CN105148974A - High-activity mpg-C3N4/RE-BiVO4 heterojunction photocatalyst and preparation method and application thereof - Google Patents

High-activity mpg-C3N4/RE-BiVO4 heterojunction photocatalyst and preparation method and application thereof Download PDF

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CN105148974A
CN105148974A CN201510638348.8A CN201510638348A CN105148974A CN 105148974 A CN105148974 A CN 105148974A CN 201510638348 A CN201510638348 A CN 201510638348A CN 105148974 A CN105148974 A CN 105148974A
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mpg
bivo
heterojunction photocatalyst
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CN105148974B (en
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谈国强
罗洋洋
董国华
刘婷
任慧君
夏傲
王通
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Shaanxi University of Science and Technology
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Abstract

The invention discloses high-activity mpg-C3N4/RE-BiVO4 heterojunction photocatalyst and a preparation method and application thereof. First, mpg-C3N4 powder is prepared and dispersed into ethyl alcohol; then a bismuth nitrate pentahydrate solution and an ammonium metavanadate solution are mixed, the pH value of the mixture is adjusted, rare earth nitrate is added, and then precursor RE-BiVO4 turbid liquid is obtained; then, an mpg-C3N4 alcoholic solution is added into the precursor RE-BiVO4 turbid liquid to obtain reaction precursor liquid, and finally a microwave hydrothermal method is adopted for preparing the mpg-C3N4/RE-BiVO4 heterojunction photocatalyst. The catalyst is of a heterojunction structure formed by mesporous mpg-C3N4 and rod-shaped tetragonal zircon phase RE-BiVO4, high photocatalytic activity is achieved under irradiation of simulated sunlight, the photocatalytic efficiency of pure-phase BiVO4 is greatly improved, and good application prospects in the aspect of treating environmental pollutants and others are achieved.

Description

A kind of high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst and its preparation method and application
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst and its preparation method and application.
Background technology
Deepen continuously along with industrialized, growing environmental problem has threatened the sustainable development of human society gradually.Conductor photocatalysis is the extraordinary selection of one solving these environmental problems, a kind of mode of green can be adopted directly to utilize sunshine degradation of contaminant because it means.Consider that photo-generated carrier has played main effect in photocatalytic process, the photochemical catalyst that activity is high should have wider spectral absorption scope and very high quantum yield.By the narrow gap semiconductor compound of two kinds of energy band couplings, the transfer of photo-generated carrier between the semiconductor of two kinds of compounds will improve quantum yield.
Graphite phase carbon nitride (mpg-C 3n 4) and BiVO 4it is the very popular narrow gap semiconductor photochemical catalyst of order first two research.Mpg-C 3n 4band gap width be 2.7eV, water-splitting hydrogen production and degradating organic dye all show excellent activity under visible light.In addition, mpg-C 3n 4large specific area and two dimensional surface conjugated structure make it be suitable as very much the matrix material of composite.BiVO 4energy gap be 2.4eV, have very strong visible absorption ability, simultaneously its nontoxicity and chemical stability make it become a kind of photochemical catalyst very with Practical significance.
Up to now, mpg-C is prepared 3n 4/ RE-BiVO 4there is not been reported in the work of heterojunction photocatalyst, also do not have patent and bibliographical information to cross preparation mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst.
Summary of the invention
The object of the present invention is to provide a kind of high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst and its preparation method and application, the method is simple to operate, and the reaction time is short, and reaction condition is gentle, the mpg-C of preparation 3n 4/ RE-BiVO 4heterojunction photocatalyst has high degrading activity, effectively can improve pure phase BiVO 4photocatalysis efficiency.
For achieving the above object, the technical solution used in the present invention is:
A kind of high activity mpg-C 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, comprises the following steps:
Step 1: be the melamine aqueous solution and the concentration of 2.1 ~ 2.15mol/L by concentration be the Nano-meter SiO_2 of 0.8 ~ 0.85mol/L 2the aqueous solution mixes for 3:2 by volume, stirs after ultrasonic disperse again, then dries, and obtains white solid, loads in crucible, at N by after white solid porphyrize 2be warming up to 540 ~ 560 DEG C of calcining 4h in atmosphere furnace, obtain pale yellow powder, then use NH 4hF 2aqueous corrosion pale yellow powder, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4it is even that powder joins ultrasonic disperse in ethanol, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is soluble in water, stirs, and obtains bismuth salting liquid; By NH 4vO 3be dissolved in hot water, heating stirs, and obtains vanadic salts solution;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, stirs, obtains mixed liquor, and the pH value regulating mixed liquor is 8, continues to stir;
Step 5: by RE (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, stir, obtain forerunner RE-BiVO 4suspension; Wherein RE (NO 3) 36H 2o is Nd (NO 3) 36H 2o or Nd (NO 3) 36H 2o and Er (NO 3) 36H 2the mixture of O, forerunner RE-BiVO 4in suspension, the mol ratio of RE and Bi is (10.52 ~ 11.11): 100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner RE-BiVO 4in suspension, first stir, then ultrasonic disperse, then continue to stir, obtain reaction precursor liquid; Mpg-C in reaction precursor liquid 3n 4be (0.8 ~ 1.2) with the mol ratio of V: 1;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 95 ~ 105 DEG C, insulation 7 ~ 9min; Then continue to be warming up to 145 ~ 155 DEG C, insulation 7 ~ 9min; Continue again to be warming up to 175 ~ 185 DEG C, after insulation 35 ~ 45min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, and washing, drying, obtain high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst.
In described step 1, the time of ultrasonic disperse is 55 ~ 65min;
In described step 2, the time of ultrasonic disperse is 1 ~ 4h;
In described step 6, the time of ultrasonic disperse is 1 ~ 2h.
Bake out temperature in described step 1 is 75 ~ 85 DEG C;
Programming rate in described step 1 is 2 ~ 3 DEG C/min.
Described NH 4hF 2the concentration of the aqueous solution is 3.5 ~ 4.5mol/L;
The concentration of described bismuth salting liquid and vanadic salts solution is 0.35 ~ 0.45mol/L.
Required time that stirs in described step 3 is 15 ~ 25min; Heating the required time that stirs is 15 ~ 25min, and heating-up temperature is 90 ~ 100 DEG C.
Regulate the pH value of mixed liquor in described step 4 by the NaOH solution that concentration is 5mol/L, and during adjust ph, the rate of addition of NaOH solution is 0.01 ~ 1mL/min.
Required time that stirs in described step 4 is 15 ~ 25min;
Required time that stirs in described step 5 is 25 ~ 35min;
Required time that stirs in described step 6 is 35 ~ 45min.
Drying in described step 8 is dry 22 ~ 24h at 75 ~ 85 DEG C.
High activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst, it is mesoporous mpg-C 3n 4with bar-shaped cubic zircon phase RE-BiVO 4two-phase coexistent structure, and mpg-C 3n 4and RE-BiVO 4form heterojunction structure, mpg-C 3n 4and RE-BiVO 4mol ratio be (0.8 ~ 1.2): 1, RE be Nd or Nd+Er, its aperture is 3 ~ 65nm.
High activity mpg-C 3n 4/ RE-BiVO 4the application of heterojunction photocatalyst in degradation of organic substances.
Relative to prior art, beneficial effect of the present invention is:
The invention provides a kind of high activity mpg-C 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst and application.First mpg-C is prepared 3n 4powder is also disperseed in ethanol, then with five water bismuth nitrate (Bi (NO 3) 35H 2o) be bismuth source, ammonium metavanadate (NH 4vO 3) be vanadium source, and rare earth nitrades (RE (NO 3) 36H 2o) carry out rare earth doped, then add mpg-C 3n 4, by microwave-hydrothermal method one-step synthesis high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst.Its intermediary hole carbonitride (mpg-C 3n 4) as a kind of organic semiconducting materials, there is the layer structure of class graphite.Applicant is by comparing mpg-C 3n 4and BiVO 4band structure, find that they are the staggered band structures of mating very much, can be used for carrying out being compounded to form heterojunction structure, can effectively be separated photoinduced electron hole, improve the photocatalytic activity of catalyst.Appropriate application mpg-C of the present invention 3n 4mesoporous and layer structure feature, by itself and RE-BiVO 4inorganic semiconductor is compounded to form mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst, this hetero-junctions catalyst of preparation is porous material, has higher photocatalytic activity, effectively improves pure phase BiVO 4the efficiency of photocatalysis to degrade organic matter.The present invention adopts microwave-hydrothermal method one-step synthesis high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst, using microwave as mode of heating, combine the advantage of heating using microwave and hydro-thermal method, its operating process is simple and easy, and the reaction time is short, and reaction condition is gentle, the mpg-C of synthesis 3n 4/ RE-BiVO 4heterojunction photocatalyst has high photocatalytic activity, has a good application prospect in the process such as environmental wastewater.
High activity mpg-C prepared by the present invention 3n 4/ RE-BiVO 4heterojunction photocatalyst is mesoporous mpg-C 3n 4with bar-shaped cubic zircon phase RE-BiVO 4two-phase coexistent structure, and mpg-C 3n 4and RE-BiVO 4form heterojunction structure, be mesoporous material, aperture is 3 ~ 65nm, has larger specific area.This mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst has higher photocatalytic activity under simulated solar irradiation irradiates, and effectively can improve pure phase BiVO 4the efficiency of photocatalysis to degrade organic matter, have a good application prospect in the process such as environmental wastewater.
Accompanying drawing explanation
Fig. 1 is mpg-C prepared by the present invention 3n 4/ RE-BiVO 4the Fourier transform infrared spectroscopy figure (FT-IR) of heterojunction photocatalyst, wherein a ~ d is respectively the mpg-C that embodiment 1 is prepared to embodiment 4 3n 4/ RE-BiVO 4the FT-IR spectrogram of heterojunction photocatalyst.
Fig. 2 is mpg-C prepared by the present invention 3n 4/ RE-BiVO 4the FE-SEM figure of heterojunction photocatalyst, wherein a ~ d is respectively the mpg-C that embodiment 1 is prepared to embodiment 4 3n 4/ RE-BiVO 4the FE-SEM figure of heterojunction photocatalyst.
Fig. 3 is mpg-C prepared by the embodiment of the present invention 3 3n 4/ RE-BiVO 4the N of heterojunction photocatalyst 2adsorption-desorption isothermal curve.
Fig. 4 is mpg-C prepared by the embodiment of the present invention 3 3n 4/ RE-BiVO 4the pore size distribution curve of heterojunction photocatalyst.
Fig. 5 is mpg-C prepared by the present invention 3n 4/ RE-BiVO 4degradation rate-the time graph of the rhodamine B degradation of heterojunction photocatalyst, wherein a ~ d is respectively the mpg-C that embodiment 1 is prepared to embodiment 4 3n 4/ RE-BiVO 4the degradation curve of heterojunction photocatalyst.
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
Embodiment 1:
Step 1: be the melamine aqueous solution and the concentration of 2.12mol/L by concentration be the Nano-meter SiO_2 of 0.83mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 1h, then the oven for drying putting into 80 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 550 DEG C of insulation 4h with the programming rate of 2.5 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 2h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 20min, obtains the bismuth salting liquid that concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 95 DEG C, add thermal agitation 20min, obtain the vanadic salts solution that concentration is 0.4mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 20min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.5mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 20min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 30min, obtain forerunner Nd-BiVO 4suspension, wherein the mol ratio of Nd and Bi is 11.11:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-BiVO 4in suspension, magnetic stirring apparatus stirs 40min, ultrasonic disperse 1h, then stir 40min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 0.9:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 8min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 8min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 40min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 80 DEG C freeze-day with constant temperature 24h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 2:
Step 1: be the melamine aqueous solution and the concentration of 2.12mol/L by concentration be the Nano-meter SiO_2 of 0.83mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 1h, then the oven for drying putting into 80 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 550 DEG C of insulation 4h with the programming rate of 2.5 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 3h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 20min, obtains the bismuth salting liquid that concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 95 DEG C, add thermal agitation 20min, obtain the vanadic salts solution that concentration is 0.4mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 20min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.5mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 20min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 30min, obtain forerunner Nd-BiVO 4suspension, wherein the mol ratio of Nd and Bi is 11.11:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-BiVO 4in suspension, magnetic stirring apparatus stirs 40min, ultrasonic disperse 1h, then stir 40min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 1.0:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 8min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 8min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 40min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 80 DEG C freeze-day with constant temperature 24h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 3:
Step 1: be the melamine aqueous solution and the concentration of 2.12mol/L by concentration be the Nano-meter SiO_2 of 0.83mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 1h, then the oven for drying putting into 80 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 550 DEG C of insulation 4h with the programming rate of 2.5 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 3h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 20min, obtains the bismuth salting liquid that concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 95 DEG C, add thermal agitation 20min, obtain the vanadic salts solution that concentration is 0.4mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 20min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.5mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 20min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 30min, then by Er (NO 3) 36H 2o adds in mixed liquor, and magnetic stirring apparatus stirs 30min, obtains forerunner Nd-Er-BiVO 4suspension, wherein the mol ratio of (Nd+Er) total amount and Bi is 10.52:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-Er-BiVO 4in suspension, magnetic stirring apparatus stirs 40min, ultrasonic disperse 2h, then stir 40min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 0.9:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 8min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 8min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 40min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 80 DEG C freeze-day with constant temperature 24h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 4:
Step 1: be the melamine aqueous solution and the concentration of 2.12mol/L by concentration be the Nano-meter SiO_2 of 0.83mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 1h, then the oven for drying putting into 80 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 550 DEG C of insulation 4h with the programming rate of 2.5 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 4h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 20min, obtains the bismuth salting liquid that concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 100 DEG C, add thermal agitation 20min, obtain the vanadic salts solution that concentration is 0.4mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 20min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 1mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 20min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 30min, then by Er (NO 3) 36H 2o adds in mixed liquor, and magnetic stirring apparatus stirs 30min, obtains forerunner Nd-Er-BiVO 4suspension, wherein the mol ratio of (Nd+Er) total amount and Bi is 10.52:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-Er-BiVO 4in suspension, magnetic stirring apparatus stirs 40min, ultrasonic disperse 2h, then stir 40min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 1.1:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 8min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 8min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 40min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 80 DEG C freeze-day with constant temperature 24h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 5:
Step 1: be the melamine aqueous solution and the concentration of 2.1mol/L by concentration be the Nano-meter SiO_2 of 0.8mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 55min, then the oven for drying putting into 75 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 540 DEG C of insulation 4h with the programming rate of 2 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 3.5mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 1h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 15min, obtains the bismuth salting liquid that concentration is 0.35mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 90 DEG C, add thermal agitation 15min, obtain the vanadic salts solution that concentration is 0.35mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 15min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.01mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 15min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 25min, obtain forerunner Nd-BiVO 4suspension, wherein the mol ratio of Nd and Bi is 10.65:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-BiVO 4in suspension, magnetic stirring apparatus stirs 35min, ultrasonic disperse 1.2h, then stir 35min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 0.8:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 95 DEG C, at 95 DEG C of insulation 9min; Then 145 DEG C are warming up to from 95 DEG C, at 145 DEG C of insulation 9min; Be warming up to 175 DEG C from 145 DEG C again, after 175 DEG C of insulation 45min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 75 DEG C freeze-day with constant temperature 23.5h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 6:
Step 1: be the melamine aqueous solution and the concentration of 2.15mol/L by concentration be the Nano-meter SiO_2 of 0.85mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 65min, then the oven for drying putting into 85 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 560 DEG C of insulation 4h with the programming rate of 3 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4.5mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 1.5h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 25min, obtains the bismuth salting liquid that concentration is 0.45mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 92 DEG C, add thermal agitation 25min, obtain the vanadic salts solution that concentration is 0.45mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 25min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.1mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 35min, obtain forerunner Nd-BiVO 4suspension, wherein the mol ratio of Nd and Bi is 10.8:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-BiVO 4in suspension, magnetic stirring apparatus stirs 45min, ultrasonic disperse 1.4h, then stir 45min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 1.2:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 105 DEG C, at 105 DEG C of insulation 7min; Then 155 DEG C are warming up to from 105 DEG C, at 155 DEG C of insulation 7min; Be warming up to 185 DEG C from 155 DEG C again, after 185 DEG C of insulation 35min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 85 DEG C freeze-day with constant temperature 22h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 7:
Step 1: be the melamine aqueous solution and the concentration of 2.11mol/L by concentration be the Nano-meter SiO_2 of 0.82mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 58min, then the oven for drying putting into 78 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 545 DEG C of insulation 4h with the programming rate of 2.2 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 3.8mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 2.5h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 18min, obtains the bismuth salting liquid that concentration is 0.38mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 98 DEG C, add thermal agitation 18min, obtain the vanadic salts solution that concentration is 0.38mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 18min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.3mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 18min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 28min, then by Er (NO 3) 36H 2o adds in mixed liquor, and magnetic stirring apparatus stirs 28min, obtains forerunner Nd-Er-BiVO 4suspension, wherein the mol ratio of (Nd+Er) total amount and Bi is 10.9:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-Er-BiVO 4in suspension, magnetic stirring apparatus stirs 38min, ultrasonic disperse 1.6h, then stir 38min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 0.95:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 98 DEG C, at 98 DEG C of insulation 8.5min; Then 148 DEG C are warming up to from 98 DEG C, at 148 DEG C of insulation 8.5min; Be warming up to 178 DEG C from 148 DEG C again, after 178 DEG C of insulation 42min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 78 DEG C freeze-day with constant temperature 23h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Embodiment 8:
Step 1: be the melamine aqueous solution and the concentration of 2.13mol/L by concentration be the Nano-meter SiO_2 of 0.84mol/L 2the aqueous solution is 3:2 mixing and stirring by volume, and ultrasonic disperse 62min, then the oven for drying putting into 82 DEG C after stirring, obtain white solid, is ground in thin rear loading crucible, at N 2rise to 555 DEG C of insulation 4h with the programming rate of 2.8 DEG C/min in atmosphere furnace to calcine, obtain pale yellow powder, then use the NH of 4.2mol/L 4hF 2the aqueous solution corrodes, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4powder is added in 15mL ethanol, and ultrasonic disperse 3.5h, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is dissolved in deionized water, and magnetic stirring apparatus stirs 22min, obtains the bismuth salting liquid that concentration is 0.42mol/L; By NH 4vO 3be dissolved in the deionized water of 90 DEG C, at 96 DEG C, add thermal agitation 22min, obtain the vanadic salts solution that concentration is 0.42mol/L;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, magnetic stirring apparatus stirs 22min, obtains mixed liquor; Then in mixed liquor, drip with the rate of addition of 0.8mL/min the NaOH solution that concentration is 5mol/L, the pH regulating mixed liquor is 8, and stirs 22min on magnetic stirring apparatus;
Step 5: by Nd (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, magnetic stirring apparatus stirs 32min, then by Er (NO 3) 36H 2o adds in mixed liquor, and magnetic stirring apparatus stirs 32min, obtains forerunner Nd-Er-BiVO 4suspension, wherein the mol ratio of (Nd+Er) total amount and Bi is 11:100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner Nd-Er-BiVO 4in suspension, magnetic stirring apparatus stirs 42min, ultrasonic disperse 1.8h, then stir 42min on magnetic stirring apparatus, obtain reaction precursor liquid, wherein mpg-C 3n 4be 1.05:1 with the mol ratio of V;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, packing ratio is 70%, then microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 102 DEG C, at 102 DEG C of insulation 7.5min; Then 152 DEG C are warming up to from 102 DEG C, at 152 DEG C of insulation 7.5min; Be warming up to 182 DEG C from 152 DEG C again, after 182 DEG C of insulation 38min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, respectively washs three times with deionized water and absolute ethyl alcohol, then at 82 DEG C freeze-day with constant temperature 22.5h, obtain high activity mpg-C 3n 4/ Nd-BiVO 4heterojunction photocatalyst.
Fig. 1 is mpg-C prepared by the present invention 3n 4/ Nd-BiVO 4the Fourier transform infrared spectroscopy figure (FT-IR) of heterojunction photocatalyst, wherein a ~ d is respectively the mpg-C that embodiment 1 is prepared to embodiment 4 3n 4/ Nd-BiVO 4the FT-IR spectrogram of heterojunction photocatalyst, " mpg-C 3n 4" be the obtained mpg-C of the step 1 of embodiment 1 3n 4the FT-IR spectrogram of powder, " Nd-Er-BiVO 4" for not add mpg-C according to the step of embodiment 3 3n 4nd-Er-BiVO obtained during powder 4the XRD collection of illustrative plates of powder.See from Fig. 1, mpg-C prepared by the embodiment of the present invention 1 ~ 4 3n 4/ RE-BiVO 4heterojunction photocatalyst powder is at 3000-3600cm -1the peak that place occurs is because the stretching vibration of N-H and O-H produces, at 1200 ~ 1700cm -1strong peak that scope occurs (respectively 1240,1320,1407,1567 and 1640cm -1place) cause, at 808cm owing to the feature stretching vibration of CN heterocycle -1the peak that place occurs corresponds to mpg-C 3n 4triazine ring vibration mode, also 750 and 1640cm -1there is the stretching vibration peak of Bi-V key and V-O double bond respectively in place.So mpg-C 3n 4and RE-BiVO 4characteristic absorption peak all appear at mpg-C 3n 4/ RE-BiVO 4in heterojunction photocatalyst powder, this absolutely proves the mpg-C of preparation 3n 4/ RE-BiVO 4heterojunction photocatalyst is by mpg-C 3n 4and RE-BiVO 4two-phase is formed.
Fig. 2 is mpg-C prepared by the present invention 3n 4/ Nd-BiVO 4the FE-SEM figure of heterojunction photocatalyst, wherein a ~ d is respectively the mpg-C that embodiment 1 is prepared to embodiment 4 3n 4/ Nd-BiVO 4the FE-SEM figure of heterojunction photocatalyst.See from Fig. 2, the mpg-C of preparation 3n 4/ RE-BiVO 4heterojunction photocatalyst powder is by large layer structure mpg-C 3n 4with bar-shaped RE-BiVO 4composition, just looks at rod-shpaed particle and is attached to layered m pg-C 3n 4in structure, mpg-C is described 3n 4and RE-BiVO 4there is good contact on surface, can form heterojunction structure, is conducive to the separation that photoinduced electron hole is right, obtains high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst.
Fig. 3 is mpg-C prepared by the embodiment of the present invention 3 3n 4/ Nd-BiVO 4the N of heterojunction photocatalyst 2adsorption-desorption isothermal curve.See from Fig. 3, mpg-C prepared by the present invention 3n 4/ RE-BiVO 4heterojunction photocatalyst powder shows the thermoisopleth of IV type, is the hysteresis loop that 0.4-0.9 scope has H1 type at relative pressure, and the mpg-C of preparation is described 3n 4/ RE-BiVO 4heterojunction photocatalyst belongs to porous material.
Fig. 4 is mpg-C prepared by the embodiment of the present invention 3 3n 4/ Nd-BiVO 4the pore size distribution curve of heterojunction photocatalyst, finds out from the pore size distribution curve of Fig. 4, mpg-C prepared by embodiment 3 3n 4/ Nd-BiVO 4the aperture of heterojunction photocatalyst is mainly distributed in 3 ~ 65nm.
Fig. 5 is mpg-C prepared by the present invention 3n 4/ Nd-BiVO 4degradation rate-the time graph of the rhodamine B degradation of heterojunction photocatalyst, wherein a ~ d is respectively mpg-C prepared by embodiment 1 ~ 4 3n 4/ Nd-BiVO 4the degradation curve of heterojunction photocatalyst, RhB is the degradation curve that when not adding catalyst, rhodamine B is spontaneous.The C/C of ordinate in Fig. 5 0for the ratio of the concentration after certain rhodamine B degraded and its initial concentration in moment.See from Fig. 5, mpg-C prepared by the present invention 3n 4/ RE-BiVO 4heterojunction photocatalyst all has higher the disposal efficiency, and this is mainly due to mpg-C 3n 4/ RE-BiVO 4the result that the formation of heterojunction structure and porous and bar-shaped pattern etc. promote jointly.Wherein by mpg-C prepared by embodiment 1 ~ 3 3n 4/ RE-BiVO 4the degrading activity of heterojunction photocatalyst is the highest, under 120min simulated solar irradiation irradiates, and mpg-C 3n 4/ RE-BiVO 4the degradation rate of heterojunction photocatalyst to rhodamine B all reaches more than 96%.Illustrate that the present invention prepares high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst, can effectively utilize sunshine degradable organic pollutant, have potential using value.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading description of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.

Claims (10)

1. a high activity mpg-C 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that, comprises the following steps:
Step 1: be the melamine aqueous solution and the concentration of 2.1 ~ 2.15mol/L by concentration be the Nano-meter SiO_2 of 0.8 ~ 0.85mol/L 2the aqueous solution mixes for 3:2 by volume, stirs after ultrasonic disperse again, then dries, and obtains white solid, loads in crucible, at N by after white solid porphyrize 2be warming up to 540 ~ 560 DEG C of calcining 4h in atmosphere furnace, obtain pale yellow powder, then use NH 4hF 2aqueous corrosion pale yellow powder, removing SiO wherein 2template, finally washing, drying, obtain mpg-C 3n 4powder;
Step 2: by mpg-C 3n 4it is even that powder joins ultrasonic disperse in ethanol, obtains mpg-C 3n 4alcoholic solution;
Step 3: by Bi (NO 3) 35H 2o is soluble in water, stirs, and obtains bismuth salting liquid; By NH 4vO 3be dissolved in hot water, heating stirs, and obtains vanadic salts solution;
Step 4: be that vanadic salts solution is added in bismuth salting liquid by 1:1 by the mol ratio of Bi and V, stirs, obtains mixed liquor, and the pH value regulating mixed liquor is 8, continues to stir;
Step 5: by RE (NO 3) 36H 2in mixed liquor after O joins and have adjusted pH value, stir, obtain forerunner RE-BiVO 4suspension; Wherein RE (NO 3) 36H 2o is Nd (NO 3) 36H 2o or Nd (NO 3) 36H 2o and Er (NO 3) 36H 2the mixture of O, forerunner RE-BiVO 4in suspension, the mol ratio of RE and Bi is (10.52 ~ 11.11): 100;
Step 6: by mpg-C 3n 4alcoholic solution adds forerunner RE-BiVO 4in suspension, first stir, then ultrasonic disperse, then continue to stir, obtain reaction precursor liquid; Mpg-C in reaction precursor liquid 3n 4be (0.8 ~ 1.2) with the mol ratio of V: 1;
Step 7: reaction precursor liquid is added in microwave hydrothermal reaction kettle, microwave hydrothermal reaction kettle is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.3MPa, under the microwave power of 300W, from room temperature to 95 ~ 105 DEG C, insulation 7 ~ 9min; Then continue to be warming up to 145 ~ 155 DEG C, insulation 7 ~ 9min; Continue again to be warming up to 175 ~ 185 DEG C, after insulation 35 ~ 45min, terminate reaction;
Step 8: after question response terminates, is cooled to room temperature, takes out the sediment in microwave hydrothermal reaction kettle, and washing, drying, obtain high activity mpg-C 3n 4/ RE-BiVO 4heterojunction photocatalyst.
2. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: in described step 1, the time of ultrasonic disperse is 55 ~ 65min;
In described step 2, the time of ultrasonic disperse is 1 ~ 4h;
In described step 6, the time of ultrasonic disperse is 1 ~ 2h.
3. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: the bake out temperature in described step 1 is 75 ~ 85 DEG C;
Programming rate in described step 1 is 2 ~ 3 DEG C/min.
4. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: described NH 4hF 2the concentration of the aqueous solution is 3.5 ~ 4.5mol/L;
The concentration of described bismuth salting liquid and vanadic salts solution is 0.35 ~ 0.45mol/L.
5. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: the required time that stirs in described step 3 is 15 ~ 25min; Heating the required time that stirs is 15 ~ 25min, and heating-up temperature is 90 ~ 100 DEG C.
6. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: the pH value regulating mixed liquor in described step 4 by the NaOH solution that concentration is 5mol/L, and during adjust ph, the rate of addition of NaOH solution is 0.01 ~ 1mL/min.
7. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: the required time that stirs in described step 4 is 15 ~ 25min;
Required time that stirs in described step 5 is 25 ~ 35min;
Required time that stirs in described step 6 is 35 ~ 45min.
8. high activity mpg-C according to claim 1 3n 4/ RE-BiVO 4the preparation method of heterojunction photocatalyst, is characterized in that: the drying in described step 8 is 22 ~ 24h dry at 75 ~ 85 DEG C.
9. according to the high activity mpg-C in claim 1-8 described in any one 3n 4/ RE-BiVO 4the high activity mpg-C that the preparation method of heterojunction photocatalyst obtains 3n 4/ RE-BiVO 4heterojunction photocatalyst, is characterized in that: it is mesoporous mpg-C 3n 4with bar-shaped cubic zircon phase RE-BiVO 4two-phase coexistent structure, and mpg-C 3n 4and RE-BiVO 4form heterojunction structure, mpg-C 3n 4and RE-BiVO 4mol ratio be (0.8 ~ 1.2): 1, RE be Nd or Nd+Er, its aperture is 3 ~ 65nm.
10. high activity mpg-C according to claim 9 3n 4/ RE-BiVO 4the application of heterojunction photocatalyst in degradation of organic substances.
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