CN106076392A - A kind of titanium dioxide/g C3n4the preparation method of quantum dot composite catalyst - Google Patents
A kind of titanium dioxide/g C3n4the preparation method of quantum dot composite catalyst Download PDFInfo
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- CN106076392A CN106076392A CN201610449256.XA CN201610449256A CN106076392A CN 106076392 A CN106076392 A CN 106076392A CN 201610449256 A CN201610449256 A CN 201610449256A CN 106076392 A CN106076392 A CN 106076392A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002096 quantum dot Substances 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 title claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 title claims description 17
- 238000002360 preparation method Methods 0.000 title claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000011218 binary composite Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 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 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing 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
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention provides one to utilize sol-gal process to prepare titania nanoparticles and g C3N4The method of quantum dot binary composite catalyst.The present invention uses sol-gal process first to prepare anatase titanium dioxide nano-particle, then by g C3N4Quantum dot joins in titania nanoparticles, utilizes ultrasonic and heating in water bath stirring, makes the two mix, obtain the heterojunction composite with excellent photocatalysis performance.This composite, compared to existing titanic oxide material, has the photocatalysis performance of excellence, has good application prospect in photocatalysis treatment organic pollution field.
Description
Technical field
The present invention relates to a kind of titanium dioxide/g-C3N4The preparation method of quantum dot composite catalyst, particularly belongs to photocatalysis multiple
Condensation material preparing technical field.
Background technology
The photocatalytic activity of titanium dioxide is limited by its energy gap, and (energy gap of Rutile Type is 3.0eV, and sharp
The energy gap of titanium ore phase is 3.2eV), can only be excited by the wavelength ultraviolet light less than below 380nm.On the other hand, when
When TiO2 photocatalyst is by solar radiation, the electron-hole pair of generation is excited to move to the most rapidly surface by sunlight,
It is combined rapidly in inside on the contrary, becomes another factor limiting its photocatalytic activity.Therefore, synthesis has narrower carrying
Width can also suppress the compound TiO2 photocatalyst of photo-generate electron-hole to be a challenging difficult problem simultaneously.Existing
, there are many means to realize this idea, such as incorporation noble metal in titanium dioxide, metal-oxide,
(Jin Chunji, the preparation of titanium dioxide/graphene composite material and the research of photocatalysis performance, the Jilin such as c-based nanomaterial
University, Materials Physics and Chemistry, 2014, Master's thesis), obtain people by synthesizing a series of composite titania materials
Desired photocatalyst.There now have been a series of about titanium dioxide/nitridation carbon composite to improve its photocatalysis
Report (Cui Yumin, Zhang Wenbao, the g-C of efficiency3 N4/TiO2The preparation of composite photo-catalyst and performance study thereof, apply chemical industry,
The 8th phase of volume 43, in August, 2014).But the synthetic method of titanium dioxide nitridation carbon composite now compares
Complicated and loaded down with trivial details, by-product is more, all uses the organic solvent that toxicity is bigger.Secondly, titanium dioxide/nitridation carbon composite
Although photocatalysis efficiency has obtained raising to a certain extent, but is also far from reaching satisfactory degree, still have
Bigger room for promotion.Based on above some, quantum dot is incorporated into photocatalysis field, the special construction of quantum dot result in it
There is skin effect, quantum size effect, Dielectric confinement effect and macro quanta tunnel effect, thus derive and macroscopic view
The low-dimensional physical property that system is different with microsystem, shows many and is different from the physicochemical properties of macroscopic view block materials, just
The deficiency of titanium dioxide can be made up.
The present invention is by nano titanium oxide and g-C3N4Both quantum dots combine, the binary complex system prepared
Belong to environmentally friendly composite, and catalytic efficiency is high.It addition, preparation technology of the present invention is easy, production efficiency is high, and
Preparation process introduces without poisonous and harmful substance, belongs to green preparation process, beneficially industrialized production.
Summary of the invention
It is an object of the invention to provide a kind of titanium dioxide/g-C3N4The preparation method of quantum dot composite catalyst, in order to solve
The problem that organic wastewater efficiently processes.
One titanium dioxide/g-C of the present invention3N4The preparation method of quantum dot composite catalyst comprises the steps of
(1) under conditions of strong stirring, 5-15ml tetra-n-butyl titanate is slowly added in 20-50ml dehydrated alcohol, stirs
After mixing 10-60min, obtain the mixed solution A of ethanol and tetra-n-butyl titanate.
(2) 2-6ml glacial acetic acid and 5-15ml deionized water are added in 20-50ml dehydrated alcohol, strong stirring 10-
After 60min, obtain the mixed solution B of ethanol, glacial acetic acid, deionized water;In mixed solution B, drip hydrochloric acid, regulate PH < 3.
(3) under 10-30 DEG C of water-bath, stirring condition, by above-mentioned mixed solution A with the speed of 0.5-2 drop/sec, it is added drop-wise to
In mixed solution B;After dropping, after being stirred continuously until generation gel, then stand to gel complete under 20-60 DEG C of water-bath
Entirely.
(4) by the gel of above-mentioned steps gained in 40-80 DEG C of dry 6-24h more ground, calcining, the coldest
But, grind, obtain nano titanium oxide;Described 3 DEG C/min of calcining heating rate, maintains 500 DEG C, calcines 3 hours.
(5) 100mg nano titanium oxide is joined in the deionized water of 100-n milliliter, after ultrasonic disperse 30min, add
Enter n milliliter 0.5mol/L g-C3N4Quantum dot solution, the most again under 10-30 DEG C of water bath condition, is stirred overnight, obtains titanium dioxide
Titanium/g-C3N4Quantum dot binary composite catalyst.
In described step (5), the value of n is 1,2,4 or 8.
Advantages of the present invention:
The present invention is from the angle of composite, by g-C3N4Quantum dot and TiO2Spherical nanoparticle is combined with each other, permissible
Effectively suppression photo-generated carrier in conjunction with, increase the stability of composite, and catalytic efficiency is high, belongs to environmental friendliness
Type composite.It addition, preparation technology of the present invention is easy, production efficiency is high, introduces without poisonous and harmful substance in preparation process, belongs to
In green preparation process, beneficially industrialized production.
Accompanying drawing explanation
Fig. 1: titanium dioxide/g-C of the present invention3N4Quantum dot composite catalyst be used for degrading under simulated solar irradiation 50ml,
The degradation curve figure of the methyl orange solution of 10PPm.
Detailed description of the invention
Below by embodiment, the invention will be further described, titanium dioxide/g-C that embodiment 1-4 prepares3N4Quantum dot is multiple
Close catalyst TiO2-CNQDsX represents, X represents g-C3N4The volume of quantum dot solution.
Embodiment 1
1) measure 35mL dehydrated alcohol in a clean beaker A with graduated cylinder, under conditions of strong stirring, be slowly added into 10mL titanium
Acid N-butyl, then strong stirring 20min, obtain the mixed solution A of ethanol and tetra-n-butyl titanate.
2) measure 35mL dehydrated alcohol in a clean beaker B, in B beaker, add 4mL glacial acetic acid and 10mL deionization
Water, strong stirring 20min, obtain ethanol, glacial acetic acid, the mixed solution B of deionized water three.Drip appropriate concentrated hydrochloric acid, regulation
PH 。
3) B beaker it is placed under 25 DEG C of water bath condition and is stirred vigorously, being slowly added dropwise unsettled for solution A in B beaker.
4) after dropping, stirring at low speed is continued, until producing gel.And stand to gel complete under 40 DEG C of water-baths
5) gel 80 DEG C obtained is dried, 12 hours drying times.And dried sample is ground.
6) by the sample high-temperature calcination in Muffle furnace after above-mentioned grinding.After natural cooling levigate, obtain white TiO2 receive
The powder of rice grain.
7) weighing 100mg TiO2 nano-particle, add in 99ml deionized water, ultrasonic 30min makes dispersion,
8) in above-mentioned mixed liquor, 1ml g-C is added3N4Quantum dot solution, is placed in heating in water bath agitator by the two mixed liquor
In, control temperature 25 DEG C, be stirred overnight.
9) binary composite catalyst after above-mentioned mechanical mixture loads adds 50ml 10ppm methyl orange to degrade
Experiment.
Products therefrom is TiO2-CNQDs 1.0ml, under simulated solar irradiation, the methyl orange for degrade 50ml, 10PPm is molten
Liquid, after 120min, degradation rate reaches 92.82%.
Embodiment 2
In step (7), add and 98ml deionized water, step (8) add g-C3N4Quantum dot solution 2ml, other steps are with real
Execute example 1.
Products therefrom is TiO2-CNQDs2.0ml, under simulated solar irradiation, the methyl orange for degrade 50ml, 10PPm is molten
Liquid, after 100min, degradation rate reaches 90.15%.
Embodiment 3
In step (7), adding and add g-C3N4 quantum dot solution 4ml in 96ml deionized water, step (8), other steps are with real
Execute example 1.
Products therefrom is TiO2-CNQDs4.0ml is molten for the methyl orange of the 50ml 10PPm that degrades under simulated solar irradiation
Liquid, after 120min, degradation rate reaches 91.38%.
Embodiment 4
In step (7), add and 92ml deionized water, step (8) add g-C3N4Quantum dot solution 8ml, other steps are with real
Execute example 1.
Products therefrom is TiO2-CNQDs8.0ml, under simulated solar irradiation, the methyl orange for degrade 50ml, 10PPm is molten
Liquid, after 120min, degradation rate reaches 96.17%.
Knowable to above-described embodiment, the quantum dot solution of different ratio and the catalytic effect of TiO2 nano particle composite material are the most relatively
Ideal, this is all owing to, g-C3N4Quantum dot as electron transmission person, can effectively suppress photo-generated carrier in conjunction with, from
And improve photocatalytic activity, enhance the charge transfer rate between interface.
Claims (2)
1. titanium dioxide/g-C3N4The preparation method of quantum dot composite catalyst, it is characterised in that: described preparation method
Comprise the steps of
(1) under conditions of strong stirring, 5-15ml tetra-n-butyl titanate is slowly added in 20-50ml dehydrated alcohol, stirs
After mixing 10-60min, obtain the mixed solution A of ethanol and tetra-n-butyl titanate;
(2) 2-6ml glacial acetic acid and 5-15ml deionized water are added in 20-50ml dehydrated alcohol, after strong stirring 10-60min,
Obtain the mixed solution B of ethanol, glacial acetic acid, deionized water;In mixed solution B, drip hydrochloric acid, regulate PH < 3;
(3) under 10-30 DEG C of water-bath, stirring condition, by above-mentioned mixed solution A with the speed of 0.5-2 drop/sec, it is added drop-wise to mixing
In solution B;After dropping, after being stirred continuously until generation gel, then under 20-60 DEG C of water bath condition, stand complete to gel
Entirely;
(4) by 40-80 DEG C of dry 6-24h more ground for the gel of step (3) gained, calcining, natural cooling, grind
Mill, obtains nano titanium oxide;Described 3 DEG C/min of calcining heating rate, maintains 500 DEG C to calcine 3 hours;
(5) 100mg nano titanium oxide is joined in the deionized water of 100-n milliliter, after ultrasonic disperse 30min, add n milli
Rise 0.5mol/L g-C3N4Quantum dot solution, the most again under 10-30 DEG C of water bath condition, is stirred overnight, and obtains titanium dioxide/g-
C3N4Quantum dot binary composite catalyst.
A kind of titanium dioxide/g-C the most according to claim 13N4The preparation method of quantum dot composite catalyst, its feature
It is: in described step (5), the value of n is 1,2,4 or 8.
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Cited By (15)
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CN107649107A (en) * | 2017-09-25 | 2018-02-02 | 兰州大学 | A kind of quantum dot/TiO2The preparation method and applications of composite |
CN108686691A (en) * | 2018-03-26 | 2018-10-23 | 南昌航空大学 | A kind of preparation method of Gd2 O3 class graphite phase carbon nitride catalysis material |
CN108772094A (en) * | 2018-07-12 | 2018-11-09 | 重庆交通大学 | A kind of nitridation carbon quantum dot/TiO 2 sol and preparation method thereof |
CN109158088A (en) * | 2018-09-06 | 2019-01-08 | 潘钕 | A kind of preparation method of cellulose aerogels adsorbent |
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CN113457652A (en) * | 2021-06-04 | 2021-10-01 | 华侨大学 | Ag-g-C3N4QDs-TiO2Preparation method and application of ternary photocatalyst |
CN113828294A (en) * | 2021-10-29 | 2021-12-24 | 盐城工学院 | Nano TiO (titanium dioxide)2/g-C3N4Preparation method of photocatalytic material |
CN114602527A (en) * | 2022-03-31 | 2022-06-10 | 浙江省科创新材料研究院 | g-C3N4/TiO2In-situ preparation method of nano heterojunction photocatalyst |
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