CN111996613B - Preparation method of cerium dioxide-graphite phase carbon nitride photocatalyst fiber - Google Patents
Preparation method of cerium dioxide-graphite phase carbon nitride photocatalyst fiber Download PDFInfo
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- CN111996613B CN111996613B CN202010831866.2A CN202010831866A CN111996613B CN 111996613 B CN111996613 B CN 111996613B CN 202010831866 A CN202010831866 A CN 202010831866A CN 111996613 B CN111996613 B CN 111996613B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The invention discloses a preparation method of cerium dioxide-graphite phase carbon nitride photocatalyst fiber, which comprises the step of preparing CeO 2 Nanoparticles of urea reagent with CeO 2 Uniformly stirring nano particles, grinding the nano particles into powder, heating the powder to 450-650 ℃ for calcination treatment, cooling the powder to room temperature, grinding the powder to obtain cerium dioxide-graphite phase carbon nitride, adding polyethylene glycol terephthalate and the cerium dioxide-graphite phase carbon nitride into hexafluoroisopropanol in a mass ratio of 0.1-10.01-1, performing ultrasonic dispersion to prepare photocatalyst emulsion, performing electrostatic spinning by using the photocatalyst emulsion, putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, washing the product after the water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Description
Technical Field
The invention belongs to the technical field of textile engineering, and relates to a preparation method of cerium dioxide-graphite phase carbon nitride photocatalyst fibers.
Background
With the rapid development of global science and technology and the rapid progress of society, people rely on the exploitation of earth energy and the utilization of resources to create unequally economic wealth for the human society. While the science and technology brings wealth to human beings, along with the increasing demand of society for energy, increasingly serious environmental pollution and energy crisis come on. Environmental pollution and energy crisis become important problems to be urgently solved all over the world, so that the method is an efficient, quick, economic and environment-friendly treatment method, and the semiconductor photocatalysis technology is generated. Compared with the common treatment method, the technology has the advantages of rich material sources, simple preparation process, no secondary pollution to the environment and the like, and the technology is rapidly in the fields of sewage treatment and new energy development. g-C as a modern novel highly efficient visible light responsive photocatalytic material 3 N 4 The star material has the unique advantages of excellent Valence Band (VB) and Conduction Band (CB) positions, capability of being excited under visible light to carry out photocatalytic hydrogen production, simple and green preparation process, stable physical and chemical properties, wide precursor source, no secondary pollution and the like, and becomes a star material in the field of photocatalysis. But, in the same way, g-C 3 N 4 The material has the defects of small specific surface area, rapid recombination of photon-generated carriers, low quantum efficiency, low utilization rate of visible light, difficult recovery and the like, and also seriously influences the research prospect of the material in the field of photocatalysis.
Disclosure of Invention
The invention aims to provide a preparation method of a cerium dioxide-graphite phase carbon nitride photocatalyst fiber, and the prepared cerium dioxide-graphite phase carbon nitride photocatalyst fiber has larger specific surface area and visible light utilization rate and is convenient to recycle.
The technical scheme adopted by the invention is that the preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, preparationCeO 2 A nanoparticle;
and 4, performing electrostatic spinning by using the photocatalyst emulsion, putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, washing the product after the water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
The present invention is also technically characterized in that,
the specific process of step 1 is as follows:
step 1.1, preparing NaOH solution with the concentration of 0.1 g/mL-0.3 g/mL;
step 1.2, taking Ce (NO) 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 1-5 h, then putting the solution into a drying oven for drying, and finally taking out and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 50-70 ℃;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating to 500-600 ℃, calcining, cooling to room temperature, taking out and grinding into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
In step 1.2, ce (NO) 3 ) 3 ·6H 2 The mass ratio of O to NaOH solid in the NaOH solution is 1.74:12.
in the step 1.2, the solution is put into an oven to be dried, the drying temperature is 110-130 ℃, and the drying time is 2-30 h.
In the step 1.4, the heating rate during the calcination treatment is 3 ℃/min to 6 ℃/min, and the calcination treatment time is 1.5h to 2.5h.
In step 2, urea reagent and CeO 2 The mass ratio of the nano particles is 30.
In the step 2, the heating rate during the calcination treatment is 3-6 ℃/min, and the calcination treatment time is 1.5-2.5 h.
In the step 3, the solid-to-liquid ratio of the polyethylene terephthalate to the hexafluoroisopropanol in the photocatalyst emulsion is 0.5-50 g:3 to 300mL.
In step 4, the electrostatic spinning parameters are as follows: the voltage is 10-15 kV, the spinning speed is 0.1-2 mL/h, and the receiving distance is 10-50 cm.
And step 4, putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 0.4-40 g/L, the concentration of CTAB in the aqueous solution is 0.04-4 g/L, the temperature of the water bath is 60-70 ℃, and the time of the water bath is 0.5-5 hours.
The beneficial effect of the invention is that CeO 2 The nano particles are combined with a urea reagent to generate the cerium oxide-graphite phase carbon nitride heterojunction photocatalyst, so that the migration and separation efficiency of a photon-generated carrier of a composite system is improved, the rapid recombination of photon-generated electron hole pairs is reduced, and the bulk phase g-C is further improved 3 N 4 The quantum efficiency and the visible light utilization rate of the quantum are overcome, and the pure phase g-C is overcome 3 N 4 The prepared cerium oxide-graphite phase carbon nitride heterojunction photocatalyst fiber has larger specific surface area and quantum efficiency and is easy to recycle.
Drawings
FIG. 1 is a low power transmission electron microscope image of cerium oxide nanotubes (CeNT);
FIG. 2 is a high transmission electron microscope image of cerium oxide nanotubes (CeNT);
FIG. 3 is a low power transmission electron microscope photograph of the ceria-graphite phase carbon nitride prepared in example 1 of the present invention;
FIG. 4 is a high-power transmission electron microscope photograph of the ceria-graphite phase carbon nitride prepared in example 1 of the present invention;
FIG. 5 is a graph showing the degradation activity of the cerium oxide-graphite phase carbon nitride prepared in examples 1 to 5 of the present invention against rose bengal B under visible light irradiation;
FIG. 6 is a first order kinetic fit graph of the degradation of rose bengal B under visible light irradiation of the ceria-graphite phase carbon nitride prepared in examples 1-5 of the present invention;
FIG. 7 is a graph showing the degradation rate of rose bengal B under visible light irradiation by the ceria-graphite phase carbon nitride prepared in examples 1 to 5 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of cerium dioxide-graphite phase carbon nitride photocatalyst fiber, which comprises the following steps:
step 1, ceO preparation 2 Nanoparticles
Step 1.1, preparing NaOH solution with the concentration of 0.1 g/mL-0.3 g/mL;
step 1.2, taking Ce (NO) 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 0.5-5h 3 ) 3 ·6H 2 The mass ratio of O to NaOH in the NaOH solution is 1.74:12, then putting the solution into an oven for drying at the temperature of 110-130 ℃ for 2-30 h, and finally taking out and grinding the solution into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 50-70 ℃;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible to 500-600 ℃ from room temperature at a heating rate of 3-6 ℃/min, calcining the alumina crucible for 1.5-2.5 h, cooling the alumina crucible to room temperature, taking out the alumina crucible and grinding the alumina crucible into nano-particles to obtain CeO 2 And (3) nanoparticles.
the solid-to-liquid ratio of the polyethylene terephthalate to the hexafluoroisopropanol in the photocatalyst emulsion is 0.5-50 g:3 to 300mL.
And 4, performing electrostatic spinning by using the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 10-15 kV, the spinning speed is 0.1-2 mL/h, and the receiving distance is 10-50 cm; then putting the electrostatic spinning product into an aqueous solution formed by NaOH and CTAB (cetyl trimethyl ammonium bromide) to carry out water bath heating, wherein the concentration of NaOH in the aqueous solution is 0.4-40 g/L, the concentration of CTAB is 0.04-4 g/L, the temperature of the water bath is 60-70 ℃, and the time of the water bath is 0.5-5 h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Example 1
The preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, preparation of CeO 2 Nanoparticles
Step 1.1, putting 12g of flake NaOH into 60mL of deionized water, and stirring to completely dissolve the NaOH to prepare NaOH solution;
step 1.2, 1.74g of Ce (NO) is taken 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 2h, then putting the beaker containing the solution into an oven for drying, heating to 120 ℃ at the speed of 2.3 ℃/min, then preserving heat for 24h, finally taking out the solid in the beaker, and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 60 ℃ for 12 hours;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible to 550 ℃ from room temperature at the heating rate of 4.6 ℃/min, calcining the alumina crucible for 2 hours, and cooling the alumina crucible to room temperatureTaking out and grinding into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
and 4, carrying out electrostatic spinning by adopting the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 10kV, the spinning speed is 1mL/h, and the receiving distance is 10cm; putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 0.5g/L, the concentration of CTAB is 0.04g/L, the temperature of the water bath is 60 ℃, and the time of the water bath is 1h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Fig. 1 and 2 are low-power and high-power transmission electron micrographs of cerium oxide nanotubes (CeNT), respectively, and the clear morphology of the cerium oxide nanotubes can be clearly seen from fig. 1 and 2. FIG. 3 is a low transmission electron microscope photograph of the ceria-graphite phase carbon nitride prepared in example 1 of the present invention, in which CeO is shown as a black region in FIG. 3 2 Nanoparticles with grey areas of g-C 3 N 4 Nanoparticles, as can be seen in FIG. 3, ceO was present in the ceria-graphite phase carbon nitride prepared in example 1 2 The particle size of the nano-particles is about 20nm 2 And g-C 3 N 4 The surfaces of the nano particles are tightly connected together to form a semiconductor heterojunction structure, and the surfaces of the nano particles are tightly connected, so that the charge transfer efficiency is accelerated, and the photocatalytic activity of the material is improved. FIG. 4 is a cerium oxide-graphite prepared in example 1 of the present inventionFIG. 4 is a high-power transmission electron micrograph of phase carbonitride showing CeO in the ceria-graphite phase carbonitride 2 The internal lattice structure is measured at a place with a clear image, and the interplanar spacing d =0.31nm can be obtained, corresponding to CeO 2 The (111) crystal plane of (a).
Example 2
The preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, preparation of CeO 2 Nanoparticles
Step 1.1, putting 10g of flake NaOH into 50mL of deionized water, and stirring to completely dissolve the NaOH to prepare NaOH solution;
step 1.2, 1.45g of Ce (NO) is taken 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 0.5h, then putting the beaker containing the solution into an oven for drying, heating to 110 ℃ at the speed of 2.5 ℃/min, then preserving heat for 20h, finally taking out the solid in the beaker, and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 50 ℃ for 12 hours;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible from room temperature to 500 ℃ at the heating rate of 3 ℃/min, calcining the alumina crucible for 2 hours, cooling the alumina crucible to the room temperature, taking out the alumina crucible and grinding the alumina crucible into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
and 4, performing electrostatic spinning by using the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 12kV, the spinning speed is 0.5mL/h, and the receiving distance is 20cm; putting the electrostatic spinning product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 10g/L, the concentration of CTAB is 2g/L, the temperature of the water bath is 65 ℃, and the time of the water bath is 0.5h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Example 3
The preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, ceO preparation 2 Nanoparticles
Step 1.1, putting 10g of flake NaOH into 100mL of deionized water, and stirring to completely dissolve the NaOH to prepare NaOH solution;
step 1.2, 1.45g of Ce (NO) is taken 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 3h, then putting the beaker containing the solution into an oven for drying, heating to 120 ℃ at the speed of 2 ℃/min, then preserving heat for 24h, finally taking out the solid in the beaker, and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 55 ℃ for 12 hours;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible from room temperature to 570 ℃ at the heating rate of 5 ℃/min, calcining the alumina crucible for 2 hours, cooling the alumina crucible to the room temperature, taking out the alumina crucible and grinding the alumina crucible into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
and 4, carrying out electrostatic spinning by adopting the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 13kV, the spinning speed is 1.5mL/h, and the receiving distance is 20cm; putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 10g/L, the concentration of CTAB is 2.5g/L, the temperature of the water bath is 65 ℃, and the time of the water bath is 3h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Example 4
The preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, ceO preparation 2 Nanoparticles
Step 1.1, putting 30g of flake NaOH into 100mL of deionized water, and stirring to completely dissolve NaOH to prepare NaOH solution;
step 1.2, 43.5g of Ce (NO) is taken 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 4h, then putting the beaker containing the solution into an oven for drying, heating to 130 ℃ at the speed of 2.3 ℃/min, then preserving heat for 24h, finally taking out the solid in the beaker, and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 60 ℃ for 15 hours;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible from room temperature to 580 ℃ at the heating rate of 5 ℃/min, calcining the alumina crucible for 2.3 hours, cooling the alumina crucible to the room temperature, taking out the alumina crucible and grinding the alumina crucible into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
and 4, carrying out electrostatic spinning by adopting the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 14kV, the spinning speed is 1.8mL/h, and the receiving distance is 40cm; putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 25g/L, the concentration of CTAB is 3g/L, the temperature of the water bath is 68 ℃, and the time of the water bath is 4h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
Example 5
The preparation method of the cerium dioxide-graphite phase carbon nitride photocatalyst fiber comprises the following steps:
step 1, ceO preparation 2 Nanoparticles
Step 1.1, putting 12g of flake NaOH into 60mL of deionized water, and stirring to completely dissolve the NaOH to prepare NaOH solution;
step 1.2, 1.74g of Ce (NO) is taken 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 2h, then putting the beaker containing the solution into an oven for drying, heating to 120 ℃ at the speed of 2.3 ℃/min, then preserving heat for 24h, finally taking out the solid in the beaker, and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 60 ℃ for 12 hours;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating the alumina crucible to 550 ℃ from room temperature at the heating rate of 4.6 ℃/min, calcining the alumina crucible for 2 hours, cooling the alumina crucible to the room temperature, taking out the alumina crucible and grinding the alumina crucible into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
and 3, adding the polyethylene terephthalate and the cerium dioxide-graphite phase carbon nitride in a mass ratio of 5 into hexafluoroisopropanol together, and performing ultrasonic dispersion to prepare a photocatalyst emulsion, wherein the solid-to-liquid ratio of the polyethylene terephthalate to the hexafluoroisopropanol in the photocatalyst emulsion is 5g:6mL;
and 4, carrying out electrostatic spinning by adopting the photocatalyst emulsion, wherein the electrostatic spinning parameters are as follows: the voltage is 10kV, the spinning speed is 1mL/h, and the receiving distance is 50cm; putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, wherein the concentration of NaOH in the aqueous solution is 40g/L, the concentration of CTAB is 4g/L, the temperature of the water bath is 70 ℃, and the time of the water bath is 5h; and washing the product after water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber.
FIG. 5 is a graph showing the degradation activity of the ceria-graphite phase carbon nitride prepared in examples 1 to 5 of the present invention under visible light irradiation on Rose Bengal B, which is an organic pollutant RhB, and it can be seen from the graph that the degradation rate and the final degradation efficiency of the ceria-graphite phase carbon nitride prepared in the present application on the organic pollutant RhB are much higher than those of pure CeO after 120min degradation 2 (i.e., ceria nanotubes CeNT).
FIG. 6 is a first order kinetic fit graph of Rose Bengal B degradation under visible light irradiation for the ceria-graphite phase carbon nitrides prepared in examples 1-5 of the present invention, from which it can be seen that-ln (C/C) of the ceria-graphite phase carbon nitrides prepared in examples 1-5 0 ) Linear with illumination time, -ln (C/C) 0 ) Is an equation of reaction kinetics, showing that the photocatalytic reaction of the ceria-graphite phase carbon nitride prepared in examples 1-5 conforms to a first order kinetic model.
FIG. 7 is a graph showing the degradation rate of rose bengal B under visible light irradiation for the ceria-graphite phase carbon nitride prepared in examples 1 to 5 of the present invention, in which a represents pure CeO 2 B represents the ceria-graphite phase carbon nitride prepared in example 1, c represents the ceria-graphite phase carbon nitride prepared in example 2, d represents the ceria-graphite phase carbon nitride prepared in example 3, e represents the ceria-graphite phase carbon nitride prepared in example 4, and f represents the ceria-graphite phase carbon nitride prepared in example 5, from which it can be seen that pure CeO 2 The degradation rate of rose bengal B under visible light irradiation was about 9%, the degradation rate of the ceria-graphite phase carbon nitride prepared in example 1 under visible light irradiation was about 83%, the degradation rate of the ceria-graphite phase carbon nitride prepared in example 2 under visible light irradiation was about 91%, the degradation rate of the ceria-graphite phase carbon nitride prepared in example 3 under visible light irradiation was about 100%, the degradation rate of the ceria-graphite phase carbon nitride prepared in example 4 under visible light irradiation was about 75%, and the degradation rate of the ceria-graphite phase carbon nitride prepared in example 5 under visible light irradiation was about 62%. CeO is clearly shown therein 2 /g-C 3 N 4 The degradation rate is faster than that of pure CeO 2 The ceria-graphite phase carbon nitride prepared in example 3 has the fastest degradation rate, the highest degradation efficiency and the best photocatalytic activity. The ceria-graphite phase carbon nitride prepared in example 3 exhibited the highest degradation rate with a degradation rate constant of: k =0.035min -1 Is pure CeO 2 The degradation rate constant of the reagent is 21 times, and the highest photocatalytic activity is shown.
Claims (9)
1. A preparation method of a cerium dioxide-graphite phase carbon nitride photocatalyst fiber is characterized by comprising the following steps:
step 1, preparation of CeO 2 A nanoparticle;
step 2, mixing urea reagent with CeO 2 The nano particles are evenly stirred and then ground into powderHeating the powder to 450-650 ℃ for calcination treatment, cooling to room temperature, and grinding to powder to obtain cerium dioxide-graphite phase carbon nitride;
step 3, adding polyethylene glycol terephthalate and cerium dioxide-graphite phase carbon nitride into hexafluoroisopropanol in a mass ratio of 0.1-10;
step 4, performing electrostatic spinning by using the photocatalyst emulsion, putting the product into an aqueous solution formed by NaOH and CTAB for water bath heating, washing the product after the water bath heating by using deionized water and absolute ethyl alcohol, and finally drying to obtain the cerium dioxide-graphite phase carbon nitride photocatalyst fiber;
the specific process of the step 1 is as follows:
step 1.1, preparing NaOH solution with the concentration of 0.1 g/mL-0.3 g/mL;
step 1.2, taking Ce (NO) 3 ) 3 ·6H 2 Adding O into the NaOH solution prepared in the step 1.1, stirring for 1-5 h, then putting the solution into a drying oven for drying, and finally taking out and grinding into powder;
step 1.3, washing the powder prepared in the step 1.2 to be neutral by using deionized water and alcohol, and drying the washed powder at 50-70 ℃;
step 1.4, placing the dried powder in an alumina crucible, placing the alumina crucible in a muffle furnace, heating to 500-600 ℃, calcining, cooling to room temperature, taking out and grinding into nano-scale particles to obtain CeO 2 And (3) nanoparticles.
2. The method of claim 1, wherein in step 1.2, ce (NO) is added 3 ) 3 ·6H 2 The mass ratio of O to NaOH solid in the NaOH solution is 1.74:12.
3. the method for preparing a ceria-graphite phase carbon nitride photocatalyst fiber according to claim 1, wherein in the step 1.2, the solution is dried in an oven, wherein the drying temperature is 110 to 130 ℃, and the drying time is 20 to 30 hours.
4. The method for preparing a ceria-graphite phase carbon nitride photocatalyst fiber according to claim 1, wherein in the step 1.4, the temperature rise rate during the calcination treatment is 3 ℃/min to 6 ℃/min, and the calcination treatment time is 1.5h to 2.5h.
5. The method of claim 1, wherein in step 2, the urea reagent and CeO are added 2 The mass ratio of the nano particles is 30.
6. The method for preparing a ceria-graphite phase carbon nitride photocatalyst fiber as claimed in claim 5, wherein in the step 2, the temperature rise rate during the calcination treatment is 3 ℃/min to 6 ℃/min, and the calcination treatment time is 1.5h to 2.5h.
7. The method for preparing a ceria-graphite phase carbon nitride photocatalyst fiber as claimed in claim 6, wherein in the step 3, the solid-to-liquid ratio of polyethylene terephthalate to hexafluoroisopropanol in the photocatalyst emulsion is 0.5 to 50g:3 to 300mL.
8. The method of claim 7, wherein in step 4, the electrospinning parameters are as follows: the voltage is 10-15 kV, the spinning speed is 0.1-2 mL/h, and the receiving distance is 10-50 cm.
9. The method for preparing a ceria-graphite phase carbon nitride photocatalyst fiber as claimed in claim 7, wherein, in the step 4, the product is put into an aqueous solution formed by NaOH and CTAB to be heated in a water bath, the concentration of NaOH in the aqueous solution is 0.4-40 g/L, the concentration of CTAB is 0.04-4 g/L, the temperature of the water bath is 60-70 ℃, and the time of the water bath is 0.5-5 hours.
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