CN115999603A - Method for constructing graphite phase carbon nitride/bismuth tungstate nano heterojunction - Google Patents
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 16
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 16
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 16
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction, which is prepared by using Bi based on an electrostatic spinning technology 2 WO 6 The nanofiber is taken as a substrate, and urea is combined with a gas-solid reaction method to form a gas precursor in Bi 2 WO 6 In situ generation of g-C on the surface of nanofibers 3 N 4 A nano-sheet. The graphite-phase carbon nitride/bismuth tungstate nano heterojunction prepared by the method has obviously better energy band structure and light response characteristic, and the unique nanofiber network structure increases the reaction sites contacted with pollutants, so that organic pollutants in water can be efficiently degraded.
Description
Technical Field
The invention relates to the field of photocatalytic material, in particular to a method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction.
Background
Currently, energy crisis caused by unstable fossil fuel depletion and supply is increasingly receiving attention. Meanwhile, rapid developments in cities and industry introduce many pollutants into the environment, particularly in water bodies, causing water pollution. Therefore, development of a technology for treating wastewater using clean energy is urgently required. The photocatalysis technology is a technology for carrying out sustainable degradation on pollutants by utilizing solar energy. The photocatalyst is certainly the core of photocatalysis, so the design, construction and modification of the photocatalyst are one of the hot spots of research. Among various novel photocatalysts, bi 2 WO 6 The band gap is narrow, and the valence and conduction band positions are suitable. To overcome Bi 2 WO 6 The self-existing defects of high photo-generated electron-hole recombination speed, short service life and the like are overcome, and people try to combine the self-existing defects with graphite phase carbon nitride (g-C 3 N 4 ) Coupling forms a heterojunction, which benefits from g-C 3 N 4 With Bi 2 WO 6 Has a well-matched energy band structure, g-C 3 N 4 With Bi 2 WO 6 The formed heterostructure can effectively reduce the recombination of photo-generated electron-hole pairs, so that the photocatalysis efficiency is greatly improved.
So far, the construction of g-C is common 3 N 4 With Bi 2 WO 6 The heterojunction method includes coprecipitation method, hydrothermal method, mixed electrostatic spinning method, etc. Wherein, the physical mixing mode of the coprecipitation method is difficult to construct a stable heterostructure; g-C grown by hydrothermal method 3 N 4 The space distribution is uneven, and the photocatalytic activity is affected; mixed electrostatic spinning method, g-C 3 N 4 Is embedded in Bi 2 WO 6 Inside, a large number of active sites are wasted. In summary, these current conventional methods of constructing heterojunctions generally result in a non-uniform spatial distribution of the solid precursor, g-C 3 N 4 With Bi 2 WO 6 The lack of interface contact is provided by the lack of interface contact,barrier g-C 3 N 4 Is a growth of aggregates of (a) in the culture medium. These problems restrict g-C 3 N 4 With Bi 2 WO 6 The formation of heterojunction also affects its stability and efficiency in terms of photocatalysis, and it can be seen that a new g-C must be built 3 N 4 With Bi 2 WO 6 The coupling mode of the heterojunction improves the photocatalysis performance of the heterojunction.
Disclosure of Invention
The invention aims to provide a method for conveniently, homogeneously and efficiently constructing a graphite-phase carbon nitride/bismuth tungstate nano heterojunction based on an electrostatic spinning technology and a gas-solid reaction method.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method comprises the following steps:
1) Configuration Bi 2 WO 6 Spinning solution
Dissolving 0.01 mol of citric acid in 7 mL deionized water, adding 3 mL mol of hydrochloric acid and 0.02 mol of Bi (NO) 3 ) 3 ·5H 2 O, continuously stirring to obtain Bi (NO) 3 ) 3 A solution; will 0.01 mol Na 2 WO 4 ·2H 2 O is dissolved in 10ml deionized water to obtain Na 2 WO 4 A solution; subsequently, na was added under continuous magnetic stirring 2 WO 4 Slowly drop-wise adding the solution to Bi (NO) 3 ) 3 Adding the mixed solution of 6 mL into a solvent which uses PVP-ethanol solution (2.0 g: 20 mL) as a polymer, and magnetically stirring for 10-12 h to obtain Bi 2 WO 6 Spinning solution;
2) Preparation of Bi by electrostatic spinning 2 WO 6 Nanofiber
Transferring 20 mL spinning solution into a 20 mL injector (with 20-gauge stainless steel needle), taking a roller covered with aluminum foil as a collecting device, applying a positive voltage of 25-30 kilovolts to the needle and a negative voltage of 5 kilovolts to the roller, keeping the rotating speed of the roller at 500-550 r/min, and pushing the injector2.0-3.0 mL/h, heating the collected fiber to 480-500 ℃ in a muffle furnace at a heating rate of 1 ℃/min after spinning, preserving heat for 1.5-2 h, and finally naturally cooling to room temperature to obtain Bi 2 WO 6 A nanofiber;
3) g-C is prepared by adopting a gas-solid method 3 N 4 nanoplatelets/Bi 2 WO 6 Nanometer heterojunction
Uniformly spreading urea powder of 0.5-3 g on the bottom of a crucible, and uniformly spreading Bi of 100 mg 2 WO 6 The nanofiber is paved on a 20-mesh titanium net, a titanium net support is placed on urea powder at intervals of 5 mm, a crucible is sealed by aluminum foil and covered, then the crucible is placed in a muffle furnace, the temperature is increased to 480-500 ℃ at the heating rate of 2 ℃/min, the temperature is kept for 1.5-2 h, and the g-C is obtained after natural cooling 3 N 4 nanoplatelets/Bi 2 WO 6 A nano heterojunction.
The invention adopts the technical proposal, and uses Bi prepared based on electrostatic spinning technology 2 WO 6 The nanofiber is taken as a substrate, and urea is combined with a gas-solid reaction method to form a gas precursor in Bi 2 WO 6 In situ generation of g-C on the surface of nanofibers 3 N 4 The nano-sheet has the advantages that: bi prepared by electrostatic spinning method 2 WO 6 The open network and the high specific area of the nanofiber are beneficial to the diffusion of urea molecules, and then the urea molecules are uniformly adsorbed on Bi in the form of single gas molecules through intermolecular interaction 2 WO 6 Surface, finally grow into uniform g-C in situ 3 N 4 A layer coated on Bi 2 WO 6 g-C prepared by adopting the gas-solid reaction method on a matrix 3 N 4 The nanoplatelets have a more uniform spatial distribution with Bi 2 WO 6 Constructed g-C 3 N 4 nanoplatelets/Bi 2 WO 6 Compared with the heterojunction prepared by other traditional modes, the nanofiber homogeneous heterostructure has obviously better energy band structure and light response characteristic, and the unique nanofiber reticular structure increases the reaction sites of the nanofiber homogeneous heterostructure contacted with pollutants, so that organic pollutants in water can be efficiently degraded.
Drawings
FIG. 1 shows the synthesis of g-C by the method of the present invention 3 N 4 nanoplatelets/Bi 2 WO 6 Infrared spectrum of nanofiber heterojunction.
FIG. 2 shows the synthesis of g-C by the method of the present invention 3 N 4 nanoplatelets/Bi 2 WO 6 Microcosmic morphology structure of nanofiber heterojunction.
FIG. 3 shows the synthesis of g-C by the method of the present invention 3 N 4 nanoplatelets/Bi 2 WO 6 Effect of nanofiber heterojunction to degrade tetracycline.
Detailed Description
Example 1
A method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method comprises the following steps:
1) Configuration Bi 2 WO 6 Spinning solution
Dissolving 0.01 mol of citric acid in 7 mL deionized water, adding 3 mL mol of hydrochloric acid and 0.02 mol of Bi (NO) 3 ) 3 ·5H 2 O, continuously stirring to obtain Bi (NO) 3 ) 3 A solution; will 0.01 mol Na 2 WO 4 ·2H 2 O is dissolved in 10mL deionized water to obtain Na 2 WO 4 A solution; subsequently, na was added under continuous magnetic stirring 2 WO 4 Slowly drop-wise adding the solution to Bi (NO) 3 ) 3 Adding 6 mL mixed solution into solvent containing PVP-ethanol solution (2.0 g:20 mL) as polymer, and magnetically stirring 12 h to obtain Bi 2 WO 6 Spinning solution;
2) Preparation of Bi by electrostatic spinning 2 WO 6 Nanofiber
Transferring 20 mL spinning solution into 20 mL syringe (equipped with 20 # stainless steel needle), collecting with aluminum foil covered roller as collecting device, keeping distance between needle and roller at 20 cm, applying 30 KV positive voltage to needle, applying 5 KV negative voltage to roller, maintaining roller rotation speed at 500 r/min, pushing the syringe at 3.0mL/h, heating collected fiber to 500 deg.C in muffle furnace at 1 deg.C/min, and maintaining temperature for 2%h, finally naturally cooling to room temperature to obtain Bi 2 WO 6 A nanofiber;
3) g-C is prepared by adopting a gas-solid method 3 N 4 nanoplatelets/Bi 2 WO 6 Nanometer heterojunction
The urea powder of 0.2. 0.2 g was uniformly spread on the bottom of the crucible, and 100 mg Bi was added 2 WO 6 Spreading the nanofibers on 20 mesh titanium mesh, placing titanium mesh supports on urea powder at intervals of 5 mm, sealing the crucible with aluminum foil, covering, placing the crucible in a muffle furnace, heating to 500 deg.C at a heating rate of 2 deg.C/min, maintaining the temperature for 2h, and naturally cooling to obtain g-C 3 N 4 nanoplatelets/Bi 2 WO 6 A nano heterojunction.
Example 2
A method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method comprises the following steps:
1) Configuration Bi 2 WO 6 Spinning solution
Dissolving 0.01 mol of citric acid in 7 mL deionized water, adding 3 mL mol of hydrochloric acid and 0.02 mol of Bi (NO) 3 ) 3 ·5H 2 O, continuously stirring to obtain Bi (NO) 3 ) 3 A solution; will 0.01 mol Na 2 WO 4 ·2H 2 O is dissolved in 10mL deionized water to obtain Na 2 WO 4 A solution; subsequently, na was added under continuous magnetic stirring 2 WO 4 Slowly drop-wise adding the solution to Bi (NO) 3 ) 3 Adding 6 mL mixed solution into solvent containing PVP-ethanol solution (2.0 g:20 mL) as polymer, and magnetically stirring for 10 hr to obtain Bi 2 WO 6 Spinning solution;
2) Preparation of Bi by electrostatic spinning 2 WO 6 Nanofiber
Transferring 20 mL spinning solution into 20 mL syringe (equipped with 20 # stainless steel needle), taking aluminum foil covered roller as collecting device, with distance between needle and roller of 25 cm, applying 25 kv positive voltage to needle, applying 5 kv negative voltage to roller, maintaining roller rotation speed of 550 r/min, syringe pushing speed of 2.0 mL/h,after spinning, heating the collected fiber to 480 ℃ in a muffle furnace at a heating rate of 1 ℃/min, preserving heat for 1.5 h, and naturally cooling to room temperature to obtain Bi 2 WO 6 A nanofiber;
3) g-C is prepared by adopting a gas-solid method 3 N 4 nanoplatelets/Bi 2 WO 6 Nanometer heterojunction
The urea powder of 0.15. 0.15 g was uniformly spread on the bottom of the crucible, and 100 mg Bi was added 2 WO 6 Spreading the nanofibers on 20 mesh titanium mesh, placing titanium mesh supports on urea powder at intervals of 5 mm, sealing the crucible with aluminum foil, covering, placing the crucible in a muffle furnace, heating to 480 deg.C at a heating rate of 2 deg.C/min, maintaining the temperature of 1.5 h, and naturally cooling to obtain g-C 3 N 4 nanoplatelets/Bi 2 WO 6 A nano heterojunction.
Example 3
g-C 3 N 4 nanoplatelets/Bi 2 WO 6 Photocatalytic performance of nanofiber heterojunction materials
The photocatalytic activity of the samples was evaluated by degradation of the tetracycline solution under simulated visible light irradiation. The visible light source used a 350W band filter (UV filtered) xenon lamp with an initial tetracycline concentration of 30 ppm. Before the reaction started, 0.1. 0.1 g photocatalyst (g-C 3 N 4 nanoplatelets/Bi 2 WO 6 Nano heterojunction) is dispersed in 100 mL tetracycline solution, magnetically stirred in the dark for 40 minutes, and placed under visible light irradiation after reaching adsorption-desorption equilibrium. During the whole reaction, magnetic stirring was continued, 3 mL suspensions were withdrawn with a syringe every 40 minutes, filtered through a 0.22 μm filter membrane, and the absorption value of the solution was measured at 357 nm with an ultraviolet spectrophotometer, and the degradation efficiency of the sample was calculated.
The results were as follows:
(1) After 160 min of reaction without photocatalyst, tetracycline was hardly degraded.
(2) Adding pure Bi 2 WO 6 Under the conditions of (1) and (b) after 160 min of reaction, the tetracycline degradation efficiency was 49.2%.
(3) After adding pure g-C 3 N 4 Under the conditions of (1) and (b) after 160 min of reaction, the tetracycline degradation efficiency is 52.6%.
(4) After adding g-C prepared in example 1 of the present invention 3 N 4 nanoplatelets/Bi 2 WO 6 Under the condition of nano heterojunction, after 160 min of reaction, the tetracycline degradation efficiency reaches 88.5%.
The above results illustrate the g-C constructed according to the present invention 3 N 4 nanoplatelets/Bi 2 WO 6 The nanofiber heterojunction has obviously enhanced photocatalytic degradation performance.
Claims (7)
1. The method for constructing the graphite-phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method is characterized by comprising the following steps of:
1) Configuration Bi 2 WO 6 Spinning solution
2) Preparation of Bi by electrostatic spinning 2 WO 6 Nanofiber
Bi is taken 2 WO 6 Transferring the spinning solution into an injector with a stainless steel needle, adopting a roller covered with aluminum foil as a collecting device, enabling the distance between the needle and the roller to be 20-25 cm, applying a positive voltage of 25-30 kilovolts to the needle, applying a negative voltage of 5 kilovolts to the roller, keeping the rotating speed of the roller to be 500-550 r/min, enabling the pushing speed of the injector to be 2.0-3.0 mL/h, heating the collected fiber to 480-500 ℃ in a muffle furnace at a heating rate of 1 ℃/min after spinning, preserving heat for 1.5-2 h, and finally cooling to room temperature to obtain Bi 2 WO 6 A nanofiber;
3) g-C is prepared by adopting a gas-solid method 3 N 4 nanoplatelets/Bi 2 WO 6 Nanometer heterojunction
Uniformly spreading urea powder at the bottom of a crucible, spreading nanofibers on a titanium mesh serving as a bracket, placing the titanium mesh on the urea powder at intervals, sealing the crucible with aluminum foil, covering, placing the crucible in a muffle furnace, heating to 480-500 ℃, preserving heat for 1.5-2 h, and naturally cooling to obtain g-C 3 N 4 nanoplatelets/Bi 2 WO 6 A nano heterojunction.
2. The method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by electrospinning-gas-solid method as in claim 1, wherein in step 1), said Bi 2 WO 6 The preparation method of the spinning solution comprises the following steps: dissolving 0.01 mol of citric acid in 7 mL deionized water, adding 3 mL mol of hydrochloric acid and 0.02 mol of Bi (NO) 3 ) 3 ·5H 2 O, continuously stirring to obtain Bi (NO) 3 ) 3 A solution; will 0.01 mol Na 2 WO 4 ·2H 2 O is dissolved in 10mL deionized water to obtain Na 2 WO 4 A solution; subsequently, na was added under continuous magnetic stirring 2 WO 4 Slowly drop-wise adding the solution to Bi (NO) 3 ) 3 Adding the mixed solution of 6 mL into PVP-ethanol solution, magnetically stirring for 10-12 h to obtain Bi 2 WO 6 Spinning solution.
3. The method for constructing the graphite-phase carbon nitride/bismuth tungstate nano heterojunction by the electrostatic spinning-gas-solid method as claimed in claim 2, wherein the ratio of the mixed solution to the PVP-ethanol solution is 6 mL:2.0 g:20 mL.
4. The method for constructing a graphite-phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method as claimed in claim 1, wherein in the step 2), the heating rate of the fiber is 1 ℃/min.
5. The method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by electrostatic spinning-gas-solid method as claimed in claim 1, wherein in step 3), urea powder and Bi 2 WO 6 The mass ratio of the nanofibers is 0.5-3 g:100 mg.
6. The method for constructing a graphite phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method as claimed in claim 1, wherein in the step 3), the titanium mesh is a 20 mesh titanium mesh, and a spacing distance between the titanium meshes is 5 mm.
7. The method for constructing a graphite-phase carbon nitride/bismuth tungstate nano heterojunction by an electrostatic spinning-gas-solid method as claimed in claim 1, wherein in the step 3), the heating rate is 2 ℃/min.
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