g-C3N4, g-C3N4The g-C that/PDI and embodiment 1 are modified3N4The XRD of/PDI/Fe schemes;
Fig. 5 is g-C3N4The g-C that/PDI and embodiment 1 are modified3N4The infrared spectrum of/PDI/Fe
Fig. 6 is g-C3N4The modified g-C with embodiment 13N4The 1h yields of hydrogen peroxide figure of/PDI;
Fig. 7 is g-C3N4, g-C3N4The g-C that/PDI and embodiment 1 are modified3N4/ PDI/Fe degradation of contaminant (PNP) figure is (not
Add NTA);
Fig. 8 is g-C3N4, g-C3N4The g-C that/PDI and embodiment 1 are modified3N4/ PDI/Fe degradation of contaminant (PNP) figure (is thrown
Add NTA).
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
The present invention provides a kind of visible-light response type catalyst g-C3N4/ PDI/Fe includes in the catalyst molecule structure
Fe-O key, infrared spectroscopy is in 463cm-1Position there is the peak of Fe-O key;It passes through first by g-C3N4With PMDA it is compound after
Obtain g-C3N4/ PDI intermediate product, then by g-C3N4The further compound ferric iron of/PDI makes iron atom replace the g-
C3N4Hydrogen in/PDI intermediate product forms Fe-O key.The band gap width of the catalyst is 2.4~2.8eV, can directly absorb wave
The visible light of a length of 440nm, and the visible light of entire visible light region can be absorbed indirectly.
Visible-light response type catalyst g-C3N4The preparation method of/PDI/Fe, includes the following steps:
(1) by substance A at 400 DEG C~500 DEG C, 3~5 hours are fired under inert atmosphere conditions, obtain presoma g-
C3N4;The substance A can generate the g-C of three s-triazine structures after 400 DEG C~500 DEG C polymerizations3N4;Substance A be melamine or
Urea, preferably melamine.Heating rate control is in 3~15 DEG C/min when firing melamine.Firing temperature is preferably 400
DEG C~450 DEG C, particularly preferably 425 DEG C.
(2) by the resulting presoma g-C of step (1)3N4With PMDA (pyromellitic acid anhydride) according to mass ratio 1:(1~
4) it mixes, at 300 DEG C~400 DEG C, 3~5 hours is fired under inert atmosphere conditions, drying obtains g-C after washing3N4/PDI;
Firing temperature is preferably 300 DEG C~350 DEG C, particularly preferably 325 DEG C.Heating rate is controlled in 5~15 DEG C/min.
(3) g-C for obtaining step (2)3N4/ PDI is mixed with NaOH solution, stirring, obtains processed g- after suction filtration
C3N4/PDI;
(4) g-C for obtaining step (2)3N4/ PDI is mixed with lye, stirring, and it is at lye that solid phase is obtained after separation of solid and liquid
The g-C managed3N4/PDI;The lye be sodium hydroxide solution, potassium hydroxide solution, sodium carbonate liquor or solution of potassium carbonate, it is excellent
It is selected as sodium hydroxide solution;The process of base extraction makes H in catalyst be replaced into Na.
(4) g-C for the base extraction for obtaining step (3)3N4/ PDI and ferric salt solution, preferably FeCl3Solution is mixed
It closes, stirring, after filtering drying, ferro element displacement sodium element obtains the visible-light response type catalyst g-C3N4/PDI/Fe。
Fe element and g-C3N4The mass ratio of/PDI is (0.4-2): 100, preferably 0.7:100.Mixing time is 12~50h, preferably
For 40h.
Since ferrous iron is unstable, present invention selection first loads ferric iron, and the mode that reducing agent is then added is formed from fragrant
System.But how ferric iron load to be got on, directly whether load can be be the difficult point in design process of the present invention.It is logical
A large amount of experiment discovery is crossed, by base extraction, first replaces g-C3N4Hydrogen on/PDI, is then added ferric ion, and iron is set
Hydrogen is changed, finally realizes and ferric successfully loads.
Visible-light response type catalyst g-C provided by the invention3N4/ PDI/Fe can be applied to building and realize from Fenton-like system
The degradation of organic pollutant.Because load is ferric iron on a catalyst, to promote degradation of contaminant process, added to system
Reducing agent of the NTA (nitrilotriacetic acid) as iron adds reducing agent and not only facilitates generation ferrous iron, and building is embodied from Fenton, separately
On the one hand inhibition of the ferric iron to hydrogen peroxide is generated is also eliminated, the generation of hydrogen peroxide is promoted, substantially increases pollution
Object degradation effect.In application, by the catalyst g-C3N4/ PDI/Fe is added in the treated waste containing organic pollutant, adds
Enter reducing agent, adjust pH to 2~5, preferably adjusting pH to 4.Reducing agent can commonly be gone back for Fenton-like system or Fenton-like
Former agent, such as oxalic acid, citric acid or nitrilotriacetic acid, preferably nitrilotriacetic acid.The concentration of reducing agent is 0.1~0.5mM, preferably
0.4mM.Treated waste containing organic matter is organic wastewater, and concentration of the catalyst in organic wastewater is 0.5g/L~2g/
L, preferably 1g/L;The mass ratio of organic matter in catalyst and organic wastewater is 100:1 or so.
The following are embodiments:
Embodiment 1
A kind of g-C of modification3N4The preparation method of base visible-light photocatalyst, include the following steps: the photochemical catalyst be can
Light-exposed response type g-C3N4Based photocatalyst.
(1) g-C is prepared3N4
Melamine is put into tube furnace, 5 DEG C/min of heating rate, burns 4h under 425 DEG C of condition of nitrogen gas, make melamine
High temperature polymerization forms semiconductor material g-C3N4。
(2) g-C is prepared3N4/PDI
By material obtained in (1) and PMDA according to mass ratio to be put into tube furnace after 1:2 mixed grinding, heating rate
7 DEG C/min, 4h is burnt under 325 DEG C of condition of nitrogen gas, the material after firing is washed 3 times, can be prepared by g-C after dry3N4/PDI。
(3) g-C is prepared3N4/PDI/Fe
The NaOH solution of material obtained in (2) is handled for a period of time, after suction filtration, with FeCl3With ferro element and g-
C3N4/ PDI mass ratio is that 0.7:100 is mixed in 30ml pure water, stirs 40h, obtains required modified g-C after filtering drying3N4Base
Catalyst.
Interpretation of result: g-C mentioned below is carried out to photochemical catalyst manufactured in the present embodiment3N4Refer to 1 step of embodiment
(1) obtained g-C is fired at 425 DEG C3N4;g-C3N4/ PDI refers to that 1 step of embodiment (1) fires obtained g-C at 425 DEG C3N4
The catalyst obtained through step (2);g-C3N4/ PDI/Fe refers to that 1 step of embodiment (1) fires obtained g-C at 425 DEG C3N4
The g-C of the modification obtained through step (2) (3)3N4Based photocatalyst.
(1)g-C3N4, g-C3N4The g-C that/PDI and the present embodiment are modified3N4The UV-vis spectrogram of/PDI/Fe
As shown in Figure 1, it can be seen that g-C from UV-vis spectrogram3N4G- is significantly lower than for the absorbability of visible light
C3N4/ PDI, at the same time, g-C3N4/ PDI/Fe compares g-C for the absorption of visible light3N4/ PDI is promoted there has also been certain.From
The range of visible absorption is compared, g-C3N4Absorbent wavelength is again smaller than modified g-C3N4/ PDI is absorbent
Wavelength, after load iron, absorption region broadens again, therefore modified g-C3N4/ PDI/Fe has the utilization rate of visible light
Very big promotion.
(2)g-C3N4, g-C3N4The g-C that/PDI and the present embodiment are modified3N4The band gap diagram of/PDI/Fe can from Fig. 2
Out, g-C3N4Band gap is 2.92eV, g-C3N4/ PDI band gap is 2.85eV, and modified g-C3N4/ PDI/Fe band gap is 2.83eV,
Illustrate that the present invention by the improvement to material, changes its band gap width, increases its absorption for visible light, improve and urge
Agent photo-catalysis capability.
(3)g-C3N4The g-C that/PDI and the present embodiment are modified3N4The photoluminescence spectra figure of/PDI/Fe is from luminescence generated by light light
It can be evident that in spectrogram Fig. 3, g-C3N4/ PDI luminous intensity is very high, illustrates that its electrons and holes recombination rate is very high, light
The electrons and holes really to play a role when catalysis reaction are seldom.And g-C3N4/ PDI/Fe luminous intensity is very weak, illustrates its electronics
Very low with the combined efficiency in hole, photocatalysis efficiency is very high, is more advantageous to the utilization to visible light.
(4)g-C3N4, g-C3N4The g-C that/PDI and the present embodiment are modified3N4The XRD diagram of/PDI/Fe is as shown in figure 4, in 2 θ
Peak at=27.42 is sheet g-C3N4Structure, with PDI and g-C3N4It is compound, which substantially reduces.It is right
Compare g-C3N4X-ray diffractogram, composite material forms first new peak at 2 θ=19.01, this is because PDI and g-C3N4
Forming stacking for pi-pi bond causes.Diffraction maximum at 2 θ=6.02 and 31.02 is the peak that the iron of load up is formed, this shows
Fe has successfully been loaded to g-C by loading process3N4On/PDI, to constitute from Fenton-like system.
(5)g-C3N4The g-C that/PDI and the present embodiment are modified3N4The infrared spectrum of/PDI/Fe
By to g-C3N4/ PDI and modified g-C3N4The comparative analysis of the infared spectrum of/PDI/Fe, as shown in figure 5, can
With discovery, modified g-C3N4/ PDI/Fe is in 463cm-1Position there is new peak, this position is the peak of Fe-O, illustrates to pass through
Overload process, ferric iron have been incorporated on catalyst in the form of Fe-O key, so that the photo-catalysis capability of catalyst be made to obtain
Enhancing.
(6)g-C3N4And g-C3N4/ PDI illumination 1h yields of hydrogen peroxide compares
It is g-C shown in Fig. 63N4With modified g-C3N4/ PDI produces the comparison of hydrogen peroxide, reaction system are as follows: 50mL
Deionized water is added in 250mL beaker, then weighs 0.05g catalyst, after stirring 30 minutes under dark condition, with 300W xenon lamp
Irradiation samples every half an hour and surveys concentration of hydrogen peroxide.It can be it is clear to see that g-C from figure3N4It is very low to produce amount of hydrogen peroxide,
Do not leading to when close to 0, and passing through the composite modified 1h concentration of hydrogen peroxide of catalysis later and reached 250 μm of ol/L, and reacting
It is carried out under the air conditions of gas, illustrates g-C3N4Have significantly in the amount for producing hydrogen peroxide after composite modified
It is promoted, can be used for constructing from Fenton-like system degradation of contaminant.
(7)g-C3N4, g-C3N4The g-C that/PDI and the present embodiment are modified3N4/ PDI/Fe degradation of contaminant (PNP) figure (is not thrown
Add NTA)
Shown in fig. 7 is g-C3N4, g-C3N4/ PDI and modified g-C3N4The comparison of/PDI/Fe degradation of contaminant PNP,
Reaction system are as follows: 50mL reaction solution is added in 250mL beaker, wherein including 0.05g catalyst, the PNP of 10mg/L.It is dark
Under the conditions of stir 30 minutes after, with 300W xenon lamp irradiate, sampling and measuring PNP concentration.It can be seen from the figure that not adding NTA
In the case where, compare g-C3N4, g-C3N4/ PDI and modified g-C3N4/ PDI/Fe is significantly improved for the degradation of PNP.
But due to producing promotion for catalyst after load iron and inhibiting both sides effect, on the one hand due to ferric multiple
It closes, competes electronics with oxygen in water on catalyst conduction band, cause dissolved oxygen to form superoxide radical and then form peroxide
The process for changing hydrogen is hindered, and influences the effect of degradation of contaminant;On the other hand, after load iron, catalyst is for visible light
Influx and translocation, and the recombination rate in light induced electron and hole reduce, promote the generation of light-catalysed efficiency and hydrogen peroxide,
Facilitation effect is generated to degradation process.In the case where cancelling out each other, modified g-C3N4The degradation effect that/PDI/Fe is presented is anti-
And it is not so good as g-C3N4/PDI。
(8)g-C3N4, g-C3N4The g-C that/PDI and the present embodiment are modified3N4/ PDI/Fe degradation of contaminant (PNP) figure (adds
NTA)
Shown in fig. 8 is g-C3N4, g-C3N4/ PDI and modified g-C3N4The comparison of/PDI/Fe degradation of contaminant PNP,
Reaction system are as follows: 50mL reaction solution is added in 250mL beaker, wherein include 0.05g catalyst, the PNP of 10mg/L and
The NTA of 0.4mmol/L.After being stirred 30 minutes under dark condition, irradiated with 300W xenon lamp, sampling and measuring PNP concentration.It can from figure
To find out, in the case where adding NTA, g-C3N4And g-C3N4The not big fluctuation of the degradation of/PDI for PNP, but it is modified
G-C3N4/ PDI/Fe has great promotion for the degradation of PNP, in 1 hour, reaches to the degradation of pollutant PNP
80% or so, illustrate to achieve very good effect from Fenton-like system degradation of contaminant by building, while adding NTA as Fe
Reducing agent for degradation greatly facilitate effect.
By above-mentioned analysis it is found that the g-C with visible light catalysis activity prepared by the method for the present embodiment3N4Base light is urged
Agent g-C3N4/ PDI/Fe has very strong photocatalytic activity, and can generate degradation to pollutant (PNP), while adding
After NTA is as the reducing agent of Fe, there is the promotion of high degree for the degradation of pollutant (PNP).
Embodiment 2
A kind of g-C of modification3N4The preparation method of base visible-light photocatalyst, include the following steps: the photochemical catalyst be can
Light-exposed response type g-C3N4Based photocatalyst.
(1) g-C is prepared3N4
Melamine is put into tube furnace, 10 DEG C/min of heating rate, burns 4h under 400 DEG C of condition of nitrogen gas, make melamine
Amine high temperature polymerization forms semiconductor material g-C3N4。
(2) g-C is prepared3N4/PDI
By material obtained in (1) and PMDA according to mass ratio to be put into tube furnace after 1:1 mixed grinding, heating rate
10 DEG C/min, 4h is burnt under 300 DEG C of condition of nitrogen gas, the material after firing is washed 3 times, can be prepared by g-C after dry3N4/PDI。
(3) g-C is prepared3N4/PDI/Fe
The NaOH solution of material obtained in (2) is handled for a period of time, after suction filtration, with FeCl3With ferro element and g-
C3N4/ PDI mass ratio is that 1.4:100 is mixed in 30ml pure water, and stirring for 24 hours, obtains required modified g-C after filtering drying3N4Base
Catalyst.
Embodiment 3
A kind of g-C of modification3N4The preparation method of base visible-light photocatalyst, include the following steps: the photochemical catalyst be can
Light-exposed response type g-C3N4Based photocatalyst.
(1) g-C is prepared3N4
Melamine is put into tube furnace, 5 DEG C/min of heating rate, burns 4h under 500 DEG C of condition of nitrogen gas, make melamine
High temperature polymerization forms semiconductor material g-C3N4。
(2) g-C is prepared3N4/PDI
By material obtained in (1) and PMDA according to mass ratio to be put into tube furnace after 1:3 mixed grinding, heating rate
5 DEG C/min, 4h is burnt under 300 DEG C of condition of nitrogen gas, the material after firing is washed 3 times, can be prepared by g-C after dry3N4/PDI。
(3) g-C is prepared3N4/PDI/Fe
The NaOH solution of material obtained in (2) is handled for a period of time, after suction filtration, with FeCl3With ferro element and g-
C3N4/ PDI mass ratio is that 0.4:100 is mixed in 30ml pure water, stirs 12h, obtains required modified g-C after filtering drying3N4Base
Catalyst.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of visible-light response type catalyst g-C3N4/ PDI/Fe, which is characterized in that include Fe- in the catalyst molecule structure
O key, infrared spectroscopy is in 463cm-1Position there is the peak of Fe-O key;By first by g-C3N4With the compound rear acquisition g- of PMDA
C3N4/ PDI intermediate product, then by g-C3N4The further compound ferric iron of/PDI makes iron atom replace the g-C3N4In/PDI
Between hydrogen in product form Fe-O key;
The visible-light response type catalyst g-C3N4The preparation method of/PDI/Fe, includes the following steps:
(1) by substance A at 400 DEG C~500 DEG C, 3~5 hours are fired under inert atmosphere conditions, obtain presoma g-C3N4;Institute
The g-C of three s-triazine structures can be generated after 400 DEG C~500 DEG C polymerizations by stating substance A3N4;
(2) by the resulting presoma g-C of step (1)3N4With PMDA according to mass ratio 1:(1~4) it mixes, at 300 DEG C~400 DEG C,
3~5 hours are fired under inert atmosphere conditions, drying obtains g-C after washing3N4/PDI;
(3) g-C for obtaining step (2)3N4/ PDI is mixed with lye, stirring, and it is base extraction mistake that solid phase is obtained after separation of solid and liquid
G-C3N4/PDI;The lye is sodium hydroxide solution, potassium hydroxide solution, sodium carbonate liquor or solution of potassium carbonate;
(4) g-C for the base extraction for obtaining step (3)3N4/ PDI is mixed with ferric salt solution, stirring, after filtering drying,
Obtain the visible-light response type catalyst g-C3N4/PDI/Fe。
2. visible-light response type catalyst g-C as described in claim 13N4/ PDI/Fe, which is characterized in that the catalyst
Band gap width is 2.4eV~2.8eV, directly absorbing wavelength can be the visible light of 440nm, and can be absorbed indirectly entire visible
The visible light in light region.
3. visible-light response type catalyst g-C as described in claim 13N4/ PDI/Fe, which is characterized in that step (1) is described
Substance A is melamine or urea.
4. visible-light response type catalyst g-C as described in claim 13N4/ PDI/Fe, which is characterized in that step (4) is described
Ferric salt solution is FeCl3Solution.
5. visible-light response type catalyst g-C as described in claim 13N4/ PDI/Fe, which is characterized in that step (4) is described
Fe element and g-C in trivalent iron salt3N4The mass ratio of/PDI is (0.4~2): 100.
6. visible-light response type catalyst g-C as described in claim 13N4/ PDI/Fe, which is characterized in that step (4) is described
Mixing time is 12~50h.
7. a kind of such as visible-light response type catalyst g-C as claimed in any one of claims 1 to 63N4The application of/PDI/Fe, it is special
Sign is, realizes the degradation of organic pollutant from Fenton-like system applied to building.
8. the use as claimed in claim 7, which is characterized in that by the catalyst g-C3N4/ PDI/Fe, which is added, contains organic dirt
In the treated waste for contaminating object, reducing agent is added, adjusts pH to 2~5.
9. application as claimed in claim 8, which is characterized in that the reducing agent is oxalic acid, citric acid or nitrilotriacetic acid.
10. application as claimed in claim 8, which is characterized in that the treated waste containing organic matter is organic wastewater,
Concentration of the catalyst in organic wastewater is 0.5g/L~2g/L;The concentration of the reducing agent is 0.1~0.5mM.
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