CN110947411A - Nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound with good visible light catalytic performance and preparation method thereof - Google Patents
Nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound with good visible light catalytic performance and preparation method thereof Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 76
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 38
- 239000002071 nanotube Substances 0.000 title claims abstract description 24
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 16
- 150000001875 compounds Chemical class 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 18
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims 5
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 7
- 229960000907 methylthioninium chloride Drugs 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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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
- 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
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- 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
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound with good visible light catalytic performance and a preparation method thereof. According to the invention, nitrogen is introduced into the titanium dioxide nanotube and reduced graphene oxide composite material through one-step hydrothermal reaction, so that the composite material has very good visible light catalytic degradation performance, the application of titanium dioxide in the field of photocatalysis is greatly widened, and the application prospect is very good.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite with good visible light catalytic performance and a preparation method thereof.
Background
Titanium dioxide is used as a photocatalyst material with the most research and development value in the 21 st century, can be widely applied to the field of photocatalysis of light, and has the advantages of no toxicity, environmental protection, economy, stable physical and chemical properties, high reaction activity and the like in the field of photocatalytic degradation of organic matters. However, titanium dioxide itself has obvious defects, such as high band gap energy of electron transition, activity only under ultraviolet light, low utilization rate of sunlight, large forbidden band width under visible light, low catalytic efficiency and the like, which limit its application under visible light, and at the same time, photo-generated electron and hole pairs also have high recombination rate, which severely restricts the wide application of titanium dioxide photocatalysts.
Graphene as a precursor of other carbon materials is a monolayer of carbon atoms sp2Hybrid cellular packed lenses. The material has unique physical, chemical and thermal properties, has very superior strength, flexibility, electric conductivity, heat conductivity and optical properties, and is developed in the fields of materials, physics, electronic information, computers, aerospace and the like. In recent years, graphene has also received much attention in the field of photocatalysis.
Titanium dioxide, graphene and composites thereof have certain limitations in the field of visible light catalysis. The non-metal doping or the compounding with the graphene can possibly widen the photoresponse range of the titanium dioxide and improve the efficiency of photo-generated electron and hole pairs, thereby improving the photocatalytic performance of the nano compound.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound and a preparation method thereof, aiming at improving the visible light catalytic performance of the compound.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a preparation method of a nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound with good visible light catalytic performance is characterized by comprising the following steps:
step 1, dissolving urea into a sodium hydroxide solution, adding graphene oxide, and performing ultrasonic dispersion to obtain a mixed solution A;
step 2, adding titanium dioxide powder into the mixed solution A, and after ultrasonic dispersion, continuing stirring to obtain a mixed solution B;
step 3, pouring the mixed solution B into a high-pressure reaction kettle, and carrying out hydrothermal reaction to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, then acid washing, and finally washing with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then performing high-temperature heat treatment in a vacuum drying oven to obtain the target product, namely the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound.
Further, in step 1: the concentration of the sodium hydroxide solution is 5-20 mol/L; the mass ratio of the urea to the graphene oxide is 1: 1; the time of ultrasonic dispersion is 0.5-4 hours.
Further, in step 2: the mass ratio of the titanium dioxide to the urea and the graphene oxide in the mixed solution A is 5-1: 1: 1; the time of ultrasonic dispersion is 0.5-4 hours, and the time of continuous stirring is 1-5 hours.
Further, in step 3: the temperature of the hydrothermal reaction is 120-180 ℃ and the time is 10-30 hours.
Further, in step 4: the acid used for acid cleaning is hydrochloric acid with the concentration of 0.05-1 mol/L, and the acid cleaning time is 5-48 hours.
Further, in step 5: the high-temperature heat treatment is carried out at the temperature of 200-500 ℃ for 2-10 hours.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, nitrogen is introduced into the titanium dioxide nanotube and reduced graphene oxide composite material through a hydrothermal one-step reaction, so that the composite material has very good visible light catalytic degradation performance, the application of titanium dioxide in the field of photocatalysis is greatly widened, and the application prospect is very good.
Drawings
FIG. 1 is a TEM photograph of a sample obtained in example 1;
FIG. 2 is the catalytic degradation performance of the sample obtained in example 1 on a methylene blue solution under the irradiation of visible light;
FIG. 3 is a comparison of the samples obtained in example 1 before and after the catalytic degradation of the methylene blue solution under the irradiation of visible light.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite is synthesized by the following steps:
step 1, firstly, dissolving 40mg of urea into 100mL of sodium hydroxide aqueous solution (10mol/L), then adding 40mg of graphene oxide, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution A;
step 2, adding 40mg of titanium dioxide powder into the mixed solution A, performing ultrasonic dispersion for 1 hour, and then continuing stirring for 4 hours to obtain a mixed solution B;
step 3, pouring the mixed solution B into a 50mL high-pressure reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 20 hours to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, pouring the precipitate into 500mL of 0.1mol/L HCl solution for acid washing for 24 hours, and finally washing the precipitate with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then placing the dried product in a vacuum drying oven for 5 hours at the high temperature of 300 ℃ to obtain the target product, namely the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound.
Fig. 1 is a TEM photograph of the target product nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite obtained in this example, from which the nanotube structure of the nanocomposite can be clearly seen, and from which the lamellar structure of the large lamellar reduced graphene oxide which is nearly transparent can also be clearly seen, which verifies that the nitrogen-doped nanocomposite prepared by the hydrothermal method not only has the structure of the titanium dioxide nanotube, but also has the structure of the reduced graphene oxide.
100mL of methylene blue solution with the concentration of 20mg/L is prepared, and 50mg of the target product prepared in the embodiment is added to verify the photocatalytic degradation efficiency of the methylene blue under the irradiation of visible light, and the result is shown in FIG. 2. It can be seen that under the irradiation of visible light, the absorbance of the methylene blue solution is in a trend of decreasing along with the time extension, and at 150min, the absorbance is close to 0, which indicates that the visible light catalysis effect of the obtained compound is better.
Fig. 3 is a comparison graph before and after degradation, from which it can be seen that the methylene blue stock solution (a) is darker in color, and the water sample (b) after the sample is degraded by visible light catalysis is almost transparent, which indicates that the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite has a very good catalytic effect on the methylene blue solution under the irradiation of visible light, and is consistent with the result of fig. 2.
Example 2
The nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite is synthesized by the following steps:
step 1, firstly, dissolving 50mg of urea into 120mL of sodium hydroxide aqueous solution (10mol/L), then adding 50mg of graphene oxide, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution A;
step 2, adding 50mg of titanium dioxide powder into the mixed solution A, performing ultrasonic dispersion for 1 hour, and then continuing stirring for 4 hours to obtain a mixed solution B;
step 3, pouring the mixed solution B into a 50mL high-pressure reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 20 hours to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, pouring the precipitate into 500mL of 0.1mol/L HCl solution for acid washing for 24 hours, and finally washing the precipitate with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then placing the dried product in a vacuum drying oven for 5 hours at the high temperature of 300 ℃ to obtain the target product, namely the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound.
Through analysis and test, the product obtained in the embodiment is a target product and also has very good visible light catalytic degradation performance.
Example 3
The nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite is synthesized by the following steps:
step 1, firstly, dissolving 40mg of urea into 100mL of sodium hydroxide aqueous solution (10mol/L), then adding 40mg of graphene oxide, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution A;
step 2, adding 40mg of titanium dioxide powder into the mixed solution A, performing ultrasonic dispersion for 1 hour, and then continuing stirring for 4 hours to obtain a mixed solution B;
step 3, pouring the mixed solution B into a 50mL high-pressure reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 24 hours to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, pouring the precipitate into 500mL of 0.1mol/L HCl solution for acid washing for 24 hours, and finally washing the precipitate with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then placing the dried product in a vacuum drying oven for 5 hours at the high temperature of 400 ℃, thus obtaining the target product of the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite.
Through analysis and test, the product obtained in the embodiment is a target product and also has very good visible light catalytic degradation performance.
Example 4
The nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite is synthesized by the following steps:
step 1, firstly, dissolving 50mg of urea into 120mL of sodium hydroxide aqueous solution (10mol/L), then adding 50mg of graphene oxide, and performing ultrasonic dispersion for 1 hour to obtain a mixed solution A;
step 2, adding 50mg of titanium dioxide powder into the mixed solution A, performing ultrasonic dispersion for 2 hours, and then continuing stirring for 6 hours to obtain a mixed solution B;
step 3, pouring the mixed solution B into a 50mL high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ for 20 hours to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, pouring the precipitate into 500mL0.2mol/L HCl solution for acid washing for 24 hours, and finally washing with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then placing the dried product in a vacuum drying oven for 5 hours at the high temperature of 300 ℃ to obtain the target product, namely the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound.
Through analysis and test, the product obtained in the embodiment is a target product and also has very good visible light catalytic degradation performance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A preparation method of a nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound with good visible light catalytic performance is characterized by comprising the following steps:
step 1, dissolving urea into a sodium hydroxide solution, adding graphene oxide, and performing ultrasonic dispersion to obtain a mixed solution A;
step 2, adding titanium dioxide powder into the mixed solution A, and after ultrasonic dispersion, continuing stirring to obtain a mixed solution B;
step 3, pouring the mixed solution B into a high-pressure reaction kettle, and carrying out hydrothermal reaction to obtain a reaction solution;
step 4, cooling the reaction liquid to room temperature, and pouring out the reaction kettle; washing the obtained precipitate with water to neutrality, then acid washing, and finally washing with water to neutrality;
and 5, firstly drying the product obtained in the step 4 in a forced air drying oven, and then performing high-temperature heat treatment in a vacuum drying oven to obtain the target product, namely the nitrogen-doped titanium dioxide nanotube/reduced graphene oxide compound.
2. The method according to claim 1, wherein in step 1: the concentration of the sodium hydroxide solution is 5-20 mol/L; the mass ratio of the urea to the graphene oxide is 1: 1; the time of ultrasonic dispersion is 0.5-4 hours.
3. The method according to claim 1, wherein in step 2: the mass ratio of the titanium dioxide to the urea and the graphene oxide in the mixed solution A is 5-1: 1: 1; the time of ultrasonic dispersion is 0.5-4 hours, and the time of continuous stirring is 1-5 hours.
4. The method according to claim 1, wherein in step 3: the temperature of the hydrothermal reaction is 120-180 ℃ and the time is 10-30 hours.
5. The method according to claim 1, wherein in step 4: the acid used for acid cleaning is hydrochloric acid with the concentration of 0.05-1 mol/L, and the acid cleaning time is 5-48 hours.
6. The method according to claim 1, wherein in step 5: the high-temperature heat treatment is carried out at the temperature of 200-500 ℃ for 2-10 hours.
7. The nitrogen-doped titanium dioxide nanotube/reduced graphene oxide composite prepared by the preparation method of any one of claims 1 to 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113262772A (en) * | 2021-05-13 | 2021-08-17 | 岭南师范学院 | Preparation method of high photocatalytic efficiency nano composite material |
| CN115672300A (en) * | 2022-09-07 | 2023-02-03 | 福建省蓝光节能科技有限公司 | Novel high-efficiency VOCs photocatalytic purification material |
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| CN104415772A (en) * | 2013-08-23 | 2015-03-18 | 国家纳米科学中心 | Nitrogen-doped reduced graphene oxide / nitrogen-doped titanium dioxide composite material and preparation method and application thereof |
| CN105536848A (en) * | 2016-03-01 | 2016-05-04 | 常州墨之萃科技有限公司 | Graphene composite and preparation method thereof |
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