CN103920520A - Preparation method for synthesizing nano SnO2/g-C3N4 composite visible-light-driven photocatalyst by ultrasonic assisted deposition method - Google Patents
Preparation method for synthesizing nano SnO2/g-C3N4 composite visible-light-driven photocatalyst by ultrasonic assisted deposition method Download PDFInfo
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Abstract
The invention discloses a preparation method for synthesizing a nano SnO2/g-C3N4 composite visible-light-driven photocatalyst by an ultrasonic assisted deposition method, and belongs to the technical field of preparation of a photocatalytic material for purifying the environment. The method comprises the following processes: preparing nano SnO2 by microwave hydrolysis and microwave drying methods; preparing g-C3N4 through polycondensation of melamine, and then dispersing an obtained mixture into a methanol solvent after evenly grinding and mixing nano SnO2 and g-C3N4 according to the ratio; and evenly depositing nano SnO2 on the surface of g-C3N4 by the ultrasonic assisted deposition method, thereby obtaining the nano SnO2/g-C3N4 composite visible-light-driven photocatalyst. The prepared nano SnO2/g-C3N4 composite visible-light-driven photocatalyst disclosed by the invention has an excellent visible light catalytic property and good catalysis stability, and is simple in preparation method, short in reaction time, high in preparation efficiency and applicable to large-scale production, and the raw materials are readily available.
Description
Technical field
The present invention relates to a kind of ultrasonic wave assistant depositing method synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, belongs to depollution of environment photocatalyst material preparing technical field.
Background technology
From 1972, find that nano titanium oxide can be at decomposition water under illumination, Nano semiconductor photocatalysis technology has caused the extensive concern in the world, and is considered to the green environment purification techniques of tool development prospect and application prospect.Traditional Nano semiconductor photocatalyst material is as nano-TiO
2be widely studied with ZnO etc., but be subject to himself impact of large (3.2eV) of energy gap, had the problems such as under visible ray, response is weak, quantum efficiency is low, seriously restricted the practical application of photocatalysis technology.Therefore find the problem urgently to be resolved hurrily that development of new efficient visible light catalysis material becomes current photocatalysis field.
By research in recent years, find g-C
3n
4there is conjugated pi structure and be the most stable material in all carbonitride allotropes, there is very high heat endurance, chemical stability and excellent machinery, electrical and optical properties.Wang Xinchen etc. (Nature Materials, 2009,8:76-80) determine by experiment g-C
3n
4optical band gap is 2.7eV, and under radiation of visible light, the hydrogen manufacturing of energy catalytic decomposition water, is the potential novel visible catalysis material of a class.But regrettably, g-C
3n
4the quantum efficiency that generates hydrogen at 420nm place is about 0.1%, so g-C
3n
4in actual application, there is the limitation that self cannot break through.In order to improve g-C
3n
4visible light catalysis activity and catalytic stability, researcher has carried out a series of g-C
3n
4study on the modification as dye sensitization, transition metal modified, nano semiconductor material and g-C
3n
4the methods such as forming hetero-junctions that combines improves g-C
3n
4photocatalytic activity.Miao Xu (ACS Applied Materials & Interfaces, 2013,5:12533-12540) use Ag
2o and g-C
3n
4under room temperature, with liquid phase synthesizing method, prepare hetero-junctions composite semiconductor light-catalyst.Work as g-C
3n
4with Ag
2when O ratio is 1:4, can effectively suppress light induced electron and hole-recombination probability, improve photocatalytic, degradation rate is pure g-C
3n
411 times.The people such as Zhu Yongfa (Energy & Environmental Science, 2011,4:2922 – 2929) utilize g-C
3n
4conjugated pi structure, by g-C
3n
4carry out hydridization with ZnO, ZnO and g-C after hydridization
3n
4between produce cooperative effect, improved separation of charge efficiency and suppressed ZnO photoetch, under visible ray, observed photoelectric current.
Tetragonal SnO
2be the nano semiconductor material of broad-band gap, in fields such as lithium battery, air-sensitive and opto-electronic conversion, be widely used.Recently research is found, nano SnO
2be one and compare TiO
2with the better electron acceptor of ZnO, be more conducive to prepare highly active hetero-junctions catalyst.The people such as M Tamez Uddin (Inorganic Chemistry, 2012,51:7764-7773) adopt two-step method to prepare mesoporous nano SnO
2-ZnO heterojunction photochemical catalyst, effectively suppresses SnO
2-ZnO photochemical catalyst light induced electron-hole-recombination, thereby the photocatalytic activity of raising heterojunction photocatalyst.The people (Chemical Engineering Journal, 2014,246:277 – 286) such as Guangshe Li are with K
2snO
3for raw material, hydrolysis 12h in the autoclave of 180 ℃ makes nano SnO through 80 ℃ of dry 24h again
2, then joined the g-C after ultrasonic dispersion 30min
3n
4in ethanolic solution, mechanical agitation 24h evaporates after alcohol solvent, then calcines 1h at 400 ℃, has prepared the good nanometer g-C of photocatalytic activity
3n
4/ SnO
2composite visible light catalysis material.But the problem that this preparation method exists is, need experience reaction or dry processing procedure for several times, and reaction temperature is high, pressure is large, and the reaction time is long, also easily causes the reunion of nano particle, can affect nanometer g-C
3n
4/ SnO
2giving full play to of composite photocatalytic activity.
Summary of the invention
The object of the present invention is to provide a kind of ultrasonic wave assistant depositing method synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, with the standby nano SnO of this legal system
2/ g-C
3n
4composite has excellent visible light catalytic performance and good stability, and preparation method is simple, and the reaction time is short, and preparation efficiency is high.
For achieving the above object, the present invention is achieved by following technical proposals: with SnCl
45H
2o is raw material, adopts microwave induced hydrolysis, produces fast a large amount of SnO
2nucleus, and form small grains, suppress crystal grain and further grow up; Adopt microwave rapid draing simultaneously, remove high-temperature calcination from and process, guaranteed nano SnO
2the size homogeneous of particle, does not reunite.The melamine of take is prepared g-C as presoma adopts condensation methods
3n
4, then adopt ultrasonic wave assistant depositing method by prepared nano SnO
2with g-C
3n
4carry out compoundly, utilize the high-speed micro-jet that ultrasonic cavitation effect produces to make nano SnO
2at g-C
3n
4high-speed impact is carried out on surface, by nano SnO
2with good dispersity, deposit securely or be embedded in g-C
3n
4surface, make nano SnO
2/ g-C
3n
4composite visible light catalyst.Described preparation method mainly comprises the steps:
A. by 1.0g～10.5g SnCl
45H
2o adds in 10mL～20mL methyl alcohol, and ultrasonic dispersion 20min, is made into SnCl
4methanol solution, then under stirring condition to this SnCl
4methanol solution in to add the pH of weak aqua ammonia regulator solution be 2～3, slowly add again 50mL～100mL distilled water, continuing to stir 10min～15min mixes reactant liquor, then put into micro-wave oven and under microwave power 300W and 500W, respectively add thermal response 5min～15min, after having reacted, be cooled to room temperature, suction filtration.Filter cake carries out dry heat processing under microwave, and microwave drying condition is 300W and each 2min～6min of 500W, and taking-up obtains white powder after grinding, and is nano SnO
2.
B. get 3.0g～20.0g melamine and carry out polycondensation reaction in the inherent Muffle furnace of crucible, with the speed of 10 ℃/min～30 ℃/min, be warming up to 300 ℃, constant temperature 30min; Speed with 30 ℃/min～50 ℃/min is warming up to 400 ℃, constant temperature 30min again; Speed with 30 ℃/min～50 ℃/min is warming up to 500 ℃, constant temperature 30min afterwards; Finally the speed with 5 ℃/min～20 ℃/min is warming up to 520 ℃～600 ℃, constant temperature 0.5h～2h.React complete and take out after sample is naturally cooling, grind into powder.Gained powder is placed in to Muffle furnace again and carries out secondary polycondensation reaction, with the speed of 10 ℃/min～30 ℃/min, be warmed up to 500 ℃～580 ℃ constant temperature 0.5h～2h, after having reacted, after system is naturally cooling, take out sample and grind, obtain g-C
3n
4.
C. by the g-C of above-mentioned prepared 0.15g～0.8g
3n
4with 0.1g～0.7g nano SnO
2after ground and mixed 20min～30min, then join in 20mL～40mL methyl alcohol, ultrasonic dispersion 10min～20min under air-proof condition, then uncoveredly ultrasonicly become powder to mixture, continue again ultrasonic dispersion 5min～10min, gained powder is respectively washed 3 times with distilled water and methyl alcohol, dry 0.5h～1h at 50 ℃～70 ℃, taking-up obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.
Preferably, SnCl in step a
4snCl in methanol solution
4concentration be 0.6mol/L～1.0mol/L.
Preferably, in step a microwave hydrolysis process, under microwave power 300W and 500W, respectively heat 8min～12min.
Preferably, in step a microwave drying process, adopt power 300W and each 2min～3min of 500W, interval 1min.
Preferably, SnO described in step c
2and g-C
3n
4mixing quality is than 1:1～1:4.
Preferably, nano SnO in step c
2with g-C
3n
4the concentration of mixture in methyl alcohol be 20g/L～30g/L.
The invention has the advantages that:
(1) adopt microwave hydrolysis and micro-wave drying method to prepare nano SnO
2, obtain the SnO that average grain diameter is 2nm～3nm
2, fast, efficiency is high in reaction, and has avoided conventional high-temperature calcination to process the problems such as grain growth, reunion and catalytic activity reduction that cause.
(2) prepare nano SnO
2/ g-C
3n
4during composite visible light catalyst, adopt ultrasonic wave householder method, both can make nano SnO
2and g-C
3n
4in solvent, keep good dispersity, the high-speed micro-jet that ultrasonic cavitation effect produces simultaneously can make nano SnO again
2at g-C
3n
4high-speed impact is carried out on surface, thereby by nano SnO
2with good dispersity, deposit securely or be embedded in g-C
3n
4surface.Ultrasonic wave householder method completes recombination process fast, and reaches the incomparable effect of common mechanical complex method.
(3) nano SnO
2be one and compare TiO
2with the better electron acceptor of ZnO, with g-C
3n
4after compound, there is significant cooperative effect, can accept fast and shift g-C
3n
4be subject to the light induced electron of optical excitation generation, thereby effectively suppress the recombination probability in light induced electron-hole, make prepared nano SnO
2/ g-C
3n
4composite visible light catalyst shows excellent visible light catalytic performance.
(4) this method raw material sources are extensive, low price, and preparation method is simple, and reaction speed is fast, and the time is short, and preparation efficiency is high, is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the prepared nano SnO of embodiment 1
2/ g-C
3n
4the X ray diffracting spectrum of composite visible light catalyst;
Fig. 2 is the prepared nano SnO of embodiment 1
2/ g-C
3n
4the transmission electron microscope photo of composite visible light catalyst;
Fig. 3 is the prepared nano SnO of embodiment 1
2/ g-C
3n
4composite visible light catalyst (a) and pure g-C
3n
4and nano SnO (b)
2(c) catalytic degradation methyl orange experimental result picture under visible ray;
Fig. 4 is the prepared nano SnO of embodiment 1
2/
g-C
3n
4the circulation experiment result figure of composite visible light catalyst visible light photocatalytic degradation methyl orange.
The specific embodiment
Embodiment 1
Get 2.10g SnCl
45H
2o is dissolved in 10mL methyl alcohol, and ultrasonic dispersion 20min, is made into SnCl
4concentration is the methanol solution of 0.6mol/L, under stirring condition, adding weak aqua ammonia to regulate pH is 2.5, slowly add again 50mL distilled water, continuing to stir 15min mixes reactant liquor, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake is dried processing under microwave, and drying condition is microwave power 300W and each 3min of 500W, and interval 1min takes out, and grinds, and obtains white powder, is nano SnO
2.Get 15g melamine and in crucible, put into Muffle furnace, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set and with the speed of 10 ℃/min, is warming up to 300 ℃, constant temperature 30min; Speed with 40 ℃/min continues to be warming up to 400 ℃, constant temperature 30min; Speed with 40 ℃/min is warming up to 500 ℃, constant temperature 30min; 5 ℃/min is warming up to 560 ℃, and constant temperature 2h takes out grind into powder after sample is naturally cooling.Carry out polycondensation reaction by gained powder is uncovered in crucible, with the speed of 15 ℃/min, be warming up to 580 ℃, constant temperature 1h takes out and grinds and to obtain g-C after system is naturally cooling
3n
4.By 0.35g g-C
3n
4with 0.15g SnO
2in mortar, grind after 20min, join in 20mL methyl alcohol, seal ultrasonic dispersion 20min, the uncovered ultrasonic mixture that is dispersed to becomes powder again, after continuing ultrasonic dispersion 10min, powder is respectively washed 3 times with distilled water and methyl alcohol respectively, at 50 ℃, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.
Prepared nano SnO in the present embodiment
2/ g-C
3n
4the X ray diffracting spectrum of composite visible light catalyst as shown in Figure 1.In Fig. 1, locate diffraction maximum corresponding g-C respectively for 27.4 °, 13.2 °
3n
4(002) and (100) crystal face, locate respectively corresponding nano SnO of diffraction maximum for 33.5 °, 51.4 °
2(101) and (211) crystal face, with g-C
3n
4and SnO
2standard spectrogram (JCPDS87-1526 and JCPDS070-6153) identical.The prepared nano SnO showing from Fig. 2
2/ g-C
3n
4the transmission electron micrograph of composite photo-catalyst can be found out, g-C
3n
4for smooth and smooth layer structure, SnO
2evenly be embedded in g-C
3n
4surface, average grain diameter is 2～3nm, and without agglomeration.
Prepared nano SnO
2/ g-C
3n
4the performance test of composite visible light catalyst is as follows: in open reactor, add the prepared nano SnO of 0.1g
2/ g-C
3n
4the methyl orange solution that composite visible light catalyst and 100mL concentration are 10mg/L, with the concentrated sulfuric acid, regulating pH value is 3, under dark condition, stirring 1h reaches after adsorption equilibrium, open visible light source (two 36W fluorescent lamps, add a cover the following light of optical filter filtering 400nm) irradiate, from reaction system, sample in a certain time interval, after high speed centrifugation separated light catalyst, get supernatant liquor and measure full wave absorbance with ultraviolet-visible spectrophotometer, the change in concentration situation of methyl orange in solution is detected.Fig. 3 is the prepared nano SnO of embodiment 1
2/ g-C
3n
4composite visible light catalyst (a) and pure g-C
3n
4and nano SnO (b)
2(c) catalytic degradation methyl orange experimental result picture under visible ray.
As can be seen from Figure 3, when radiation of visible light 100min, the nano SnO that the present embodiment is prepared
2/ g-C
3n
4visible light catalyst reaches 95% to the visible light photocatalytic degradation rate of methyl orange, and the pure g-C preparing under the same terms
3n
4to the visible light photocatalytic degradation rate of methyl orange, be 15%, pure nano SnO
2degradation rate less than 3% to methyl orange, does not have visible light photocatalytic degradation active substantially.Nano SnO prepared by this method is described
2/ g-C
3n
4between two kinds of components in composite visible light catalyst, there is obvious cooperative effect, can effectively suppress the recombination probability in light induced electron-hole, the visible light catalysis activity of composite catalyst is significantly improved.
Embodiment 2
Get 4.20g SnCl
45H
2o is dissolved in 10mL methyl alcohol, and ultrasonic dispersion 20min, is made into SnCl
4concentration is the methanol solution of 1.2mol/L, under stirring condition, adding weak aqua ammonia to regulate pH is 2.5, slowly add again 50mL distilled water, continuing to stir 15min mixes reactant liquor, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake is dried processing under microwave, and drying condition is microwave power 300W and each 3min of 500W, and interval 1min, then takes out and grind, and obtains white powder, is nano SnO
2.Get 10g melamine and in crucible, put into Muffle furnace, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set and with the speed of 10 ℃/min, is warming up to 300 ℃, constant temperature 30min; Speed with 30 ℃/min continues to be warming up to 400 ℃, constant temperature 30min; Speed with 30 ℃/min is warming up to 500 ℃, constant temperature 30min; 5 ℃/min is warming up to 560 ℃, and constant temperature 1h takes out grind into powder after sample is naturally cooling.Carry out polycondensation reaction by gained powder is uncovered in crucible, with the speed of 20 ℃/min, be warmed up to 560 ℃, constant temperature 1.5h takes out after system is naturally cooling, after grinding g-C
3n
4.By 0.40g g-C
3n
4with 0.10g SnO
2in mortar, grind after 20min, join in 20mL methyl alcohol, seal ultrasonic dispersion 10min, the uncovered ultrasonic mixture that is dispersed to becomes powder again, and after continuing ultrasonic dispersion 10min, powder respectively washs 3 times with distilled water and methyl alcohol respectively, at 50 ℃, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.Experiment records above-mentioned nano SnO when radiation of visible light 100min
2/ g-C
3n
4composite photo-catalyst is 76% to the photocatalytic activity of methyl orange solution.
Embodiment 3
Get 6.20g SnCl
45H
2o is dissolved in 30mL methyl alcohol, and ultrasonic dispersion 20min, is made into SnCl
4concentration is the methanol solution of 0.6mol/L, under stirring condition, adding weak aqua ammonia to regulate pH is 2.5, slowly add again 100mL distilled water, continuing to stir 15min mixes reactant liquor, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake is dried processing under microwave, and drying condition is microwave power 300W and each 3min of 500W, and interval 1min takes out, and grinds, and obtains white powder, is nano SnO
2.Get 20g melamine and in crucible, put into Muffle furnace, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set and with the speed of 10 ℃/min, is warming up to 300 ℃, constant temperature 30min; Speed with 30 ℃/min continues to be warming up to 400 ℃, constant temperature 30min; Speed with 30 ℃/min is warming up to 500 ℃, constant temperature 30min; 5 ℃/min is warming up to 580 ℃, and constant temperature 1h takes out grind into powder after sample is naturally cooling.Carry out polycondensation reaction by gained powder is uncovered in crucible, with the speed of 20 ℃/min, be warmed up to 580 ℃ of constant temperature 1h, after system is naturally cooling, takes out and grind and to obtain g-C
3n
4.By 0.25g g-C
3n
4with 0.25g SnO
2in mortar, grind after 20min, join in 20mL methyl alcohol, seal ultrasonic dispersion 20min, the uncovered ultrasonic mixture that is dispersed to becomes powder again, and after continuing ultrasonic dispersion 5min, powder respectively washs 3 times with distilled water and methyl alcohol respectively, at 50 ℃, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.Experiment records above-mentioned nano SnO when radiation of visible light 100min
2/ g-C
3n
4composite visible light catalyst is 87% to the photocatalytic activity of methyl orange solution.
Embodiment 4
Choose the prepared nano SnO of embodiment 1
2/ g-C
3n
4composite visible light catalyst carries out cycle down solution methyl orange solution experiments to investigate its photocatalysis stability under visible ray.In circulation experiment, nano SnO
2/ g-C
3n
4composite visible light catalyst is used to repeat the methyl orange solution of degrading, and after illumination 160min, catalyst is through centrifugation, and washing, carries out the test of methyl orange solution degraded next time after being dried, and result is by shown in accompanying drawing 4.Fig. 4 is the prepared nano SnO of embodiment 1
2/ g-C
3n
4the circulation experiment result figure of composite visible light catalyst visible light photocatalytic degradation methyl orange, circulation experiment result from Fig. 4 can be found out, after 4 times are cycled to repeat use, this photochemical catalyst still keeps efficient photocatalytic activity, shows that this photochemical catalyst has good photocatalysis stability.
Claims (5)
1. a ultrasonic wave assistant depositing method synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, with SnCl
45H
2o is raw material, adopts microwave hydrolysis and micro-wave drying method to prepare nano SnO
2, the melamine of take is prepared g-C as presoma adopts condensation methods
3n
4, then by liquid phase deposition, prepare nano SnO under ultrasonic wave is auxiliary
2/ g-C
3n
4composite visible light catalyst, its method comprises the steps:
A. by 1.0g～10.5g SnCl
45H
2o adds in 10mL～20mL methyl alcohol, and ultrasonic dispersion 20min, is made into SnCl
4methanol solution, then under stirring condition to this SnCl
4methanol solution in to add the pH of weak aqua ammonia regulator solution be 2～3, slowly add again 50～100mL distilled water, continuing to stir 10min～15min mixes reactant liquor, put it into afterwards in micro-wave oven, under microwave power 300W and 500W, respectively heat 5min～15min reaction that is hydrolyzed, after having reacted, be cooled to room temperature, suction filtration, filter cake is carried out under microwave to dry heat processing, microwave drying condition is 300W and each 2min～6min of 500W, after filter cake is ground, obtain white powder, be nano SnO
2;
B. get 3.0g～20.0g melamine and carry out polycondensation reaction in the inherent Muffle furnace of crucible, first the speed with 10 ℃/min～30 ℃/min is warming up to 300 ℃, constant temperature 30min; Speed with 30 ℃/min～50 ℃/min is warming up to 400 ℃, constant temperature 30min again; Speed with 30 ℃/min～50 ℃/min is warming up to 500 ℃, constant temperature 30min afterwards; Finally the speed with 5 ℃/min～20 ℃/min is warming up to 520 ℃～600 ℃, constant temperature 0.5h～2h; React complete takes out after sample is naturally cooling, and grind into powder, gained powder is placed in to Muffle furnace again and carries out secondary polycondensation reaction, speed with 10 ℃/min～30 ℃/min is warmed up to 500 ℃～580 ℃ constant temperature 0.5h～2h, after having reacted, after system is naturally cooling, take out sample and grind, obtain g-C
3n
4;
C. by step a and the prepared 0.1g～0.7g nano SnO of b
2g-C with 0.15g～0.8g
3n
4after ground and mixed 20min～30min, join again in 20mL～40mL methyl alcohol, ultrasonic dispersion 10min～20min under air-proof condition, then uncoveredly ultrasonicly become powder to mixture, continue again ultrasonic dispersion 5min～10min, gained powder is respectively washed 3 times with distilled water and methyl alcohol, dry 0.5h～1h at 50 ℃～70 ℃, then can obtain nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.
2. ultrasonic wave assistant depositing method synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, SnCl in described step a
4snCl in methanol solution
4concentration be 0.6mol/L～1.0mol/L.
3. ultrasonic wave assistant depositing method synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, in described step a microwave hydrolysis course of reaction, under microwave power 300W and 500W condition, respectively heats 8min～12min.
4. ultrasonic wave assistant depositing method synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, microwave drying adopts batch (-type) mode of heating, 2min～3min circulating-heating under 300W and 500W, midfeather 1min described in step a.
5. ultrasonic wave assistant depositing method synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, nano SnO described in step c
2with g-C
3n
4mass ratio be 1:1～1:4, nano SnO
2with g-C
3n
4the concentration of mixture in methyl alcohol be 20g/L～30g/L.
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