CN112275272A - Preparation method and application of reduced graphene oxide titanium dioxide composite material - Google Patents
Preparation method and application of reduced graphene oxide titanium dioxide composite material Download PDFInfo
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- CN112275272A CN112275272A CN202010937175.0A CN202010937175A CN112275272A CN 112275272 A CN112275272 A CN 112275272A CN 202010937175 A CN202010937175 A CN 202010937175A CN 112275272 A CN112275272 A CN 112275272A
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- graphene oxide
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- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002351 wastewater Substances 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical class CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002834 transmittance 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/32—Freeze drying, i.e. lyophilisation
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
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- Optics & Photonics (AREA)
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Abstract
The invention discloses a preparation method of a reduced graphene oxide titanium dioxide composite material, which comprises the steps of dispersing reduced graphene oxide by a hydrothermal method, reacting the dispersed reduced graphene oxide with a titanium tetrachloride solution in a tetrafluoroethylene hydrothermal kettle, washing and drying after the reaction is finished, and obtaining the reduced graphene oxide titanium dioxide composite material.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method and application of a reduced graphene oxide titanium dioxide composite material.
Background
With the acceleration of industrial process, the problem of water environment pollution is getting worse. The organic pollutants difficult to degrade have the characteristics of stable chemical property, high biological toxicity and the like, and can bring great harm to an ecosystem and human health when being discharged into a water body. The printing and dyeing wastewater contains azo refractory organic matters and has the characteristics of high chroma, difficult biodegradation, complex components, large discharge amount and the like, so the treatment is difficult to reach the standard. A plurality ofResearchers use titanium dioxide photocatalysis technology to carry out photocatalysis treatment on some pollutants which are difficult to degrade, such as petroleum refining sewage, printing and dyeing wastewater, coking wastewater and the like, and remarkable effect is achieved. The pure titanium dioxide photocatalytic material generates a high recombination rate of photo-generated electron hole pairs after photo-excitation, so that the photocatalytic activity is reduced. Therefore, an effective method for modifying titanium dioxide is urgently needed. GO/TiO2The preparation of the composite photocatalytic material is always a research focus, but the GO/TiO synthesized at present2Composite material with Graphene Oxide (GO) sheet coated on TiO2In addition, excessive GO can affect the light transmittance, and the improvement effect on the photocatalytic activity is not ideal, so that the composite material of the reduced graphene oxide and the titanium dioxide is provided, the problem of the reverse cladding is further solved, and the composite material is used for treating organic polluted wastewater.
Disclosure of Invention
Aiming at the technical defects, the preparation method and the application of the reduced graphene oxide titanium dioxide composite material are provided, so that the problem of excessive coating of titanium dioxide by graphene oxide lamella is solved, and the treatment capacity of organic polluted wastewater can be improved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a reduced graphene oxide titanium dioxide composite material comprises the following steps:
(1) preparing a reduced graphene oxide dispersion liquid: putting the reduced graphene oxide into a beaker, adding deionized water, stirring with a glass cup, and putting into an ultrasonic instrument for ultrasonic treatment;
(2) preparing a reduced graphene oxide titanium dioxide mixed solution: sequentially adding acid and titanium tetrachloride solution into the reduced graphene oxide dispersion liquid in the step (1), and putting the solution into an ultrasonic instrument for ultrasonic reaction;
(3) hydrothermal reaction: and (3) putting the mixture obtained in the step (2) into a tetrafluoroethylene hydrothermal kettle for reaction, and washing and drying after the reaction is finished to obtain the reduced graphene oxide titanium dioxide composite material.
Further, the time of the ultrasonic treatment in the step (1) is 1-3h, and the ultrasonic power is 800-1200W.
Further, the mass ratio of the reduced graphene oxide to the titanium tetrachloride is 1:2-1: 8.
Further, the acid in the step (2) is hydrochloric acid or sulfuric acid.
Further, the pH of the reaction system in the step (2) is 3-6.
Further, the ultrasonic time in the step (2) is 30-240 min.
Further, the hydrothermal reaction temperature in the step (3) is 120-.
Further, the washing in the step (3) is washed by deionized water, and the standard of the clean washing is that the pH is neutral.
Further, the drying method in the step (3) is freeze drying, and the freeze drying time is 12-24 h.
Further, the reduced graphene oxide titanium dioxide composite material is used for treating organic dye wastewater.
The invention has the beneficial effects that:
the preparation method of the reduced graphene oxide titanium dioxide composite material provided by the invention is simple and easy to operate. Can obviously remove the dye color in the dye wastewater and degrade organic pollutants.
Detailed Description
In order to make the purpose and technical solution of the embodiments of the present invention clearer, the technical solution of the embodiments of the present invention will be clearly and completely described below with reference to the implementation examples of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments.
Example 1
A preparation method of a reduced graphene oxide titanium dioxide composite material comprises the following steps: weighing 1g of reduced graphene oxide, putting the reduced graphene oxide into a beaker with the volume of 1L, adding 500mL of deionized water, stirring the graphene oxide powder at the bottom of the beaker by using a glass cup to avoid occupying the bottom, then sealing the opening of the beaker, and putting the beaker into an ultrasonic instrument for ultrasonic dispersion for 2 hours, wherein the ultrasonic power is 800W. And taking out the reduced graphene oxide titanium dioxide ultrasonic dispersion liquid, adding 70mL of hydrochloric acid solution, continuously adding 7mL of titanium tetrachloride solution, stirring for a while by using a glass cup, and then carrying out ultrasonic reaction for 1 h. Then the ultrasonic dispersion liquid is transferred into a polytetrafluoroethylene hydrothermal kettle and reacts for 24 hours at the temperature of 200 ℃. After the water was heated, the cooled reaction solution was taken out, filtered, washed with distilled water to neutrality, and then freeze-dried for 24 hours.
Example 2
A preparation method of a reduced graphene oxide titanium dioxide composite material comprises the following steps: weighing 1.5g of reduced graphene oxide, putting the reduced graphene oxide into a beaker with the volume of 1L, adding 500mL of deionized water, stirring the graphene oxide powder at the bottom of the beaker by using a glass cup to avoid occupying the bottom, then sealing the opening of the beaker, putting the beaker into an ultrasonic instrument, and ultrasonically dispersing for 2.5h with the ultrasonic power of 800W. And taking out the reduced graphene oxide titanium dioxide ultrasonic dispersion liquid, adding 65mL of hydrochloric acid solution, continuously adding 6mL of titanium tetrachloride solution, stirring for a while by using a glass cup, and then carrying out ultrasonic reaction for 1.5 h. Then the ultrasonic dispersion liquid is transferred into a polytetrafluoroethylene hydrothermal kettle and reacts for 24 hours at 180 ℃. After the water was heated, the cooled reaction solution was taken out, filtered, washed with distilled water to neutrality, and then freeze-dried for 24 hours.
Example 3
A preparation method of a reduced graphene oxide titanium dioxide composite material comprises the following steps: weighing 0.8g of reduced graphene oxide, putting the reduced graphene oxide into a beaker with the volume of 1L, adding 500mL of deionized water, stirring the graphene oxide powder at the bottom of the beaker by using a glass cup to avoid occupying the bottom, then sealing the opening of the beaker, putting the beaker into an ultrasonic instrument, and ultrasonically dispersing for 1h, wherein the ultrasonic power is 1000W. And taking out the reduced graphene oxide titanium dioxide ultrasonic dispersion liquid, adding 60mL of hydrochloric acid solution, continuously adding 5mL of titanium tetrachloride solution, stirring for a while by using a glass cup, and then carrying out ultrasonic reaction for 1 h. Then the ultrasonic dispersion liquid is transferred into a polytetrafluoroethylene hydrothermal kettle and reacts for 24 hours at the temperature of 150 ℃. After the water was heated, the cooled reaction solution was taken out, filtered, washed with distilled water to neutrality, and then freeze-dried for 24 hours.
Example 4
A preparation method of a reduced graphene oxide titanium dioxide composite material comprises the following steps: weighing 1g of reduced graphene oxide, putting the reduced graphene oxide into a beaker with the volume of 1L, adding 500mL of deionized water, stirring the graphene oxide powder at the bottom of the beaker by using a glass cup to avoid occupying the bottom, then sealing the opening of the beaker, and putting the beaker into an ultrasonic instrument for ultrasonic dispersion for 2 hours, wherein the ultrasonic power is 1000W. And taking out the reduced graphene oxide titanium dioxide ultrasonic dispersion liquid, adding 50mL of hydrochloric acid solution, continuously adding 4mL of titanium tetrachloride solution, stirring for a while by using a glass cup, and then carrying out ultrasonic reaction for 1 h. Then the ultrasonic dispersion liquid is transferred into a polytetrafluoroethylene hydrothermal kettle and reacts for 24 hours at the temperature of 120 ℃. After the water was heated, the cooled reaction solution was taken out, filtered, washed with distilled water to neutrality, and then freeze-dried for 24 hours.
Comparative example 1
Selecting nano titanium dioxide and industrial grade.
The reduced graphene oxide titanium dioxide composite materials prepared in the embodiments 1 to 4 were subjected to a test for removing organic pollutants in dye wastewater, and the test results were as follows:
the reduced graphene oxide titanium dioxide composite material provided by the invention can obviously remove the dye color in the dye wastewater, namely, the dye organic substances are decomposed, especially, the reduced graphene oxide titanium dioxide composite material in the embodiment 1 shows a quite rapid decomposition level and is thoroughly decomposed. The composite material has wide application value for organic wastewater. The thickness of the reduced graphene oxide is lower than that of the graphene oxide layer, so that the problem of excessive coating of titanium dioxide particles is solved, the exposure of the titanium dioxide particles is facilitated, and the photocatalytic capability is more fully exerted.
In the description herein, the particular features, structures, materials, or characteristics disclosed may be combined in any suitable manner in any one or more embodiments or examples. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents, all of which are within the scope of the invention.
Claims (10)
1. A preparation method of a reduced graphene oxide titanium dioxide composite material is characterized by comprising the following steps:
(1) preparing a reduced graphene oxide dispersion liquid: putting the reduced graphene oxide into a beaker, adding deionized water, stirring with a glass cup, and putting into an ultrasonic instrument for ultrasonic treatment;
(2) preparing a reduced graphene oxide titanium dioxide mixed solution: sequentially adding acid and titanium tetrachloride solution into the reduced graphene oxide dispersion liquid in the step (1), and putting the solution into an ultrasonic instrument for ultrasonic reaction;
(3) hydrothermal reaction: and (3) putting the mixture obtained in the step (2) into a tetrafluoroethylene hydrothermal kettle for reaction, and washing and drying after the reaction is finished to obtain the reduced graphene oxide titanium dioxide composite material.
2. The method for preparing a reduced graphene oxide titanium dioxide composite material according to claim 1, wherein the ultrasonic treatment time in the step (1) is 1-3h, and the ultrasonic power is 800-.
3. The method of claim 1, wherein the mass ratio of the reduced graphene oxide to titanium tetrachloride is 1:2 to 1: 8.
4. The method of claim 1, wherein the acid in step (2) is hydrochloric acid or sulfuric acid.
5. The method for preparing a reduced graphene oxide titanium dioxide composite material according to claim 1, wherein the pH of the reaction system in the step (2) is 3 to 6.
6. The method for preparing a reduced graphene oxide titanium dioxide composite material according to claim 1, wherein the ultrasonic time in the step (2) is 30-240 min.
7. The method for preparing a reduced graphene oxide titanium dioxide composite material according to claim 1, wherein the hydrothermal reaction temperature in the step (3) is 120-200 ℃ and the reaction time is 12-36 h.
8. The method of claim 1, wherein the washing in step (3) is performed with deionized water, and the standard of clean washing is neutral pH.
9. The method for preparing a reduced graphene oxide titanium dioxide composite material according to claim 1, wherein the drying method in the step (3) is freeze drying, and the freeze drying time is 12-24 h.
10. The reduced graphene oxide titanium dioxide composite material according to any one of claims 1 to 9, for use in treatment of dye organic wastewater.
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| CN202010937175.0A CN112275272A (en) | 2020-09-08 | 2020-09-08 | Preparation method and application of reduced graphene oxide titanium dioxide composite material |
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|---|---|---|---|---|
| CN102350334A (en) * | 2011-08-08 | 2012-02-15 | 江苏大学 | Graphene/mesoporous titanium dioxide visible light catalyst and preparation method |
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2020
- 2020-09-08 CN CN202010937175.0A patent/CN112275272A/en active Pending
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| CN102350334A (en) * | 2011-08-08 | 2012-02-15 | 江苏大学 | Graphene/mesoporous titanium dioxide visible light catalyst and preparation method |
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