CN112657533B - Carbon-nitrogen-sulfur co-doped heterojunction photocatalyst and preparation method and application thereof - Google Patents
Carbon-nitrogen-sulfur co-doped heterojunction photocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
A carbon-nitrogen-sulfur co-doped heterojunction photocatalyst is prepared from graphitized carbon nitride and carbon-nitrogen-sulfur co-doped titanium dioxide nanoparticles according to a molar ratio of 1:8 composite microsphere structure, adding melamine and thiourea into the preparation of TiO 2 In the solution A of (2), preparing the CNS-TiO co-doped with carbon, nitrogen and sulfur by a one-step hydrothermal method and anaerobic calcination 2 /g‑C 3 N 4 Heterojunction photocatalysts. CNS-TiO made by the invention 2 /g‑C 3 N 4 The heterojunction photocatalyst has excellent visible light degradation activity on textile wastewater represented by methyl orange, and has wide application prospect in the field of textile wastewater treatment.
Description
Technical Field
The invention relates to the field of catalytic materials, in particular to a carbon-nitrogen-sulfur co-doped heterojunction photocatalyst, and a preparation method and application thereof.
Background
With the continuous acceleration of world industrialization, the generated pollutants such as industrial waste gas, waste water, dust and the like are rapidly increased, and the pollution to the environment becomes a serious global problem. From 1976, carey et al have found that titanium dioxide (TiO 2 ) The successful photodegradation dechlorination of polychlorinated biphenyl solutions opens a new way to treat contaminants with photocatalysts. The photocatalysis technology has the advantages of mild reaction condition, simple operation, no secondary pollution and the like, and can treat environmental pollution thoroughly, so that the photocatalysis degradation of pollutants has become a green new technology for solving environmental problems and a most promising pollution treatment way to pay attention.
TiO 2 The material has the advantages of proper energy band position, good stability, no toxicity, low price and the like, becomes an ideal environment-friendly photocatalytic material, and is widely applied to sewage treatment. However, tiO 2 In practical application, the wide band gap (eg=3.2 eV) results in a narrow light response range, which can only be excited by ultraviolet light accounting for 4% of sunlight, and has extremely low utilization rate of visible light accounting for about 50% of sunlight; and TiO 2 Photo-generated electricitySon-hole (e) - /h + ) Very easy and rapid compounding, so that TiO 2 The total efficiency of photocatalytic degradation is not high.
Nowadays, tiO can be greatly improved by doping or coupling with nonmetallic elements, narrow bandgap semiconductors, etc 2 Is used for the photocatalytic performance of the catalyst. g-C is reported 3 N 4 With a medium-width band gap, excellent photo-generated electron-hole (e - /h + ) Delivery capability, simple preparation, numerous precursor species, g-C 3 N 4 Becomes TiO and 2 the first choice of heterojunction is formed by recombination. The combination of the two can expand TiO 2 Meanwhile, the heterojunction is formed, so that the recombination rate of photo-generated electrons and holes can be reduced, and the visible light catalytic activity can be improved. Researchers have prepared g-C 3 N 4 /Ag/TiO 2 Microsphere, (Au/A-TiO) 2 )@g-C 3 N 4 Heterojunction, tiO 2 /g-C 3 N 4 /Bi 2 WO 6 Heterojunction etc. will g-C 3 N 4 And TiO 2 The heterojunction catalyst is formed by combination, and has remarkable effect in degradation of organic pollutants. However, some of the composite catalysts contain heavy metals, which may cause secondary pollution in wastewater purification.
Therefore, how to develop a safe and environment-friendly photocatalyst with high catalytic activity under visible light is a problem to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a carbon-nitrogen-sulfur co-doped heterojunction photocatalyst which has high visible light catalytic activity and strong degradation capability on organic pollutants, and is particularly suitable for treating textile wastewater containing methyl orange.
The technical scheme of the invention is as follows: a carbon-nitrogen-sulfur co-doped heterojunction photocatalyst is prepared from graphitized carbon nitride and carbon-nitrogen-sulfur co-doped titanium dioxide nanoparticles according to a molar ratio of 1:8 a microsphere structure formed by compounding.
The invention also provides a preparation method of the heterojunction photocatalyst, which comprises the following steps:
1) Dripping a titanium source into a mixed solution of water and ethanol, and stirring to obtain a solution A, wherein the temperature of the mixed solution is 0-4 ℃;
2) Adding melamine into the solution A obtained in the step 1), and carrying out ultrasonic vibration to obtain a solution B;
3) Adding thiourea into the solution B obtained in the step 2), and carrying out ultrasonic vibration to obtain a solution C;
4) Carrying out hydrothermal reaction on the solution C obtained in the step 3) at 130-170 ℃ to obtain a precipitate and obtain an intermediate;
5) Washing the intermediate obtained in the step 4), drying, and calcining for 4-5 hours under the conditions of protective atmosphere and 300-400 ℃ to obtain the heterojunction photocatalyst.
Further, the titanium source in the step 1) is any one or more of titanium tetrachloride, tetrabutyl titanate, titanium isopropoxide, titanium sulfate and titanyl sulfate, and preferably tetrabutyl titanate.
Further, the volume ratio of water to ethanol in the mixed solution in the step 1) is 1:1, placing the mixed solution in an ice bath, wherein the stirring time is 10-12h.
Further, the molar ratio of melamine added in step 2) to titanium source added in step 1) is 1:8, the time of ultrasonic oscillation is 30min, and the temperature of ultrasonic oscillation is room temperature.
Further, the molar ratio of thiourea added in step 3) to melamine added in step 2) is 0.5-2:1, the time of ultrasonic oscillation is 10min, and the temperature of ultrasonic oscillation is room temperature.
Further, in the step 4), the solution C is transferred to a high-pressure reaction kettle with a tetrafluoroethylene lining, and is placed in an oven at 130-170 ℃ to perform a hydrothermal reaction for 8-12h, preferably at 150 ℃ for 10h.
Further, in the step 5), the washing is performed three times by deionized water and then two times by ethanol, and the drying temperature is 80 ℃ and the drying time is 2 hours.
The invention also claims the use of the heterojunction photocatalyst described above for photodegradation of contaminants.
Further, the contaminant is methyl orange.
The technical scheme has the following beneficial effects:
1. the carbon-nitrogen-sulfur co-doped heterojunction photocatalyst provided by the invention is prepared by co-doping titanium dioxide (CNS-TiO) with nonmetallic elements of carbon, nitrogen and sulfur 2 ) With graphitized carbon nitride (g-C 3 N 4 ) Forming heterojunction, on the one hand, adjusting TiO 2 Is arranged in the energy band position of TiO 2 Is a band gap constriction that generates more available photogenerated electron-holes under visible light; on the other hand, due to g-C 3 N 4 Is present in combination with TiO 2 Forming heterojunction, g-C 3 N 4 Electrons generated by visible light excitation are transferred to TiO 2 To make the separation of photon-generated carriers more effective and further improve CNS-TiO 2 /g-C 3 N 4 The visible light catalytic activity of the heterojunction photocatalyst is obviously enhanced to the degradation capability of organic pollutants.
2. The preparation method of the invention comprises the steps of adding melamine and thiourea into the catalyst for preparing TiO 2 In the solution A of (2), preparing the CNS-TiO co-doped with carbon, nitrogen and sulfur by a one-step hydrothermal method and anaerobic calcination 2 /g-C 3 N 4 The heterojunction photocatalyst has the advantages of simple preparation method and process, mild conditions and suitability for industrial production.
Further description is provided below with reference to the drawings and detailed description.
Drawings
FIG. 1 is CNS-TiO of microsphere structure prepared in example 1 2 /g-C 3 N 4 Scanning electron microscope image of heterojunction photocatalyst.
FIG. 2 is a CNS-TiO of microsphere structure obtained in example 2 2 /g-C 3 N 4 Scanning electron microscope image of heterojunction photocatalyst.
FIG. 3 is CNS-TiO of microsphere structure prepared in example 2 2 /g-C 3 N 4 Transmission electron microscopy of heterojunction photocatalysts.
FIG. 4 is CNS-TiO of microsphere structure obtained in example 2 2 /g-C 3 N 4 High resolution transmission electron microscopy of heterojunction photocatalysts.
FIG. 5 is CNS-TiO of microsphere structure prepared in example 3 2 /g-C 3 N 4 Scanning electron microscope image of heterojunction photocatalyst.
FIG. 6 shows CNS-TiO prepared in examples 1, 2 and 3 2 /g-C 3 N 4 Heterojunction photocatalyst and g-C 3 N 4 Activity comparison of catalytic degradation of methyl orange under visible light.
FIG. 7 shows CNS-TiO prepared in examples 1, 2 and 3 2 /g-C 3 N 4 Heterojunction photocatalyst and g-C 3 N 4 First order kinetics plot of catalytic degradation of methyl orange under visible light.
Detailed Description
In the invention, tetrabutyl titanate (TBOT) is used as synthetic nano crystal TiO 2 Is a precursor of melamine (C) 3 H 6 N 6 ) As synthetic g-C 3 N 4 Precursor of (C), thiourea (CH) 4 N 2 S), ethanol (CH) 3 CH 2 OH) and Methyl Orange (MO) are all purchased from Beijing City Guangdong fine chemical company.
Example 1
Carbon nitrogen sulfur co-doped CNS-TiO 2 /g-C 3 N 4 The heterojunction photocatalyst is prepared by the following method: (molar ratio of thiourea to melamine is 0.5:1)
1. Slowly dripping 6mL of tetrabutyl titanate into a mixed solution of 15mL of deionized water and 15mL of ethanol in an ice bath, marking the mixed solution as a solution A, maintaining the temperature of about 0 ℃, and magnetically stirring for 12h;
2. weighing 0.4626g of melamine, adding the melamine into the stirred solution A, and carrying out ultrasonic vibration at room temperature for 30min to obtain solution B;
3. weighing 0.0838g of thiourea to be dissolved in the solution B, and carrying out ultrasonic oscillation again for 10min to obtain a reaction mixed solution, and marking the reaction mixed solution as the solution C;
4. transfer the C solution to 50mL of high pressure reaction with tetrafluoroethylene linerPlacing the reaction kettle in an oven at 150 ℃ for hydrothermal reaction for 10h, and discarding supernatant to obtain precipitate which is CNS-TiO 2 /g-C 3 N 4 An intermediate;
5. CNS-TiO obtained in 4) 2 /g-C 3 N 4 Washing the intermediate with deionized water for 3 times and ethanol for 2 times, and then drying the intermediate in an oven at 80 ℃ for 2 hours;
6. drying the CNS-TiO obtained in 5) 2 /g-C 3 N 4 Placing the intermediate in a tube furnace, calcining for 4 hours in a nitrogen atmosphere at a high temperature of 350 ℃ to obtain CNS-TiO co-doped with carbon, nitrogen and sulfur 2 /g-C 3 N 4 Heterojunction photocatalysts.
SEM test of the heterojunction photocatalyst obtained in the step 6) shows that the sample has a spherical structure with a diameter of about 600nm as shown in FIG. 1.
Example 2
Carbon nitrogen sulfur co-doped CNS-TiO 2 /g-C 3 N 4 The heterojunction photocatalyst is prepared by the following method: (molar ratio of thiourea to melamine is 1:1)
1. Slowly dripping 6mL of tetrabutyl titanate into a mixed solution of 15mL of deionized water and 15mL of ethanol in an ice bath, marking the mixed solution as a solution A, maintaining the temperature of about 0 ℃, and magnetically stirring for 12h;
2. weighing 0.4626g of melamine, adding the melamine into the stirred solution A, and carrying out ultrasonic vibration at room temperature for 30min to obtain solution B;
3. weighing 0.1675g of thiourea to be dissolved in the solution B, and carrying out ultrasonic oscillation again for 10min to obtain a reaction mixed solution, and marking the reaction mixed solution as the solution C;
4. transferring the solution C into 50mL high-pressure reaction kettle with tetrafluoroethylene lining, placing the reaction kettle in an oven at 150 ℃ for hydrothermal reaction for 10h, and discarding supernatant to obtain precipitate which is CNS-TiO 2 /g-C 3 N 4 An intermediate;
5. CNS-TiO obtained in 4) 2 /g-C 3 N 4 Washing the intermediate with deionized water for 3 times and ethanol for 2 times, and then washingDrying in an oven at 80 ℃ for 2 hours;
6. drying the CNS-TiO obtained in 5) 2 /g-C 3 N 4 Placing the intermediate in a tube furnace, calcining for 4 hours in a nitrogen atmosphere at a high temperature of 350 ℃ to obtain CNS-TiO co-doped with carbon, nitrogen and sulfur 2 /g-C 3 N 4 Heterojunction photocatalysts.
The sample obtained in step 6) was subjected to SEM test, and as a result, as shown in FIG. 2, it was seen that the sample had a spherical structure with a diameter of about 500 nm.
TEM test and HRTEM test are carried out on the sample obtained in the step 6), and the result is shown in fig. 3 and 4, wherein the lattice spacing is 0.35nm, corresponding to TiO 2 The spherical particles are composed of CNS-TiO of nanometer scale 2 And g-C 3 N 4 And (5) compounding.
Example 3
Carbon nitrogen sulfur co-doped CNS-TiO 2 /g-C 3 N 4 The heterojunction photocatalyst is prepared by the following method: (molar ratio of thiourea to melamine is 2:1)
1. Slowly dripping 6mL of tetrabutyl titanate into a mixed solution of 15mL of deionized water and 15mL of ethanol in an ice bath, marking the mixed solution as a solution A, maintaining the temperature of about 0 ℃, and magnetically stirring for 12h;
2. weighing 0.4626g of melamine, adding the melamine into the stirred solution A, and carrying out ultrasonic vibration at room temperature for 30min to obtain solution B;
3. weighing 0.3350g of thiourea to be dissolved in the solution B, and carrying out ultrasonic oscillation again for 10min to obtain a reaction mixed solution, and marking the reaction mixed solution as the solution C;
4. transferring the solution C into 50mL high-pressure reaction kettle with tetrafluoroethylene lining, placing the reaction kettle in an oven at 150 ℃ for hydrothermal reaction for 10h, and discarding supernatant to obtain precipitate which is CNS-TiO 2 /g-C 3 N 4 An intermediate;
5. CNS-TiO obtained in 4) 2 /g-C 3 N 4 Washing the intermediate with deionized water for 3 times and ethanol for 2 times, and then drying the intermediate in an oven at 80 ℃ for 2 hours;
6. the method of 5)The resulting dried CNS-TiO 2 /g-C 3 N 4 Placing the intermediate in a tube furnace, calcining for 4 hours in a nitrogen atmosphere at a high temperature of 350 ℃ to obtain CNS-TiO co-doped with carbon, nitrogen and sulfur 2 /g-C 3 N 4 Heterojunction photocatalysts.
The sample obtained in step 6) was subjected to SEM test, and as shown in FIG. 5, it can be seen that the sample had a spherical structure with a diameter of about 650 nm.
Example 4 Performance test
CNS-TiO prepared in example 1, example 2, example 3 2 /g-C 3 N 4 Heterojunction photocatalyst, g-C 3 N 4 (control) photocatalyst catalytic activity test was performed.
The testing process comprises the following steps: using 300W xenon lamp with 420nm cut-off filter as visible light source, using the above-mentioned prepared 20mgCNS-TiO 2 /g-C 3 N 4 Heterojunction photocatalyst, g-C 3 N 4 (control) was dispersed in a quartz reactor containing 50mL of methyl orange (20 mg/L) solution, respectively. The suspension was stirred in the dark for 45min to reach adsorption-desorption equilibrium, and then the reactor was irradiated vertically with visible light to degrade methyl orange. The results show that the amount of the photocatalyst (0.5:1, 1:1, 2:1) prepared by the method of the invention for degrading methyl orange in 60 minutes is g-C respectively 3 N 4 1.125 times, 1.25 times, 1.188 times, degradation rates of 0.04211min, respectively -1 Is g-C 3 N 4 Is 3.57 times as large as 0.06874min -1 Is g-C 3 N 4 5.83 times, 0.04344min -1 Is g-C 3 N 4 Is 3.68 times (as shown in figures 6 and 7).
Claims (9)
1. The carbon-nitrogen-sulfur co-doped heterojunction photocatalyst is characterized in that graphitized carbon nitride and carbon-nitrogen-sulfur co-doped titanium dioxide nano particles are prepared according to the molar ratio of 1:8, preparing a microsphere structure formed by compounding, wherein the microsphere structure comprises the following steps:
1) Dripping a titanium source into a mixed solution of water and ethanol, wherein the volume ratio of water to ethanol in the mixed solution is 1:1, placing the solution in an ice bath, stirring for 10-12 hours to obtain a solution A, wherein the temperature of the mixed solution is 0-4 ℃;
2) Adding melamine into the solution A obtained in the step 1), and carrying out ultrasonic oscillation to obtain a solution B, wherein the molar ratio of the added melamine to the titanium source added in the step 1) is 1:8, the time of ultrasonic oscillation is 30min, and the temperature of ultrasonic oscillation is room temperature;
3) Adding thiourea into the solution B obtained in the step 2), and carrying out ultrasonic oscillation to obtain a solution C, wherein the molar ratio of the added thiourea to the melamine added in the step 2) is 0.5-2:1, the time of ultrasonic oscillation is 10min, and the temperature of ultrasonic oscillation is room temperature;
4) Carrying out hydrothermal reaction on the solution C obtained in the step 3) at 130-170 ℃ to obtain a precipitate and obtain an intermediate;
5) Washing the intermediate obtained in the step 4), drying, and calcining for 4-5 hours under the conditions of protective atmosphere and 300-400 ℃ to obtain the heterojunction photocatalyst.
2. The method for preparing the heterojunction photocatalyst as claimed in claim 1, comprising the steps of:
1) Dripping a titanium source into a mixed solution of water and ethanol, wherein the volume ratio of water to ethanol in the mixed solution is 1:1, placing the solution in an ice bath, stirring for 10-12 hours to obtain a solution A, wherein the temperature of the mixed solution is 0-4 ℃;
2) Adding melamine into the solution A obtained in the step 1), and carrying out ultrasonic oscillation to obtain a solution B, wherein the molar ratio of the added melamine to the titanium source added in the step 1) is 1:8, the time of ultrasonic oscillation is 30min, and the temperature of ultrasonic oscillation is room temperature;
3) Adding thiourea into the solution B obtained in the step 2), and carrying out ultrasonic oscillation to obtain a solution C, wherein the molar ratio of the added thiourea to the melamine added in the step 2) is 0.5-2:1, the time of ultrasonic oscillation is 10min, and the temperature of ultrasonic oscillation is room temperature;
4) Carrying out hydrothermal reaction on the solution C obtained in the step 3) at 130-170 ℃ to obtain a precipitate and obtain an intermediate;
5) Washing the intermediate obtained in the step 4), drying, and calcining for 4-5 hours under the conditions of protective atmosphere and 300-400 ℃ to obtain the heterojunction photocatalyst.
3. The method according to claim 2, wherein the titanium source in step 1) is any one or more of titanium tetrachloride, tetrabutyl titanate, titanium isopropoxide, titanium sulfate and titanyl sulfate.
4. A method of preparation according to claim 3, wherein the titanium source is tetrabutyl titanate.
5. The method according to claim 2, wherein in step 4), the solution C is transferred to a high-pressure reaction kettle with a tetrafluoroethylene lining, and the reaction kettle is placed in an oven at 130-170 ℃ for hydrothermal reaction for 8-12h.
6. The method according to claim 5, wherein the hydrothermal reaction is carried out at 150℃for 10 hours.
7. The method according to claim 2, wherein the washing in step 5) is performed three times with deionized water and then twice with ethanol, and the drying is performed at 80 ℃ for 2 hours.
8. Use of the heterojunction photocatalyst of claim 1 in photodegradation of contaminants.
9. The use according to claim 8, characterized in that the contaminant is methyl orange.
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| CN113634270A (en) * | 2021-07-20 | 2021-11-12 | 长春理工大学 | Janus nanofiber heterojunction photocatalyst modified by carbon nitride nanosheets |
| CN114100664A (en) * | 2021-12-02 | 2022-03-01 | 塔里木大学 | C-TiO2/g-C3N4Composite photocatalytic material and its synthesis method |
| CN116747897B (en) * | 2023-08-16 | 2023-10-20 | 内蒙古工业大学 | C, N, S co-doped TiO 2 Acid etching g-C 3 N 4 Heterojunction photocatalyst |
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